Nanoindentation Techniques Materials

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Micro- and nanoindentation techniques for
mechanical characterisation of materials
N. K. Mukhopadhyay*
1
and P. Paufler
2
Indentation techniques have been extensively used for mechanical characterisation of materials.
Development of instrumented indentation techniques at low and ultra low load levels has further
improved their utility for understanding the mechanical responses of solids at micro and nano
scales. The variation of hardness with the load/depth of indentation, known as indentation size
effect, has led to difficulties in using hardness as a fundamental or characteristic mechanical
property of materials. Detailed discussions are focused on the issue of indentation size effect in
brittle and ductile solids. Various theoretical models accounting for the indentation mechanics are
highlighted. The results obtained from these techniques with quasicrystals, bulk metallic glasses
and nanomaterials are reviewed. The issues related to phase transformation during indentation
tests are briefly discussed. The industrial use of the indentation technique has been pointed out.
Some of the current issues and directions for future research in this field are mentioned.
Keywords: Microindentation, Nanoindentation, Indentation mechanics, Hardness, Indentation size effect
Historical development of the concept of
hardness
There have been various approaches to the concept
of hardness. It was Aristotle (384322 BC; Bekker,
1829), who called something hard if the surface did
not move under external pressure. When subdividing
hardness tests into cutting and non-cutting methods
of deformation, early attempts belong to the former.
Cutting of the material was mainly the consequence of
scratching the specimen by needles or corners of certain
reference materials. Non-cutting methods use an inden-
tation perpendicular to the surface of the specimen by an
indenter xed to a load cell or by a bullet of known
momentum. It is not surprising that hardness values
derived from these methods, either relative or absolute,
did not agree satisfactorily, because of the different
physical processes involved in testing. Much work has
been done in the past to understand these processes at
a microscopic scale, to make hardness values more
comparable and to nd a hardness concept which
genuinely reects a materials property (Turner, 1886;
Po schl, 1909; Tertsch, 1949; Tabor, 1951; Mott, 1956;
Glazov and Vigdorovic, 1962, 1971; Juskin, 1971; Petty,
1971; Grigorovic, 1976; Fischer-Cripps, 2004).
To recognise hardness as a quantity characteristic of a
material and to use it for analysis, several stages had to be
passed through. Some are just mentioned in the present
study. Apart from Aristotles general statement men-
tioned above, at the end of the 17th century, people were
already aware of the varying resistance of minerals and
other materials against mechanical loading, in particular
against scratching. Huygens (1690) noticed the fascinating
fact that the cleavage plane of calcite may be scratched
when moving the knife forward and may not when
moving it in the opposite direction. Reaumur (1722)
differentiated the quality of steel using a bar with
increasing hardness from one end to the other. The degree
of hardness was attributed to the specimen according to
the position on the bar which the specimen could scratch
rst. Linne (1768, 1793) listed a number of terms relevant
for an appropriate terminology of the mechanics of solids
which has been adopted by other writers. Werner (1774)
introduced four categories of hardness (hard, semihard,
soft, very soft) dened by the behaviour of the material
when scratched by a knife or a le using gauge minerals
for comparison. Then Hau y (1801) classied minerals
according to their ability to scratch each other, assigning
four grades to the materials scratching quartz, glass or
calcite and those not scratching calcite, respectively. Mohs
(1812) proposed to use hardness (combined with several
other properties) as a distinguishing feature of solids.
Later on, on the basis of the denition of hardness, he
introduced a ten-stage hardness scale (now named after
him) and instructions for its realisation (Mohs, 1822). The
anisotropy of the depths of scratches along different
directions in a plane as well as on crystallographically
different planes at constant load was measured thor-
oughly by Frankenheim (1829, 1831). Performing
scratches by hand, he noticed that features of the scratch
also depend on the topology of the contact and on the
speed of scratching. Thus, he recommended using relative
measures of scratching hardness.
1
Centre of Advanced Studies, Department of Metallurgical Engineering,
Institute of Technology, Banaras Hindu University, Varanasi 221 005, India
2
Institute for Structural Physics, Dresden University of Technology,
D-01062 Dresden, Germany
*Corresponding author, email mukho@bhu.ac.in or mukho_nk@rediffmail.
com
2006 Institute of Materials, Minerals and Mining and ASM International
Published by Maney for the Institute and ASM International
DOI 10.1179/174328006X102475 International Materials Reviews 2006 VOL 51 NO 4 209
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So far, the force applied was either not determined at
all or dened only qualitatively. It was Seebeck (1833)
who built an instrument enabling well dened loads to
be applied. Hardness was taken proportional to the
minimum load applied perpendicular to the surface,
which gave just a noticeable scratch when the surface
was shifted laterally. Franz (1850) introduced a similar
method independently of Seebeck, enabling the indenter
to be moved across the xed crystal. The methods of
scratching were subsequently made on a more quanti-
tative basis by evaluating the scratch geometry. Using
essentially Seebecks device, Grailich and Peka rek (1854)
improved the mechanical parts and the optical inspec-
tion of the scratches. They called their instrument a
sclerometer and, in doing so, launched the branch of
sclerometry (e.g. Sklerometrija, 1968). With the aid of
this instrument, Exner (1873) supplied data on the
anisotropy of hardness in great detail. Sometimes
alternative denitions were applied, as, for example,
hardness being inversely proportional to the lateral force
which is needed to move the specimen under a given
normal load (Franz, 1850; Grailich and Peka rek, 1854).
In any case, hardness values obtained this way were
rather upper limits of this entity, because they were
taken from the minimum load giving rise to a visible
scratch. The visibility, however, strongly depends on the
surface state of the specimen and/or the optical method
of recording the scratch. To reduce this uncertainty,
Po schl (1909) proposed to measure the change of the
scratch width versus the change of load instead of the
width itself. Martens (1898) introduced a scratch
hardness tester which has been widely used by mechan-
ical engineers, to measure the scratch width and the
normal load. He took as hardness the normal load
which caused a given scratch width. Recent work on
nanoscratching shows a proportionality between lateral
force and (normal force)
3/2
for a number of materials
(Kaupp and Naimi-Jamal, 2004). Further development
of this idea will not be followed here because it leads to
the concept of wear, which is not in the focus of the
present review.
In addition to scratching, which is still used today to
study wear resistance, other approaches to hardness
assessment in the 19th century should be mentioned
briey. Examples are planing, drilling, and grinding.
Planing was put forward by Pfaff (1883) who improved
the accuracy of measuring the depth of a scratch by
repeating the procedure n times along the same scratch
and, moreover, employing several diamonds side-by-side
at the same time. Knowing the mass density of the
specimen and the area scanned, the scratch depth could
be calculated from the weight loss after planing. Relative
hardness values of various minerals or various planes
and directions of the same mineral were then obtained
from the proportion of inverse planing depths, keeping
parameters such as load and speed to be constant.
Drilling with the aid of a cleaved diamond tetrahedron
has been recommended for hardness measurement by
Pfaff (1884) and Jaggar (1898), taking for hardness the
number of rotations needed to penetrate the surface to a
given depth. When grinding with a standardised powder,
hardness had been taken proportional to the time
needed for the removal of a certain layer or inversely
proportional to the loss of volume during grinding
(Jannettaz and Goldberg, 1895; Rosiwal, 1896). Later
on, von Engelhardt and Haussu hl (1960) showed that
resistance against grinding varies rather with the specic
free surface/interface energy.
Coming back to non-cutting methods, an early attempt
is mentioned rst to nd numerical values for the relative
hardness of metals due to ofcers of the US Ordnance
Department who in 1856 pressed a pyramid on the metal
under test recording the volume of the indent and using
bronze as a standard (Turner, 1886). Then Calvert and
Johnson (1859) applied a steel cone to penetrate the
material under investigation until a predetermined
indentation depth was achieved. The load necessary was
used as a measure of hardness relative to the value of pig
iron. The subsequent development of indentation hard-
ness testing methods was mostly stimulated by the rapidly
growing demand of metallurgy.
A milestone towards a quantitative concept of
hardness was the approach published by Hertz (1882),
who dened the indentation hardness of solids as
contact pressure in a small circular area at the elasticity
limit. This denition was applied to brittle as well as to
ductile solids. However, experimental verication latter
proved difcult, whereas the elasticity limit of brittle
solids could be determined from the pressure at the onset
of cracking. This was the advent of contact mechanics,
an important tool of present-day hardness testing (cf.,
e.g. Johnson, 1996). In order to take the onset of plastic
deformation explicitly into account, Prandtl (1920,
1921) introduced as decisive criterion, the critical shear
stress as the difference of two principal stresses under
the indenter using a proposal made by von Mises (1913).
On the basis of Hertzs denition, Auerbach (1890,
1891) determined the hardness of brittle solids by
optically in situ monitoring the nucleation of cracks
under load in glasses and crystalline quartz. He
recognised that the hardness dened by the rst
appearance of a crack was subject to variation with
the curvature of the indenter. Since cracks opened under
tensile stress, he concluded that the surface condition
might also have inuenced crack nucleation. Extending
the in situ measurements to ductile transparent solids
such as rock salt, calcite, uorite and others, Auerbach
(1892, 1896) proposed that hardness be taken as Hertzs
pressure at the onset of plastic ow indicated by an
almost constant contact pressure. When applying to
(opaque) metals, the area of contact was determined
employing a blackened indenter (Auerbach, 1900).
Using loads below 2 N, hardness was termed micro-
hardness, though the distinction between macro- and
microhardness is rather arbitrary. Nevertheless, a micro-
hardness tester looked different mainly because of the
higher optical resolution required. Various devices have
been developed. Lips and Sack (1936) and Lips (1937)
introduced a small attachment to the light microscope
which enabled indentations into small grains of multi-
phase alloys to be made by moving the specimen
towards a Vickers diamond pyramid coupled to a
spring. In the Vickers indenter, the angle between
opposite faces is 136u. This angle results from the
condition that, from the tangents drawn from the points
of contact of an impression of diameter 0
.
375D (where D
is the ball diameter as used in the Brinell test) to the
circumference of the indent, the included angle be 136u.
Smith and Sandland (1925) found that the hardness
values obtained with the Vickers indenter of that angle
Mukhopadhyay and Paufler Micro- and nanoindentation techniques for mechanical characterisation
210 International Materials Reviews 2006 VOL 51 NO 4
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and with the Brinell ball are nearly equal, when the load
has been adjusted to produce a Brinell impression of the
diameter 0
.
375D, which is considered the ideal impres-
sion diameter halfway between 0
.
25D and 0
.
5D. Unlike
other test methods, Vickers hardness is named after the
company Vickers Ltd, which designed the rst hardness
testing machine with this indenter. After replacing this
microhardness tester by the objective of the microscope,
the diameter of the indents (of the order of 10 mm) could
be measured (for Russian devices, cf. Glazov and
Vigdorovic, 1962, 1971). While in a conventional micro-
or macrohardness test, penetration depths h of the order
of 10
1
10
3
mm and forces F in the range 10
22
10
2
N
occur, in a nanohardness test, both h and F are
signicantly smaller (F,10 mN, h,10 mm) and in
this case compulsory the dependence F(h) is recorded
throughout the loadingdeloading cycle. (cf. Fischer-
Cripps, 2004).
Indentation methods experienced another diversica-
tion. Starting with spherical indenters (Hertz, 1882;
Brinell, 1900), other shapes had been found useful
for various purposes, such as cones (Ludwik, 1908;
Rockwell, 1922), double cones (Grodzinski, 1951),
trigonal prisms (Attinger, 1947) or pyramids (tetragonal:
Smith and Sandland, 1925; orthorhombic: Knoop et al.,
1939; trigonal: Berkovic, 1951). It was already noticed
by Auerbach (1891), that the exact shape of the indenter
must have an impact upon the hardness value. The
shape of the indents as well as the relation between
hardness values and indentation geometry is displayed in
Table 1.
This brings us to the evaluation of indentation
hardness H as it is used today. Let an indenter under
load F penetrate the surface of a solid so that the contact
area between indenter and surface is A. Then the
hardness H of the solid can be dened as the ratio
H~
force F (perpendicular to the surface)
contact area A
(1)
If A is taken as the curved area of the indent, H depends
Table 1 Geometrical shape of indenter and projected indentation along with hardness equation and penetration depths
displayed for various indenters
Testing
method
Shape of
indenter
Shape of impression
protection Hardness value Penetration depth
Brinell H
e
~
2F
pD
2
1{ 1{(d=D)
2

1=2
_ _
Brinell hardness number BHN;
[F]5kg; [D], [d]5mm
t5D{1[1(d/D)
2
]
1/2
}<d
2/
2D
Vickers
H
V
~
2F sin 68
0
d
2
~
1
:
8544F
d
2
Vickers hardness number VHN;
F~kg, d~mm
t<d/7
Knoop
H
K
~
F
A
~
14
:
40F
d
2
Knoop hardness number KHN;
F~kg, d~mm
t<d/30
.
6
Ludwik
H
L
~
4Fsin45
0
pd
2
~
0
:
9F
d
2
t5d/2
Grodzinski
H
G
~F=A
t
~
6rF
pd
2
~
0
:
9F
tan(a=2)d
3
Double cone number a~154
0
r~2 mm
HGN~
2
:
77F
d
3
10
6
D~mm, a~154
0
, F~kg
t<d/80 for a5154u, r52 mm
Berkovich
H
B
~F=A~2F=a
2

3
p
t<0
.
19a
International Materials Reviews 2006 VOL 51 NO 4 211
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strongly on the shape of the indenter. Hence Brinell,
Ludwik, Grodzinski, Rockwell, Vickers, or Knoop
hardness numbers are differentiated. A more physical
meaning is assigned to H, when A is taken as the
projection of the area of contact, A
p
, between indenter
and surface onto the surface. This denition has become
known as Meyer hardness H
meyer
(Meyer, 1908), the
physical meaning of which is the mean pressure p over
the surface of the indentation, if the friction between the
surface of the indenter and the sample can be neglected.
Then the pressure is normal to the surface of the indent.
For symmetry reasons, the horizontal component of the
resultant force upon the specimen is zero. The vertical
component of that force is equal to the total force F,
which amounts to
_
r
0
p 2pxdx~ppr
2
~pA
p
~F (2)
x being the radius of an annulus of the contact surface.
2r is the chordal diameter and pr
2
the projected area of
the indentation. Thus, H
meyer
5p. Knowing the geometry
of the contact surface of any test method, the
corresponding hardness values may be readily converted
into values of H
meyer
. Recently, Pohlenz et al. (2001)
studied the different hardness denitions usable for
micro and nanoindentation in order to describe the
hardness of substrates and layers by relational coef-
cients. Malzbender (2003) discussed in detail the various
denitions of hardness and elastic modulus as obtained
with conical and spherical indenters and made a
comparison in order to obtain a relationship that
permits a conversion and assessment of their differences.
Macro-, micro- and nanoindentation hardness testing
continue to be used extensively in materials evaluation,
and various aspects of this subject have been reviewed
earlier [Westbrook and Conrad, 1973; Blau and Lawn,
1986; Biswas et al., 1996; Fischer-Cripps, 2004; special
issues in Philosophical Magazine A (1996, 2002) and
Journal of Materials Research (1999, 2004), Materials
Research Society Symposium Proceedings (Baker et al.,
1995, 2000; Drory et al., 1995; Gerberich et al., 1996;
Cammarata et al., 1997; Moody et al., 1998; Vinci et al.,
1999; Ozakan et al., 2001)]. It is interesting to note that
various techniques have been developed to study the
materials response during and after the indentation. In
addition to conventional optical microscopy, these
techniques include cathodoluminescence, scanning elec-
tron microscopy, transmission electron microscopy
(TEM), focused ion beam techniques (FIB), interface
force microscopy (IFM), atomic force microscopy
(AFM), acoustic microscopy, acoustic emission techni-
que, Raman spectroscopy (see for example Brown et al.,
1988; Boldt et al., 1992; Muraki et al., 1997; Ray et al.,
1999; Wolf and Pauer, 1999a,b,c; Kiely et al., 1999;
Mukhopadhyay et al., 2001; Tymiak et al., 2004).
Recently, Bhushan and Li (2003) have reviewed in detail
the various aspects of nanoindentation test apparatus,
the data analysis and the application of nanoindentation
techniques for determination of mechanical properties
with special emphasis on thin lms. Here, the origin of
the variation of hardness with the load/depth of
indentation is discussed in detail. The use of indentation
techniques and results on new materials such as
quasicrystals, bulk metallic glasses and nanomaterials
are clearly illustrated. The issues related to phase
transformation during indentation tests are discussed.
Current industrial practices employing indentation
techniques are mentioned.
Indentation size effect
The hardness obtained from the geometrically similar
indenters, i.e. conical or pyramidal (e.g. Knoop, Vickers,
Berkovich) at various loads is expected to remain
unchanged as the strain during the indentation is constant
unlike the spherical indenter. However, in a practical
situation, the hardness using similar indentations is found
to vary with the load. The increase in hardness with
decreasing load, which is known as indentation size effect
(ISE), is often observed in metallic, ceramic and inter-
metallic materials (Fig. 1a) (see for example, Mott, 1956;
Gane, 1970; Gane and Cox, 1971; Chen and
Hendrickson, 1973; Boldt et al., 1992; Poole et al., 1996;
Grau et al., 1998, Murthy et al., 1999; Mukhopadhyay
et al., 2001; Gong and Li, 2000; Ma and Clarke, 1995;
Gao et al., 1999a; Elmustafa and Stone, 2002, 2003;
Swadener et al., 2002; Pauer and Wolf, 2003). There is
also a report of a decrease in the hardness with the
decrease in the load, known as reverse ISE (RISE)
(Sargent, 1986; Upit and Varchenya, 1973; Lim and
Chaudhuri, 1999; Sangwal, 2000). Earlier, various
explanations were offered to account for the ISE and
RISE. All these interpretations to some extent had some
utility, but they failed to account for this effect
universally. Turley and Samuels (1981) earlier suggested
that ISE is due to abraded surface layers and oxides on
the indented surface. Pethica and Taylor (1979) inter-
preted that the ISE is due to chemical contamination.
However, Samuels (1986) proposed that the ISE is a
result of inadequate measurement capability of small
areas of indents and elastic recovery of indents. Li et al.
(1993) suggested that ISE can be attributed to the
indenterspecimen friction. These variations of the
hardness lead to uncertainty in the determination of
the characteristic mechanical properties of materials.
Therefore, it is important to understand the mechanisms
responsible for the variations in the hardness. There are
several empirical and micro-mechanism based theories
based on elastic recovery, energy balance, strain gradient
plasticity (SGP), surface roughness and friction, to
account for the ISE. However, it must be emphasised
that the origin of the ISE and the RISE are not yet clearly
understood and it is still a debatable and controversial
subject. A full hardness characterisation with a hardness
load curve is necessary to attach true signicance to
the hardness value as a characteristic property of the
material. Various approaches to account for the origin of
the ISE are discussed in the following sections.
Meyers power law
Plots of hardness versus load/indentation data are
sometimes tted to Meyers law, which was originally
developed to determine the work hardening capacity of
metals in Brinell hardness tests. The power law equation
generally employed to analyse the loadindentation data
(e.g. Mott, 1956; Bu ckle, 1965) can be expressed as
P~k
1
d
n
(3)
where P is the load, k
1
and n are materials constants and
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d is the indentation (diagonal/diameter) size. This power
law equation is also referred to in the literature as
Meyers law (Hays and Kendall, 1973; Li and Bradt,
1991; Gong and Li, 2000; Murthy et al., 1999; Liu et al.,
2003). It should be noted that Meyers equation was
originally developed for a spherical indenter, where n is
directly related to the strain hardening coefcient of the
material (Meyer, 1908). Onitsch (1947) extended
Meyers power law equation for nonspherical indenters
and observed that in a macrohardness range n is 2
.
0,
whereas in a microhardness range, n is less than 2,
irrespective of the type of material. When n is equal to 2,
the above power law equation is also quoted as Kicks
law in literature (Kick, 1885). Figure 1a shows the
indentation size effect while plotting the Vickers hard-
ness of quasicrystalline material at various loads. These
data were further analysed using Meyers power law
(equation (3)) in a loglog plot (Fig. 1b) from which the
power law index, n is obtained as 1
.
919, the index of
indentation size effect. It has been pointed out earlier by
several workers that Meyers constant, k
1
has a strange
dimension of force/(length)
n
, which is dependent on the
value of n (Li and Bradt, 1991; Sargent, 1986; Ghosh
et al., 2003). In order to resolve this problem, Li and
Bradt (1991) introduced the reference indentation size
corresponding to a load independent hardness, whereas
Sargent (1986) suggested the use of 10 mm indentation
size corresponding to the standard hardness as a
reference. Meyers power law is unable to determine
the true or load-independent hardness as it is continu-
ously decreasing with load. In fact, in an extended
load range, Meyers power law may not be able to
give a good correlation with the experimental data.
Nevertheless, it is convenient to handle the indentation
data. Grau et al. (1998) studied the strain rate
dependence of the hardness of glass and found a good
correlation with Meyers law by analysing the depth
sensing Vickers hardness data on glass for various
loading regimes. However, the differences in Meyers
parameters under different loading regimes require
further investigation for better understanding of the
implication of Meyers law.
Minimum resistance model
Hays and Kendall (1973) were the rst to suggest that
there is a minimum resistance on the surface, which
leads to the violation of Meyers law and hence the ISE
is observed. This is signicant at lower load. Therefore,
the actual force acting during indentation is lower than
that. According to this model, the forcedisplacement
relation can be expressed as
P~wzk
h
d
2
(4a)
One can determine w (minimum resistance against
plastic deformation) and constant k
h
from the intersec-
tion of the linear plot of !P versus d or P versus d
2
.
Therefore, the load-independent hardness can be
expressed as
H
T
~k
P{w
d
2
~kk
h
(4b)
where k is the indenter shape factor (e.g. 1
.
854 for
Vickers hardness). This approach has been veried in
various metallic materials, such as Al, Cu and mild steel
using the Vickers and Knoop indenter. However, the
minimum load obtained by this analysis was higher than
any practical value. It was also found that for crystals
showing a RISE, the plot of experimental data does not
give a good t. Furthermore, negative values of w for the
data at low loads do not give rise to any meaningful
interpretation.
Polynomial series
Bernhardt (1941), Mitsche (1948), Bu ckle (1965), and
other workers (Fro hlich et al., 1977; Babini et al., 1987)
have approached the relation between P and d from a
1 a Variation of microhardness obtained from AlCo
CuSi single quasicrystals with load, establishing the
indentation size effect; error bar in each measurement
can be seen (after Mukhopadhyay et al., 2001); b
variation of microhardness with load from AlCuCo
poly-quasicrystals, showing indentation size effect; c
corresponding logarithmic plot from which the Meyers
index, n is obtained as 1
.
919 (after Murthy et al., 1999)
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different point of view. They have proposed a poly-
nomial relation to correlate P and d as
P~
i
a
i
d
i
(5)
where i is a series of integers. By limiting the number of
terms and assuming a
o
is zero for P50 one gets
P~a
1
dza
2
d
2
. By considering the contracted series as
an energy balance, because Pd is equivalent to the
energy or work so that a
1
d may be related to the surface
energy (a
1
d
2
) and the a
2
d
2
term may be related to volume
energy of deformation (a
2
d
3
), some form of physical
signicance has been attributed to both a
1
and a
2
. Based
on the consideration of energybalance, Bernhardt rst
suggested that the rst term of the equation represents
the surface energy term and the second term represents
the volume energy term. As a result of this series
approach, the a
1
represents the energy per indentation
surface area and the a
2
represents the energy per
indentation induced volume deformation. From various
analyses, it appears that attaching true signicance to a
1
in terms of surface energy was not quite successful. It
can be pointed out that the a
o
term has been neglected
without sufcient justication. However, according to
the Hays and Kendall model, a
o
is w (minimum
resistance), and therefore it should be related to the
load for initiation of permanent deformation. Because
a
o
is so small, it can be neglected in microindentation.
However, to understand the nanoindentation process,
the load for indentation of permanent deformation may
need to be included, which necessitates incorporation of
the effects of the indenter tip radius effect on the elastic
limit during indentation.
Proportional specimen resistance (PSR)
Li and Bradt (1991, 1993) have extended the idea that
the resistance offered by the surface is not constant
throughout the indentation size but rather dependent on
the indentation size. They proposed a model based on a
proportional surface resistance (PSR) model. According
to this model, load is expressed as
P~a
1
dza
2
d
2
(6)
where a
1
is related to the proportional resistance offered
by the surface of the specimen and a
2
is related to the
volume. Therefore, the hardness can be expressed as ka
2
.
The effect of the rst term is larger as the load is
decreased. However, at higher load, the effect of the rst
term is negligible. The plot of Pd versus d should yield a
linear plot from which one can determine a
1
and a
2
and
thus the true hardness. This is exactly the same as the
truncated polynomial series indicated above. However,
the physical interpretation of the two constants a
1
and a
2
is distinctly different. In the Li and Bradt model (1991),
a
1
describes the Newtonian like specimen resistance
of the test specimen and a
2
is Kicks law coefcient
relating to the true hardness. Ren et al. (2002) have
investigated microhardness indentations on single-
crystal MgO (001) along ,110.in air for loads between
0
.
125 and 1
.
001 kg and temperatures between 20 and
600uC (Fig. 2a), and also the inuence of interfacial
coatings and lubricants. They observed that the ISE
decreased with increasing test temperature, and it was
unaffected by coating or lubrication. The experimental
data tted equally well either the Meyers power-law and
the proportional specimen resistance (PSR) models
(Fig. 2a,b). They have proposed qualitatively that the
ISE is controlled by the extent of elastic recovery
occurring on removal of the load, and shown the
correlation of n (as in equation (1)), the index of ISE,
with the hardness-to-elastic modulus ratio H/E (Fig. 3).
Energy balance approach
Quinn and Quinn (1997) have investigated the varia-
tion of Vickers hardness with indentation load for a
variety of ceramic materials. They observed that such
2 a Indentation data for MgO (001) along ,110. plotted
according to Meyers power law in logarithmic form; b
indentation data for MgO (001) along ,110. plotted
according to the PSR model (after Ren et al., 2002)
3 Correlation of power-law index n with hardness-
to-modulus ratio H/E for a range of single-crystal cera-
mics (after Ren et al., 2002)
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hardnessload curves exhibit a distinct transition to a
plateau with constant hardness level and concluded that
the transition in such curves corresponds to the intrinsic
hardness values of the materials. These investigators
suggested an energy balance model for the Vickers
indentation process. The model considers that the
external work applied by the indenter is consumed in
the deformation and fracture process in the material. The
load dependence of hardness has been considered by Li
and Bradt (1996) and Dutta et al. (2001). According to
their approach, the measured diagonal of an indentation
at a particular load is an apparent value, which remains
associated with an uncertain amount of relaxation. The
extent of relaxation in the indentation diagonal occurs
due to several possibilities such as crack formation,
dislocation activity, elastic recovery at the tip of the
indentation. The true hardness can be evaluated as
H~H
o
1z
d
e
d
_ _
2
(7)
where d5d
o
zd
e
is the apparent diagonal, d
o
is the true
diagonal and d
e
the relaxation in the diagonal after
removal of the indenter.
However, recent works by several researchers have
shown that the linear relationship between P/d versus d
may only be valid in a narrow range of applied loads.
When a relatively wider range of applied loads is
considered, the above equation was found insufcient.
A modication of the above equation has been
suggested (Gong and Li, 2000; Quinn and Quinn,
1997). The above equation can be written as
P
o
~ad
o
zbH
T
d
2
o
(8)
where P
o
and d
o
are the load and indentation size
without any experimental error. a is constant related to
the surface energy of the material, and b is a constant
related to the indenter. Gong and Li (2000) have argued
that experimental errors are usually inevitable in
conventional hardness testing and therefore it should
be considered. In general, the experimental error in the
test has been divided into two classes (i) measurement of
indentation size, and (ii) indentation load. Considering
the experimental error in both the load and the
indentation size as r and d, respectively, i.e. by insertion
of P
0
5Pzr and d
o
5dzd into equation (6), equa-
tion (7) may be rearranged in the following form
P~a
o
za
1
dza
2
d
2
(9a)
where a
o
~bH
T
dzad{r, a
1
~2bH
T
dza, a
2
~bH
T
. P
has now been split into three parts. It is important to note
that all of the parameters are functions of the experi-
mental error and the true hardness. However, a
2
is only
dependent on the true hardness. Equation (9a) can be
used for estimating the true hardness, i.e. the energy
needed to produce the permanent deformation of a unit
volume. Now a reasonable explanation can be offered for
the size effect in low hardness testing. The rst parameter
a
o
is related to the surface residual stress, depending on
the surface preparation, and is not really a materials
property. The second parameter is due to the creation of a
new surface by indentation and cracking, the third is
dependent on the volume of the indentation. The above
equation is easy to appreciate from the energy point of
view. The energy applied is related to Pd, and the energies
related to the surface phenomena and the volume are
basically a
1
d
2
and a
2
d
3
. The argument is, if the effective
energy or the force can be determined, then the true
hardness, which is a characteristic property of the
material, can be easily determined and in that sense, the
ISE can be tackled. Here a
2
is related to the true hardness
H
A
~
k(a
o
za
1
dza
2
d
2
)
d
2
~k
a
o
d
2
z
a
1
d
_ _
zH
T
(9b)
In many cases, it is found that the value of a
o
is so low
that the above equation without a
o
will t the
experimental data very well. The physical signicance
of the above equation lies in splitting the energy or the
force into the surface and volume related terms. This
also takes care of the effect of microcracking. The ratio
of a
2
/a
1
, has been suggested to be related to H/E
parameter of the materials. It is important to mention
that the above model is able to explain the ISE as well as
the RISE, whereas the model by Bradt and Li will not be
able to explain the RISE (Figs. 4 and 5).
4 Indentation size-dependence of apparent hardness for
annealed mullite sample (after Gong and Li, 2000)
5 Load dependence of apparent hardness for sample Ti
(C,N) based cermet; square symbols represent experi-
mentally measured data, solid line represents predic-
tion of equation (8) and dashed line represents
prediction of equation (8) assuming a
0
50 (after Gong
et al., 2001)
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Combined approach: Meyers power law and
energy balance model
Recently, Mukhopadhyay (2005) combined both the
Meyers law approach and the energy balance model
and analysed the indentation data. The analysis has been
discussed there. The hardness for an indentation using
load P, the corresponding indentation area A, and the
indentation size s, can be written using equation (1) in
terms of indentation size, Meyers constant and the
indenter shape factor as
H
s
~
P
A
~k
P
s
2
~
kk
1
s
n
s
2
~kk
1
s
n{2
(10a)
From the above equation, Meyers constant k
1
can be
written in terms of hardness as
k
1
~
H
s
ks
n{2
(10b)
Now inserting the expression for constant k
1
in
equation (1)
P~
H
s
ks
n{2
d
n
~
H
s
s
2
k
d
s
_ _
n
(11)
or simply as P~K
m
D
n
, where K
m
~
H
s
s
2
k
~P
s
is dened
as the normalised Meyers constant and D~
d
s
is dened
as the normalised indentation size. By this transfor-
mation, one can overcome the dimensional problem
encountered in the classical Meyers equation. Now, this
new Meyers constant can be related to hardness or load
for the indentation, which can be dened at any length
scale. However, as a natural choice, an indentation size
s51 mm will be assumed so that one can recover Meyers
equation in the sense of parameters but not in terms of
exact units and dimensions of Meyers constants. The
normalised Meyers constant will have a force dimen-
sion. So, equation (9) can be transformed to a hardness
equation and can be written as (using s51 mm)
H~H
1m
D
n{2
~
kK
m
s
2
D
n{2
~kK
m
D
n{2
(12)
Now, one can summarise the relations obtained by
normalising the classical Meyers power law equation
as
P~K
m
D
n
; or P~P
s
D
n
(13a)
and
H~H
1m
D
n{2
(13b)
Using the notation of Li and Bradt (1991) for the critical
indentation size as d
o
* and critical load P
c
, from
equation (6a)
P~P
c
d
d
0
_ _
n
(14)
While comparing this equation with equation (17) of Li
and Bradt (1991), it can be noted that both equations are
identical except for an extra (2/n) factor, which is
associated with the right-hand side of their equa-
tion (17). After analysing their approach, it can be seen
that this factor was erroneously incorporated in the
normalised Meyers equation proposed by them, though
the actual numerical value may not signicantly affect
the analysis. However, the normalised Meyers equation
in terms of critical load and indentation size should be
represented correctly by equation (14) above.
The nature of equation (14) suggests that hardness
continuously decreases with the increase in load/size.
Therefore, it cannot predict the transition from ISE
regime to non-ISE regime. In order to determine the
transition, the true hardness H
T
based on the energy
balance model is incorporated. Initially at lower load,
the apparent hardness will give rise to ISE. But after a
critical load or indentation size, H
A
will be equal to H
T
.
The apparent hardness obtained from normalised
Meyers equation (13b) can be equated with the true
hardness corresponding to the critical indentation size,
d*. Therefore, from the above argument, Meyers
equation can be correlated with the energy balance
model. The condition of equality is as follows
H
A
~H
1
D
n{2
, H
T
~kc
therefore
H
1
D
n{2
~kc (15)
Now from the above condition, the critical indentation
size, d* can be obtained, after which ISE should cease to
exist. Using the value of H
1
5kK
m
s
2
and the above
equation has been rearranged as
d
~
K
m
s
2
c
_ _
1
2{n
~
K
m
c
_ _ 1
2{n
in mm as s~1 mm (16)
This is an important relation, which correlates the
normalised Meyers equation and the energy balance
model. The implication of this equation suggests the
existence of a critical length scale related to the upper
bound of the ISE. Similarly, the corresponding critical
load can also be determined.
The indentation data obtained from decagonal
quasicrystals AlCoCu (Murthy et al., 1999) and
AlCoNi (Liu et al., 2003) and the intermetallic
compound Mg
32
(AlZn)
49
(Mukhopadhyay et al., 2004)
have been analysed (Mukhopadhyay, 2005). The true
hardness and critical indentation size have been deter-
mined. Figure 6 shows the plot of the loadindentation
and hardnessindentation data from Vickers microin-
dentation experiments. Both the Meyers equation and
the energy balance model are t with the experimental
data satisfactorily (Fig. 6a) with a regression coefcient
.0
.
99. The true hardness (H
T
) was obtained from the
energy balance model in each case. The details of the
coefcients are summarised as follows
(a) For the decagonal quasicrystalline material
AlCoCu (Murthy et al., 1999)
Meyers law: P~0
:
00631d
1
:
9409
; energy model:
P~{0
:
00358z0
:
0096dz0
:
0049d
2
H
T
~1
:
8544|0
:
0049
N
mm
2
~9
:
08 GPa
(b) For the decagonal quasicrystal AlCoNi (Liu et al.,
2003)
Meyers law: P~0
:
0061d
1
:
9059
; energy model:
P~0
:
058{0
:
0011dz0
:
0044d
2
H
T
~1
:
8544|0
:
0044
N
mm
2
~8
:
16 GPa
(c) For the intermetallic compound Mg
32
(AlZn)
49
(Mukhopadhyay et al., 2004)
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Meyers law: P~0
:
0021d
1
:
9243
; energy model:
P~0
:
0021z0
:
0011dz0
:
0016d
2
H
T
~1
:
8544|0
:
0016
N
mm
2
~2
:
97 GPa
Now using equation (12), d* values are 70, 27 and
36 mm for the AlCoCu and AlCoNi quasicrystals and
for the Mg
32
(AlZn)
49
phase, respectively. This appears
to be reasonable and consistent with the trend of the
hardness plot with the indentation size, which can be
seen in Fig. 6b. The intersection between Meyers curve
of hardness and the true hardness line can clearly be
seen. The true hardnesses for the AlCoCu, AlCoNi and
Mg
32
(AlZn)
49
phases were found to be 9
.
01, 8
.
16 and
2
.
97 GPa, respectively, which also seem to be consistent.
The present analysis lends strong support to the
proposed approach for determining the critical indenta-
tion diagonal by involving both Meyers power law
equation and the energy balance model. Thus, the
normalised Meyers equation proposed here can give rise
to a better understanding of Meyers constant (K
m
) and
its exponent (n). These parameters combined with the
coefcient of the energy balance model can predict the
critical indentation size after which ISE does not exist.
Elastic/plastic deformation (EPD) model
Bull et al. (1989) proposed a quantitative model to
explain the ISE often observed in the hardness response
of hard brittle material which is based on mixed
elastic and plastic deformation, whereas the plastic
deformation occurs progressively in a discrete manner to
relieve stresses created by the elastic exure of the
surface at the edges of the deformation. During
unloading of the indenter, recovery of the elastic
increment of the deformation which proceeds each new
band of plastic deformation, results in an indentation
appearing smaller than expected, particularly as the
indentation size decreases to approach the scale of
plastic deformation band spacing. The model ts
observed experimental data well and the analysis of
hardness/size data in this way is shown to allow both for
a bulk hardness value and a characteristic deformation
band scale to be calculated for a given sample.
It is proposed that this model is applicable to hard
materials where the elastic deformation effects are
signicant and the yielding or cracking occurs at
intervals forming visible lines at an average spacing
characteristic of the material, the grain size and the
surface nish. As the contact area extends further under
the increasing load, yielding occurs at the outer edges,
where the tensile stresses of the surrounding elastic eld
combine with the stretching imposed by the sloping faces
of the indenter. It seems reasonable to assume the
average elastic recovery to be d and thus
d
m
~d
i
{d (17)
The hardness H
o
of the ideal plastic material where the
deformation is completely continuous is dened as
H
o
~kPd
{2
i
(18)
where k is a constant and P is load. For the proposed
system of non-continuous deformation, the above
equation may be used to derive H
m
from d
m
H
m
~kPd
{2
m
(19a)
Also equation (18) can be rewritten as
H
o
~kP d
m
zd
{2
(19b)
Dividing equation (19b) by equation (19a) gives (by
rearrangement)
H
m
~H
o
1z
d
d
m
_ _
2
(20)
At high load d
m
&d, H
m
tends to H
o
. At lower load, as d
is the more signicant fraction of d
m
, the measured
hardness will increase. The values of H
o
and d may be
determined by tting experimentally determined values
of H
m
and d
m
. Table 1 shows tting parameters.
Indentation-induced cracking
Li and Bradt (1991) proposed that during loading, the
test load is balanced by the total specimen resistance
composed of four components due to (i) friction at the
indenter/specimen facet interface (frictional component),
(ii) elastic deformation, (iii) plastic deformation, and (iv)
specimen cracking. According to these authors, fric-
tional and elastic effects lead to the normal ISE while
indentation cracking contributes to the apparent hard-
ness, H
A
, measured by a Vickers diamond indenter. It
may be written as
H
A
~l
1
K
1
P
d
2
_ _
zK
2
P
5=3
d
3
_ _
(21)
6 a Plot of variation of load versus indentation diagonal
obtained from Vickers microindentation experiment
(Mukhopadhyay et al., 2004) of Mg
32
(AlZn)
49
intermetal-
lic phase; b experimental hardness data, hardness
curve from Meyers equation and true hardness line
obtained from energy balance model, are plotted
against indentation diagonal (after Mukhopadhyay,
2005)
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t
d
where d is the indentation diagonal, l
1
, K
1
and K
2
are
constants. The constant K
2
depends on the applied load
P while K
1
is a geometrical conversion factor whose
value depends on the indenter geometry. For an ideally
plastic body, H
A
is equal to the rst part, whereas for
brittle solids, the second part is related to H
A
.
Peng et al. (2004) investigated the nanoindentation
hardness of a commercially available soda-lime glass, a
tetragonal ZrO
2
polycrystal and a hot-pressed Si
3
N
4
in
the peak load range from 7
.
5 to 500 mN and observed
the ISE. This was further analysed using Meyers law,
the HaysKendall approach, the proportional specimen
resistance (PSR) model, the elastic recovery model and
the modied PSR model. It was established that (i)
Meyers law provides a satisfactory description for the
experimental data for each material but cannot account
for the origin of ISE; (ii) the HaysKendall approach,
the elastic recovery model, the PSR model and modied
PSR model yield meaningless values of the parameters in
the corresponding equations. For each material, the true
hardness was also determined based on the PSR model,
the elastic recovery model and the modied PSR model,
respectively. It was found that the true hardness values
obtained from these different models are similar to each
other. This similarity can be attributed to the similarity
between the empirical equations employed in these
models. A similar type of analysis and conclusions was
also made by Sangwal (2000).
Friction and surface effects
Initial elastic resistance, which is characterised by a
sharp fall in hardness above a very small indentation size
has been identied in low load indentation tests of non-
metals. Such behaviour is consistent with a requirement
for a critical strain energy to trigger permanent
deformation or more probably cracking. Atkinson
(1995a,b) has shown that, in many cases, friction has
been responsible for a marked indentation size effect in
low load testing of some metals, and the magnitude of
the effect has been associated with stain hardening. This
intrinsic form of a size effect has been related to the
special deformation conditions of a plastic hinge at the
perimeter of the indentation. The principal factor in
the size effect in low load testing of Fe and Al has been
identied as due to friction. It is, therefore, reasonable to
suppose that the minimal size effects in these ultra micro
indentation tests could be a consequence of a particu-
larly low friction condition. It has been shown by Bobji
and Biswas (1999) that the surface roughness has a
substantial inuence on the nanohardness, irrespective
of whether the bulk and surface mechanical properties
are the same. Y. Wei et al. (2004) have studied the ISE
and attributed it to dislocation density theory as well as
some environmental effects such as indenter tip curva-
ture and surface roughness. Zhang et al. (2004) discussed
the role of plastic deformation of rough surfaces in the
size-dependent hardness. They proposed a bearing ratio
for nanoindentation of rough surfaces. During an
indentation, the work done can be separated into bulk
work and surface work. The surface work causes the
plastic deformation of an indented rough surface and
thus dissipates energy, which is necessary to form the
impression of the solids. The energy dissipation occur-
ring at the indented surface is among the factors that
cause the ISE at the micro/nanoscales. The surface effect
predominates when the indentation depth is shallow.
They have found good agreement between theoretical
and experimental results of the size-dependent hardness,
indicating that the surface effect plays an important role
in size-dependent hardness.
Gerberich et al. (2002) proposed that the ISE can be
linked to energy for the newly created surface and
the plastic strain energy dissipation and estimated the
surface work and volume work associated with the
indentation. Their analysis indicates that the total
surface work is given by the product of the contact area
and the surface energy. They observed that the ratio of
surface work to plastic volume work is nearly constant
for a wide range of shallow depths and decreases rapidly
with increasing depth of penetration and consequently
giving rise to ISE. Zhang and Xu (2002) have studied the
surface effects on nanoindentation and introduced an
apparent surface stress that represents the energy
dissipated per unit area of a solid surface in nanoinden-
tation tests.
Strain gradient plasticity: geometrically
necessary dislocations
Stelmashenko et al. (1993), De Guzman et al. (1993),
Fleck et al. (1994), Ma and Clarke (1995), Poole et al.
(1996), Nix and Gao (1998), McElhaney et al. (1998),
Gao et al. (1999a,b), Acharya and Bassani (2000) and
Huang et al. (2001) advocated strain gradient theory to
account for ISE. This theory assumes that the ow stress
is related to the statistically stored dislocations and
geometrically necessary dislocations (Fig. 7). According
to the strain gradient plasticity (SGP) model, the strain
gradient plays an important role in plastic deformation.
In the formulation of plasticity theory, the constitutive
law contains strain gradient as a variable and hence
there is an intrinsic length scale. This theory is based on
the observation that gradients of plastic shear result in
the storage of the so-called geometrically necessary
dislocations (GND), which affect the yield stress in a
7 Schematic diagram of geometrically necessary disloca-
tions created by rigid conical indenter; dislocation
structure is idealised as circular dislocation loops;
angle between surface of conical indenter and surface
plane of indented material is q, and indentation depth
is denoted by h (after Qui et al., 2001)
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d
similar manner as the common statistically stored
dislocations. The densities of the geometrically necessary
dislocations being proportional to the strain gradient
become appreciable, when the relevant size of indenta-
tion is small. The indentation at low load means that the
strain gradient is higher as the strain under the indent is
constant (for example 8% in Vickers geometry). The
strain gradient is directly proportional to the geome-
trically necessary dislocation. The shear stress t is
related to dislocation densities as follows
t~CGb
r
s
zr
g
_
(22a)
where G is the shear modulus, b is the magnitude of
Burgers vector and C is a constant taken to be 1/3 by
Ashby (1970). r
s
and r
g
are the densities of the
statistically stored dislocations and GNDs. Ma and
Clarke (1995) estimated the density of GNDs of the
indentation of diagonal length d as
r
g
&
4c
bd
(22b)
For metals, the hardness is three times the ow stress, so
the hardness can be approximately written in terms of
dislocation as
H&Gbr
s
1z
4c
r
s
bd
_ _1
2
(23a)
Obviously, when r
g
&r
s
, the above equation is dominant
to control the hardness and it explains the increase in
hardness as the load decreases. However, at higher load or
indentation diameter, the densities of GNDs may be
negligible compared to the statistically stored dislocations.
The above equations can be written in the following form,
so that it can be tested by tting the experimental data
H
2
~H
2
o
1z
a
d
_ _
(23b)
where a~
4c
r
s
b
is constant for a certain material. One can
plot H
2
versus 1/d and from the intercept, the size
independent plastic hardness can be obtained and from
the slope the dislocation densities can be determined.
Ma and Clarke (1995) have done this experiment on a
silver single crystal in order to test the strain gradient
plasticity theory. GNDs are the dislocations which are
necessary to accommodate the geometry of plastic
deformation. Such dislocations are required to create
the plastic indent in a microindentation process. These
dislocations act as obstacles to the statistically stored
dislocations and cause additional work hardening of the
material. It is also important to mention that Ma and
Clarke (1995) developed a geometrical scaling model for
ISE. They partitioned the applied indentation force into
the force on the at surfaces and the force over the edges
and nally derived size-dependent hardness for various
indentation tips. The tting of the experimental data
with this geometric scaling model appears to be as good
as with the strain gradient plasticity (SGP) model. For
simplicity, in the case of the SGP model, it can be
assumed that the indent is accommodated by the
circular loops of GNDs with the Burgers vectors normal
to the plane of the surface. The presence of these GNDs
causes storage of additional defects and increases the
deformation resistance by acting as obstacles to the
statistically stored dislocations.
Nix and Gao (1998) expressed the SGP model using
the GNDs and Taylors dislocation work hardening
theory, for a geometrically similar indenter, with the
size-dependent hardness in terms of indentation depth as
H
2
~H
o
1z
h
h
_
(24a)
where h* is a characteristic length that depends on the
indenter shape, the Burgers vector and statistically
stored dislocation. Using this model, Nix and Gao
(1998) developed a law for strain gradient plasticity,
which became the theoretical basis of the mechanism
based strain gradient (MSG) plasticity to explain the
ISE (Fig. 8). Qui et al. (2001) considered the intrinsic
lattice resistance (W
o
) which varies with lattice orienta-
tion and modied the above equation as
H
2
~3s
o
zH
o
1{
3s
0
H
0
_ _
2
z
h
(24b)
With this modied model, Qui et al. (2001) explained the
dependence of ISE on the crystalline orientation, which
was reported by Stelmashenko et al. (1993) in a W
crystal. Swadener et al. (2002) have modied the above
equation by adding a contact depth-dependent constant
H
1
as
H
2
~H
o
1z
h
h
_
zH
1
(24c)
where H
1
is a work hardening component representing
the increase in hardness from the onset of yielding to an
effective strain. The modied equation was employed for
studying ISE in NaCl and LiF single crystals. Elmustafa
and Stone (2002, 2003) have added a contact depth-
dependent term H
f
(which is similar to H
1
) representing
the hardening mechanism other than dislocations. They
have observed that for indents shallower than 150 nm,
8 Microindentation hardness data for single-crystal and
polycrystalline copper, as well as for single crystal sil-
ver; h is indentation depth, H is microindentation hard-
ness, and H
0
is indentation hardness for large depths
of indentation; NixGao relation is also shown for
each set of experimental data, and it agrees well with
the microindentation hardness data (after Qui et al.,
2001)
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the slope of the plot decreased abruptly by a factor of
10 in comparison with the microhardness and deep
nanoindentation data, resulting a bilinear behaviour. As
more and more experimental results were reported, it
was found that the equation could not satisfactorily t
all the experimental results (Mukhopadhyay et al.,
2005). There are attempts to add an extra term to take
care of extra terms due to hardening or softening
depending on the material (Fig. 9).
Dislocation mechanics: classical
In the MSG model, Gao et al. (1999a) extended Taylors
dislocation model to include the strain gradient plasti-
city. In Taylors dislocation model, the dislocations are
considered as statistically stored. As the size of the
indent becomes smaller, the gradient becomes steeper.
Taylors dislocation hardening model is modied to
accommodate GNDs. Gao et al. (1999a,b) indicated that
the strain gradient plasticity is applicable between 0
.
1
and 10 mm. When the indent is less than 0
.
1 mm,
dislocation mechanics dominates. Several workers have
extended the classical theory of dislocations without
invoking the strain gradient plasticity theory to explain
the ISE and the RISE (Mott, 1956; Gane, 1970; Chen
and Hendrickson, 1973; Upit and Varchenya, 1973;
Sargent, 1986; Vitovec, 1986; Sangwal, 1989; Lim and
Chaudhuri, 1999; Sangwal, 2000). In the case of an
indentation experiment with sharp indenter, stresses
always build up under an indenter with a pointed tip
sufcient for homogeneous nucleation of dislocation in a
perfect crystal. Therefore a change in the length of
dislocation sources and in the concentration of defects in
stressed volumes of different size cannot play the
determining role compared to the conditions of disloca-
tion movement under the indenter. Upit and Varchenya
(1973) suggested that the peculiarity in the dislocation
movement in the case of indentation is that dislocation
loops nucleated under the indenter near the surface
expand and propagate into the crystal thereby causing
the ISE. Chen and Hendrickson (1973) studied the
indentation of Ag single crystals with a wide range of
loads and found both ISE and RISE below a certain
load. They observed the distinct differences in terms of
appearances of dislocation rosettes around the indents.
They concluded that the interaction of the dislocation
pattern is different and can be held responsible for ISE
and RISE. Lim and Chaudhuri (1999) made an
experimental investigation of nanohardness of the
polycrystalline work-hardened and annealed oxygen
free copper (OFC) for different indenter loads. The
work-hardened sample shows a three-stage behaviour
once H decreases (I) and increases (II) and then
decreases again (III). This phenomenon cannot be
obviously explained by the strain gradient plasticity
model. A three-stage qualitative model has been
proposed. In stage I at low penetration depth
(150 nm) dislocation loops are nucleated at a relatively
high shear stress value of about (G/75). According to this
model, at relatively low penetration depths, the nano-
hardness reects the shear stress value required for
nucleation and expansion of dislocation loops. Also in
this stage, the earlier dislocation densities have little
effect on nanohardness values. The indenter penetration
increases and consequently the numbers and diameters
of dislocation loops become signicant. This is the
beginning of the second stage, when the nanohardness of
the work-hardened material may even increase with
increasing indenter penetration owing to dislocation
interactions. For still larger indentations, the third stage
begins when a sufciently large number of dislocations is
created around the indentation. After the nucleation of
initial dislocation loops under the indenter tip, as the
load is increased, more and more dislocation loops will
be created, the diameter of which correspond to the
current size of the indentation contact. Then to increase
the indentation size further, sufciently high shear stress
9 Plot of experimental H versus d (mm) data obtained from microindentation experiment, along with those predicted
based on SGP and modied SGP model including the extra softening term; the modied SGP model shows a better
agreement compared to the SGP model (after Mukhopadhyay et al., 2005)
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values will be required to cause the dislocation loops to
grow in size and to glide. It was suggested that the shear
stress required to propagate a dislocation loop in copper
is related to its radius L by
t~
Gb
L
(25)
where G544 GPa is the shear modulus of copper and
b50
.
225 nm is the Burgers vector of dislocations.
Therefore with increasing radii of the dislocation loops
and with increasing indenter depth, the shear stress
required to glide them will decrease and consequently,
hardness will decrease with load and then nally will be
independent of load at larger load.
It can be indicated that it is difcult to explain
maxima due to the RISE using the PSR, elastic/plastic
deformation (EPD) and SGP models. It is understood
that the average hardness increases with the dislocation
density. The appearance of maxima suggests that the
indentation process is intimately connected with nuclea-
tion and motion of dislocations. The inherent defect
structures would obviously act as obstacles for the
motion of the defects produced by nucleation. It is clear
from the literature that the RISE occurs only in the
single crystals undergoing plastic deformation.
Therefore, it may be concluded that the RISE occurs
only in materials where plastic deformation is dominant.
It is well known that in the initial stage (i.e. at low loads
or strain), plastic deformation of crystals mainly
involves the nucleation of dislocations in a particular
slip system, but with increasing strain, dislocation
multiplication (by processes like cross slip and activity
of Frank read source) takes place. The latter process is
accompanied by work hardening. The RISE is also
explained based on the effects of vibration and indenter
bluntness at low load (Westbrook, 1967; Hanneman and
Westbrook, 1986), the applied energy loss as a result of
specimen chipping around the indentation (Banerjee and
Feltham, 1974; Feltham and Banerjee, 1992) and the
generation of radial or median cracks (Li and Bradt,
1996).
Sangwal (2000) suggested that at low loads, when only
one slip system is active, active parallel glide planes are
few. Therefore, the nucleation of dislocations rapidly
propagates into the material without substantially
experiencing mutual interaction stress between them.
However, with increase in load, when the number of
parallel glide planes is increased, the motion of
dislocations gliding along them slows down due to the
mutual interaction stresses between dislocations. This
leads to a slow increase in indentation depth with
increasing indentation pressure. Consequently, the
increase in H with h steadily becomes weaker until H
attains a steady value after some particular value of
load. The RISE phenomena essentially take place, which
readily undergo plastic deformation. It appears that the
RISE can be caused by (i) the relative predominance of
nucleation and multiplication of dislocations and (ii) the
relative predominance of the activity of either two sets of
slip planes of particular slip systems or two slip systems
below and above a particular load.
Mechanics of indentation
Among the several theoretical models, the three most
extensively discussed models will be highlighted here.
These are (i) the elastic indentation model, (ii) the rigid
perfectly plastic model and (iii) the spherical cavity
expansion model. The behaviour of these three solids
can be realised from the stressstrain diagram in Fig. 10.
Elastic model
The elastic indentation model was originally developed
by Hertz (1882), Boussinesq (1885) and Sneddon (1965)
independently. In this model, it is assumed that the
indenter is rigid and the material of the specimen
satises the linear elasticity theories (Fig. 11). The
pressure distribution, p(r) for the cone can be expressed
as
p(r)~
E cot h
2(1{n
2
)
cosh
{1
(a=r) (26a)
where E is the elastic modulus, v is Poissons ratio, h is
the semiapical angle of the cone, and a is indentation
diameter. The mean contact pressure can be written as
p
m
~H~
E cot h
2(1{n
2
)
(26b)
The solution for other wedge, sphere and at-end
solutions can be found in the work of Sneddon (1965)
10 Stressstrain diagram for a perfectly plastic, b elasticplastic, c real elasticplastic solids
11 Indentation of ideally elastic solids by conical indenter
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and Timoshenko and Goodier (1951). With the elastic
rubber, the indentation pressure is a direct measure of the
elastic properties of the material. One can see that the
hardness is independent of indentation size. However, for
a spherical indenter, H will be a function of the load and
the radius of the curvature R of the sphere
H~
P
1=3
p
4E
3R(1{n
2
_ _
2=3
(26c)
It has been assumed that friction and the elastic
deformation of the indenter are negligible. For elastic
material, the indentation disappears after unloading.
Therefore, the depth can be measured from the
instrumented hardness testing equipment so that the
area can be found from the depth measurement.
Rigid perfectly plastic model (slip-line field
approach)
This model is based on the slip-line eld theory
advocated by Prandtl (1920) and later generalised by
Hill et al. (1947). In this model, the material is
considered as rigid perfectly plastic, i.e. no plastic
deformation occurs until a stress Y is reached. The
hardness obtained by this theory is the upper bound of
the hardness. These solutions successfully predict the
hardness for materials with high values of E/Y, using
sharp indenters, but not so successfully for materials
with low values of E/Y or for blunt indenters. The
pressure p across the punch is uniform and has the value
p~H~cY~2k 1z
p
2
_ _
(27)
Thus H52
.
6Y (Tresca criterion) and H53Y (von Mises
criterion). In general, one can write H5cY, where c is
the appropriate constraint factor which will depend on
the geometry of the indenter and the interfacial friction.
The slip-line eld for a two-dimensional wedge of
semiapical angle h is shown in Fig. 12 and the pressure
across the face of the indenter for frictionless indenta-
tions is p5H52k(1za) where cos(2ha)5cos a/
(1zsin a). The slip-line eld approach to plastic
deformation has been widely applied to metal forming,
metal working and indentation hardness. It was pointed
out by Tabor (1986) that deformation patterns predicted
by slip-line theory were not observed in indentation
experiments in metals. However, it was later recognised
that the mode of deformation observed by Tabor (1986)
closely agrees with that proposed by Mulhearn (1959)
and Samuels and Mulhearn (1957) as compression mode
(Fig. 13). This is perhaps because the metals are not
rigid but elasticplastic materials.
Spherical cavity expansion model
The spherical cavity model (Fig. 13) was rst advocated
by Bishop et al. (1945) and later developed by Marsh
(1964), Hirst and Howse (1969) and Johnson (1970).
Among all these, Johnsons analysis has been the most
recognised analysis for indentation of elasticplastic
solids. The results are reasonably close to the experi-
mental observations for materials with either very high or
very lowvalues of E/Y. An improved analysis comes from
Johnson (1970). The radial expansion model is the
bottom half of the spherical cavity and therefore does
not provide for any piling up of any displaced material
outside the indentation. Evidently, the volume of the
indentation is ultimately taken up in the elastic hinter-
land, so that the shape of the indenter must be involved.
For a cone of semiapical angle h, the critical parameter
now becomes (E/Y)cot h, while for a spherical indenter,
the corresponding quantity is (E/Y)(a/R). The nal
relation for cones or pyramids is then
H
Y
~
2
3
1zln
E cot h
3Y
_ _
(28)
while, for spherical indenters, cot h is replaced by a/R. This
treatment assumes that the material has a constant yield
stress, Y, and that there is no work hardening produced by
the indentation process itself. According to Hills original
solution, the pressure in the cavity when the plasticelastic
boundary is at a distance c from the centre is
P
Y
~
2
3
z2 ln
c
a
(29)
This implies that the elasticplastic boundary coincides
with the boundary of the cavity itself (c5a) at P52/3Y,
and below this contact pressure, the analysis fails and no
plastic ow can occur. However, there is no case of plastic
indentation occurring in any system for an indentation
pressure less than Y. On the other hand, in the region
where p53Y, equation (27) shows that c53
.
2 and it must
be assumed that the elastic yielding of the hinterland no
longer inuences the plastic ow of the material. The
contact pressure nowcorresponds to the classic theory for
a rigid plastic solid. However, there is nothing in the
expanding cavity model to indicate that the indentation
pressure has an upper limit of 3Y. As noted by Tabor,
the expanding cavity model is a helpful and fairly
realistic description of the indentation process in the
12 Slip-line eld solution for indentation of rigid plastic solid by frictionless wedge of semiapical angle h
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compression or radial ow mode. Attempts have been
made to improve it to give better numerical agreement
with experiment. A more satisfactory approach involves
nite element analysis and the newer technique of
boundary element analysis, but even these techniques
have limitations imposed by the theoretical assumptions
involved.
Elastic and perfectly plastic model
Recently, Yu and Blanchard (1996) developed an
analytical model of hardness for four major indentation
tests. They have determined the analytical relationship
for calculating hardness from the uniaxial material
properties and indenter geometry for a wide variety of
elastic and plastic materials. The models are presented
here in order to understand the mechanics of the
indentation process. These models provide a simple
but powerful method for relating hardness from one
type of hardness test with that of a different test, or
evaluating uniaxial properties from hardness measure-
ments. For example, the hardness of a conical indenta-
tion can be directly calculated by the following
procedure if the uniaxial properties of the material and
the angle b of the indenter are known
H~
E tan b
2(1{n
2
)
tanh
2(1{n
2
)YC
b
E tan b
_ _
(30a)
where C
b
~
2
3
p
(2
:
845{2
:
3757|10
{2
b), and 0u,b(
37
.
5u. To evaluate the uniaxial properties of a material
from the hardness measurements, the yield stress can be
evaluated from the following relation
Y~
E tan b
2(1{n
2
)C
b
tanh
{1
2(1{n
2
)H
E tan b
(30b)
Determination of elastoplastic properties:
relationship between hardness and elastic
modulus
The analysis of loadindentation data following
the technique of Oliver and Pharr (1992) has been
extensively discussed by Bhushan and Li (2003) and
Oliver and Pharr (2004) and therefore it will not be
discussed here further. Some other approaches to
analysing the loadindentation data will be discussed.
It is important to mention that still the problem of
actual contact area in case pile-up and sinking-in has not
yet been sorted out. In order to obtain a more accurate
value of hardness and Youngs modulus, there are
suggestions to use the actual contact area by imaging the
indents using scanning probe microscopy (Lim and
Chaudhuri, 1999). The total work (W
tot
) of indentation
and the reversible work W
p
of indentation, dened,
respectively, as the area under the loading curve and that
between the loading and unloading curves (Fig. 14),
have also been used for materials characterisation
(Sakai, 1993; Hainsworth et al., 1996; Rother, 1995;
Rother and Dietrich, 1994; Cheng and Cheng, 1998e,
1999; Faulkner et al., 1998; Giannakopoulos and
Suresh, 1999). It is therefore relevant to review the
work investigating the relationships between these
different materials properties and the parameters obtained
from the indentation experiments. Giannakopoulos and
Suresh (1999) discussed three-dimensional nite element
simulations of elastoplastic indentation along with
Vickers and Berkovich indentation experiments and
provided the following results (assuming the loaddepth
relation as P5Ch
2
, where C is the indentation curvature)
C~
P
h
2
~M
1
s
0
:
29
1z
s
y
s
0
:
29
_ _
M
2
zln (
E
s
y
)
_ _
,
for 0
:
5
p
av
s
y
3
:
0
(31)
In the above equation, s
y
and s
0
.
29
are the yield strength
and stress corresponding to the characteristic plastic
strain of 0
.
29 for the indented material in uniaxial
compression. The constants M
1
57
.
143 and M
2
521 for
the Vickers pyramid indenter with an included tip angle
of 136u. The corresponding values for the Berkovich
indenter are M56
.
618 and M
2
520
.
875 with an included
13 Compression mechanism of indentation proposed by Mulhearn (1959) showing elasticplastic boundary and defor-
mation resembling expansion of spherical cavity into elasticplastic solid by internal hydrostatic pressure
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tip angle of 130
.
6u. The circular conical indenter also
follows the same results as the Vickers or Berkovich
depending on the apex angle of the cone. If P
av
/W
y
falls
outside the bounds of the equation, the indenter response
is either elastic or elasticperfectly plastic. By accounting
for the effects of strain hardening on pile-up and sinking-
in and on the true contact area through three-dimensional
simulations, the following relationship between the A
max
and h
max
has been derived for elastoplastic materials
A
max
h
2
~9
:
96{12
:
64(1{S)z105
:
42(1{S)
2
{
229
:
57(1{S)
3
z157
:
67(1{S)
4
, with S~
P
av
E
(32)
This equation is a polynomial t to the computationally
determined values of A
max
/h
2
. The effective Youngs
modulus of the indenterspecimen system is dened as
E
~
1{n
2
E
z
1{n
2
in
E
in
_ _
{1
~
1
c

A
max
p
dP
dh
_ _
(33)
The subscripts in (equation (33)) represent properties
of the indenter and dP/dh is the slope of the Ph curve of
the initial stages of unloading from P
max
. The constant
c*51
.
142 for the Vickers pyramid indenter, 1
.
167 for the
Berkovich indenter and 1
.
128 for the circular indenter of
any included apex angle. The ratio of the penetration h
r
upon complete unloading to the maximum penetration
depth, h
max
, before unloading, is indicative of the extent
of plastic deformation and strain hardening such that
s
0
:
29
{s
y
0
:
29E
~1{0
:
142
h
r
h
max
{0
:
957
h
r
h
max
_ _
2
(34)
Elastoplastic nite element analysis of the sharp
indenter, also reveals that
h
r
h
max
~1{d
p
av
E
(35)
where d*55 for a Vickers pyramid indenter and
d*54
.
678 for the Berkovich indenter; the conical
indenter results are similar to the Vickers or Berkovich
indenters depending on the included apex angle. The
step-by-step method has been suggested extracting
the materials properties. Following this approach,
Mukhopadhyay et al. (2001) determined the Youngs
modulus of quasicrystalline materials which matches
well the data obtained by the ultrasonic technique.
Energy-based approaches to the indentation of brittle
materials are proposed by Sakai (1993), analysing the
instrumented load indentation data. The hysteresis loop
energy, U
r
which is dissipated during the indentation
loadingunloading cycle is related to the true hardness H,
apparent hardness H
A
and the work of indentation c
1
.
The true hardness has its energy-derived meaning of the
irreversible energy consumption to create a unit volume
of indentation of ideally plastic materials. The relation-
ship between U
r
and the three half powers of indentation
load P
3/2
and between U
r
and the volume of the
indentation impression V
I
are used to separate the plastic
contribution from the complicated plastic/elastic surface
deformation processes in the indentation tests. The linear
relationship of U
r
versus P
3/2
provides an important
experimental technique for determination of true hard-
ness H of the brittle materials. The linear relationship of
U
r
versus V
1
is available to the experimental determina-
tion of c
1
. The relationship has been developed as follows
U
r
~
1
3
1
a
0
tan
2
y
_ _
1
H
p P
3=2
(36)
which enables one to evaluate the true hardness of the
brittle materials from an experimental relationship.
Theoretical predictions obtained through this formalism
were experimentally conrmed. The energy-based
approach and its application to brittle materials can
provide signicant and potential directions for studies of
the loadindentation size effect, machining-induced
damage, brittle/ductile transition behaviour at elevated
temperatures of ceramic materials, as well as of the
dislocation process and plasticity of ceramic single
crystals. H
v
Vickers hardness with Meyer denition
(indentation load divided by the projected area of
indentation impression), j ratio of residual indentation
depth and the depth at maximum load, nite element
analysis for elastoplastic Vickers indentation are con-
ducted in which the effect of strain hardening on
indentation behaviour is intensively examined. A novel
procedure of graphical superposition is proposed to
determine the representative yield stress, Y
R
. It is
conrmed that the concept of Y
R
applied to elastic
fully plastic solids is sufcient to describe the indenta-
tion behaviour of elastoplastic solids with strain hard-
ening. However, Tabors representative strain (8%) at
which Y
R
is described is only applicable to elastoplastic
solids with their ratio of Youngs modulus E to yield
ratio Y (E/Y) ranging from about 400 to 1000. The true
hardness H as a measure of plasticity is estimated from
the Meyer hardness H
M
and then successfully related to
yield stress Y and the strain-hardening modulus E
p
, as
well as Y
R
. True hardnesses obtained from this
formalism have been displayed for materials in
Table 3. The true hardness is always found to be much
higher than the conventional hardness, especially in the
14 Illustration of a conical indentation and b loading and
unloading curves, where W
tot
is total work, W
p
is irre-
versible work and W
e
is reversible work: W
tot
5
W
p
zW
e
(after Cheng et al., 2002)
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case of brittle materials. However, this approach has yet
to be adopted in real practice.
Using a scaling approach to the indentation problems,
an approximate relationship between the ratio of
hardness to elastic modulus and the ratio of irreversible
work to total work has been proposed. The work of
indentation and the geometry of indentation can be
referred in Fig. 14 (Cheng and Cheng, 1998ae; Cheng
et al., 2002). The ratio of hardness and Youngs modulus
can be obtained from measuring the work of indenta-
tion. Together with a well known relationship between
the elastic modulus, initial unloading slope and contact
area, a new method is then suggested for estimating the
hardness and the modulus of a solid using instrumented
indentation with conical or pyramidal indenters. In the
following, the relationships are shown
dF
dh
_ _
h~h
m
~
2
p
p E

A
p
(37a)
H
E
2
~
4
p
F
(dF=dh)
2
(37b)
H~
p
4
P
2
h
W
tot
{W
u
W
tot
_ _
dF=dh
2
F
(37c)
E
~
p
4
P
h
W
tot
{W
u
W
tot
_ _
dF=dh
2
F
(37d)
where P
h
W
tot
{W
u
W
tot
_ _
is a dimensionless function. Several
experimental data points from the literature using
Berkovich diamond indenters on Cu, W, Al, fused silica
and sapphire are also shown to follow this close
relationship. The nite elastic constants of the diamond
indenter are taken into account using the reduced
modulus. It has been further emphasised that further
experiments and modelling efforts will ascertain the
accuracy of this proposed method.
Mencik and Swain (1994) have explored the relation-
ship between W
p
/W
tot
and h
f
/h
m
. By assuming that
respective loading and unloading curves are given by
F~ah
m
and F~b(h{h
f
)
l
, where a and b are functions
of materials properties and indenter geometry, a
relationship between W
p
/W
tot
and h
f
/h
m
is then given by
W
p
W
tot
~
mz1
lz1
h
f
h
m
{
m{l
lz1
(38)
This discussion obviously suggests that a general
relationship exists between W
p
/W
tot
and h
f
/h
m
and this
relationship is explicitly independent of indenter geo-
metry. This relationship is also explicitly independent of
the details of the material properties and the stress and
distribution with similar indenters.
Using dimensional analysis and nite element calcula-
tions, several relationships that relate the features of
indentation loading and unloading curves to the hard-
ness, elastic modulus and work of indentation are
proposed for elasticplastic solids. These relationships
provide new insights into indentation measurements
(Cheng et al., 2002). Earlier, Lawn and Howes (1981)
studied the elastic recovery effect in the indentation of
several ceramic materials and steels. By assuming that
the respective loading and unloading curves are given by
F~ah
2
and F~B(h
2
{h
2
f
) where A and B are functions
of materials properties and indenter geometry, a
relationship between W
p
/W
tot
and h
f
/h
m
was obtained
F~B(h
2
{h
2
f
) (39)
The results from this equation are plotted in Fig. 15.
The nite element calculations and equation agree well
with each other. Finite element calculations reveal the
relationships between nal depth, hardness and elastic
modulus and they are shown in Fig. 16. It is obvious
that an approximately linear function exists between h
f
/
h
m
and H/E* for each indenter angle. The relationships
can be summarised as
h
f
h
m
~1{l
H
E
, where l~1
:
50 tan (h)z0
:
327
for 60
0
h80
0
(40)
Table 2 Fitting parameters for observed scale dependence of hardness for various ceramic materials
Material H
o
, kg mm
22
d, mm q, kg mm
22
n
Sapphire (1012) 2129 1
.
34 4265 1
.
81
Deranox (alumina pc) 1642 2
.
05 3839 1
.
79
MgO (001) (sc) 791 2
.
58 2374 1
.
73
Silicon (001) (pc) 699 3
.
97 3004 1
.
65
SiC (001) (sc) 2513 1
.
92 6972 1
.
72
REFEL SiC (pc) 2461 1
.
10 3764 1
.
90
ZrO
2
1216 1
.
58 2374 1
.
83
Parameters q and n refer to the usual ISE model of eqn. (Meyers law) while H
o
and d are derived from the new model described by
equation (18). It should be noted that while q in the ISE model is hardness value standardised at unit indentation size, H
o
in the new
model is large-scale macroscopic hardness (sc5single crystal, pc5polycrystal) (Bull et al., 1989).
Table 3 Density, elastic modulus and hardness parameters (Sakai, 1993)
Material
Bulk density,
g cm
3
E, GPa H
V
, GPa
True hardness
H, GPa
Work of indentation
c, GPa
Apparent hardness
H
A
, GPa
Al 2
.
71 74
.
7 0
.
39 0
.
40 0
.
61 0
.
65
Cu 8
.
90 139 1
.
01 1
.
05 1
.
40 1
.
56
MgO 3
.
52 309 4
.
91 7
.
46 4
.
90 6
.
81
Si
3
N
4
3
.
22 331 15
.
1 19
.
7 9
.
30 17
.
2
SiC 3
.
22 448 23
.
7 54
.
0 9
.
70 22
.
1
Glassy carbon 1
.
50 29
.
9 202 0
.
25 2
.
50
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It is important to point out that Marx and Blake (1997)
have shown a linear relationship for conical indentation
with a semicone angle of 70
.
3u, in elasticplastic solids
with bilinear uniaxial stressstrain relationships. Cheng
and Cheng (1998e, 1999) have shown a similar relation-
ship for conical indentation in elasticplastic solids with
power law work hardening for a particular semicone
angle of 68u. Several other workers have proposed
models that link the two quantities (Lawn and Howes,
1981; Sakai, 1993). In these models, the degrees of
piling-up and sinking-in of surface proles were treated
as adjustable parameters. The relationships between h
f
/
h
m
and H/E* are inuenced by these parameters. Lawn
and Howes (1981) proposed the following relationship
h
f
h
n
_ _
2
~1{ 2
c
E
c
H
_ _
tan h
_ _
H
E
(41)
where c
E
and c
H
are parameters that are affected by the
degree of surface sinking-in or piling-up. A reasonable
agreement between the LawnHowes model and the
nite element results was found when c
E/
c
H
is about
1
.
18. However, the above equation does not predict the
approximately linear relationship. Future research is
needed to understand better the relationship between h
f
/
h
m
and H/E*. From the studies of scaling and nite
element analysis, Cheng et al. (2002) have obtained the
following relation, using W
e
5W
tot
W
p
H
E
~k
W
e
W
tot
where k~
1
l(1zc)
for 60
0
h80
0
(42)
However, the value for k obtained using this expression
cannot be applied to sharp cones (45u) owing to the
validity range of l. From this relationship, the ratio of
H/E* can be obtained readily by measuring the work
of indentation to obtain W
e
/W
tot
. Furthermore, since
the ratio of H/E*
2
can be obtained from the initial
slopes of the unloading curves (Joslin and Oliver,
1990; Hainsworth et al., 1996; Cheng and Cheng,
1998a,b,c,d,e), the values of H and E* can, in principle,
be obtained from the work of indentation and the initial
unloading slope.
Indentation studies of quasicrystals
Quasicrystalline phases (QC) of either icosahedral or
decagonal symmetry share an homologous brittle-to-
ductile transition temperature (BDT) of T/T
m
,0
.
7 (T
m
melting temperature) (Bresson, 1994) with the majority
of crystalline intermetallic compounds (Fleischer, 1994;
Sauthoff, 1995). This suggests that diffusion processes
are strongly involved in plastic deformation. It also
means that nucleation and movement of cracks should
become a predominant mechanism in most of the QC
phases when subjected to shear stress at room tempera-
ture. However, due to the small ratio of indent-
to-sample diameter, indentation experiments are in
fact performed under conning pressure conditions. It
has been known for a long time that conning pres-
sure techniques, where uniaxial stress states are
16 Relationship between h
f
5h
m
and H5E* (after Cheng
et al., 2002)
15 Relationship between h
f
5h
m
and W
p
5W
tot
(after Cheng et al., 2002)
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superimposed by hydrostatic pressure, may well shift
the BDT of crystalline materials down to even room
temperature by suppressing crack growth (e.g. Castaing
et al., 1981; Francois et al., 1988; Androussi et al.,
1989). Indeed, this principle also seems to work
with QC. Recently, a permanent macroscopic plastic
strain of almost 20% has been achieved by Fikar
et al. (2001) after deformation of poly-quasicrystalline
i-Al
63
.
5
Cu
24
.
0
Fe
12
.
5
under isostatic pressure of 5 GPa
and at a strain rate of 5?10 s
21
at 300 K. Importantly,
their TEM investigation of the microstructure did not
reveal signicant differences between room temperature/
high conning pressure and high temperature/low
conning pressure specimens. The microstructure was
rather found to be characterised by either a tweed
like or a platelet like contrast and isolated dislocations.
The platelets could be shown to correspond to two
pentagonal approximant phases (Fikar et al., 2001).
Indication for phase transitions as the vehicle of
permanent deformation at room temperature were also
reported by other workers: For example, Wu et al.
(2000) and Dong et al. (2001) found a transition in
i-Al
62
Cu
25
.
5
Fe
12
.
5
to a bcc structure in the region
below scratches, whereas Kang and Dubois (1992a)
observed transitions under uniaxial compression of
i-Al
63
.
5
Cu
24
.
5
Fe
12
and d-Al
63
Cu
17
.
5
Co
17
.
5
Si
2
.
Another mechanism of plastic deformation at room
temperature has been proposed by Wollgarten and Saka
(1997) and Wollgarten et al. (1999). Examining the area
below a Vickers indent in i-AlPdMn by TEM, they
concluded, contrary to Fikar et al. (2001), that a poly-
grained material with grain sizes starting from 10 nm up
to 500 nm had been formed and deformation occurred
via grain boundary sliding. At about 200uC, dislocation
generation was found. However, the mechanism of this
fragmentation process was not specied.
Elastic properties
The reduced modulus E
r
has been derived for various
QCs from a number of indentation tests using the
nanoindenter (Table 4). Examples of corresponding F(h)
curves are displayed in Fig. 17. Aluminium-based alloys
exhibit higher moduli than others. The surprisingly
small modulus of dodecagonal NbTaTe is of the same
order of magnitude as elemental tellurium (47
.
1 GPa,
Brandes and Brook, 1992) rather than of tantalum or
niobium (185
.
7 GPa or 104
.
9 GPa, Brandes and Brook,
1992). Apart from the small effect in d-AlCuCoSi, no
pronounced elastic anisotropy has been found in any of
the QC investigated in agreement with the conclusions
of Chernikov et al. (1998), Reynolds et al. (1990) and
Spoor and Maynard (2001). Note that E
r
increases when
the contact depth h
c
approaches the surface region
(Fig. 18). It becomes fairly constant for contact depths
.200 nm. This obvious surface inuence may arise
from intrinsic as well as from extrinsic causes and is still
not understood. Future databases will have to consider
that.
Hardness: indentation depth
Despite its physical foundation, Meyer hardness H is not
a simple material property. Figure 19 displays values for
H(F) over four orders of magnitude of the load F, which
show that hardness more than doubles when lowering
the load by a factor of 10. Though this phenomenon has
principally been known for quite a long time (cf. Mott,
1956), hardness numbers are even today taken as
characteristic of the material, at least when specifying
the (large) load and the shape of the indenter applied.
Despite the problems connected with the signicance of
hardness values as a material property, the more
pragmatic view is taken to use hardness as a quantity
for comparison and as a feature which at sufciently
low loads will enable elementary processes of plastic
deformation to be detected. For the sake of comparison
with other data, microhardness results will rst be
presented (load 1 N) along with nanohardness data
(load 0
.
1 mN) in Table 5. Al-based QC proved harder
than Zn-based. The nanohardness is considerably higher
than the microhardness (see below). Anisotropies are
generally small, but reproducible. Unresolved systematic
deviations seem to prevent results of different authors
from coincidence.
The increase in hardness for FR0 or hR0 has become
known as a (positive) indentation size effect (ISE) (cf.
Fig. 19). It has been reported to occur in a wide range of
materials (e.g. Si, TiB
2
(Brookes, 1983), MgO (Ren et al.,
2002), Al (Atkinson, 1995a,b) and has been attributed to
several mechanisms such as, e.g. elastic recovery (Mott,
1956), indenterspecimen friction (Li et al., 1993) or
geometrically necessary dislocations (Fleck et al., 1994).
ISE and its RISE are discussed in more detail. The latter
Table 4 Reduced modulus E
r
at 300 K as derived from indentation experiments on surfaces with normal parallel to
rotation axes indicated
QC E
r
, GPa* E, GPa
d-AlCoCuSi 16415 {10} 87 (poly QC) (Kang and Dubois, 1992b)
17515 {2}
d-AlCoNi 19515 {2} 195 (Chernikov et al., 1998), 177 {10} (Li et al., 2004)
i-AlCuFe (poly QC) 18020 172 (Vanderwal et al., 1992), 168 (Tanaka et al., 1996),
140
.
2 (Fleury et al., 2001), 131 (Lee et al., 2001), 61268 (Kang and Dubois, 1992b)
i-AlMnPd 19012 {5} 182 (Tanaka et al., 1996)
200 (Yokoyama et al., 1993)
i-DyMgZn 12815 {5}
i-HoMgZn 13615 {5}
i-MgYZn 12515 {5} 62 (Edagawa et al., 1998)
126 (Sterzel et al., 2000)
dd-NbTaTe 3510
*Paufler and Wolf (2003).
{2}, {5} {10}, surface normal || to two-, five- or 10-fold symmetry axis.
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model leads to the following form of the depth
dependence of hardness H
H~H
0
1z
h
h
c
(43)
where h
c
is the contact depth, H
0
5H(h
c
R)527
1/2
Gba
(r
s
)
1/2
and h*5(81/2)b a
2
tan
2
q (G/H
0
)
2
, G is the shear
modulus, b the Burgers vector modulus, r
s
density of
statistically stored dislocations, q the angle between the
surface of the indenter and the surface of the specimen, a
constant <0
.
5, and h* the length that characterises the
depth dependence of the hardness (Nix and Gao, 1998).
There is certainly a lower boundary of validity of
equation (43) due to the atomic structure, i.e. h
c
.1 nm.
An upper limit for h
c
will be due to the formation of
cracks, etc., hence dependent on both the material and
the testing conditions. Equation (43) may be rewritten
as
H~H
2
0
z(40
:
5ba
2
tan
2
qG
2
=h
c
)
1=2
(44)
From measurements of H(h
c
), parameters of equa-
tion (44) may be obtained. Fitting contact depths in the
range 100 nm,h
c
,250 nm to equation (44), Pauer and
Wolf (2003) found H
0
511
.
3 GPa and h*540
.
8 nm for
unimplanted d-AlCoNi (Fig. 20). If b5b
||
50
.
377 nm
(Yan et al., 1994; Kupsch et al., 2001), then a shear
modulus G547
.
8 GPa results (with a50
.
5 and q537
.
7u).
These values are consistent with those known from other
authors. The model of geometrically necessary disloca-
tions ts well for contact depths h
c
.h*. At smaller h
c
values (i.e. higher dislocation densities), H increases more
slowly than predicted, contrary to metals (Lorenz, 2001).
Here, the validity of the Taylor model may become
questionable apart from probable surface inuences.
18 Reduced Youngs modulus of dodecagonal
(Nb
0
.
15
Ta
0
.
85
)
181
Te
112
at room temperature as a func-
tion of contact depth h
c
; different point sets corre-
spond to different sites (after Pauer and Wolf, 2003)
19 Meyer hardness versus load (indentation size effect ISE)
for i-Al
70
Pd
21
Mn
9
and i-Y
10
Mg
30
Zn
6
0 at room tempera-
ture as derived from Vickers (F.10 mN) and Berkovich
(F,10 mN) indentation tests; sample surface perpendi-
cular to vefold symmetry axis (Wolf et al., 2001)
17 F(h) curves obtained with Berkovich indenter for QC based on MgZn with Y or rare-earths as third component; sur-
face normal vefold; reduced Youngs moduli were derived from the unloading parts (after Pauer and Wolf, 2003)
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Hardness H versus contact depth h
c
for unimplanted and
for implanted i-HoMgZn (Fig. 21) and dodecagonal (dd)
NbTaTe (Fig. 22) showed similar behaviour.
Time dependence
To assess the inuence of loading time t upon the
hardness H, measurements were performed with i-
YMgZn varying t in the range 2610
22
10
2
s by a pulse
indentation method (see Golovin et al., 2002).
According to Fig. 23, the change of almost four orders
of magnitude in t leads to a decrease of only 10% in H.
Hence the contact area approaches its equilibrium value
pretty rapidly, i.e. the dominating deformation does not
require much time.
Effect of implantation
Specimens of i-AlPdMn, i-HoMgZn and d-AlCoNi
have been implanted using B
z
ions (ion dose 10
16
cm
22
,
Table 5 Hardness at room temperature
QC H
Meyer
, GPa* H
V
, GPa
{
H
Meyer
, GPa
{
d-AlCoCu 10
.
170
.
30 (Murthy et al., 1999)
d-AlCoCuSi 9
.
70
.
3 {2} (Paufler and Wolf, 2003) 8
.
10
.
4 (polyQC) (Kang and Dubois,
1992b)
16
.
81
.
2 {2} (Wolf and
Paufler, 1999b)
10
.
20
.
4 {10} (Paufler and Wolf, 2003) 7
.
820
.
10 {10} (Mukhopadhyay et al.,
2001)
14
.
61
.
5 {10} (Wolf and
Paufler, 1999b)
9
.
6 (Wittmann et al., 1991)
d-AlCoNi 10
.
90
.
3 (Paufler and Wolf, 2003) 8
.
7 {10}, 9
.
4 {2} (Takeuchi et al., 1991) 11
.
4 {10} (Li et al., 2004)
8
.
640
.
28 {10} (Liu et al., 2003)
d-AlCrCuFe 8
.
30
.
7 (Michel, 1992)
i-AlCuFe 7
.
850
.
60 (Giacometti et al., 1999)
9
.
81
.
0 (Ko ster et al., 1993)
7
.
00
.
4 (Kang and Dubois, 1992b)
i-AlCuLi 5
.
1 (Takeuchi et al., 1991)
3
.
820
.
16 (Bhaduri Sekhar, 1987)
4
.
100
.
15 (Sainfort and Dubost, 1988)
R-AlCuLi 4
.
i-AlCuRu (poly-QC) 10
.
i-AlPdMn 9
.
30
.
.
40
.
4 {5} (Deus et al., 1997) 21
.
62
.
0 (Wolf and Paufler,
1999b)
8
.
20
.
3 {2} (Deus et al., 1997)
6
.
9 {2}, 7
.
1 {5} (Yokoyama et al., 1993)
8
.
0 {3} (Yokoyama et al., 1993)
(poly-QC) 9
.
5
.
940
.
02 (Wollgarten and Saka, 1997)
i-YMgZn 5
.
70
.
.
3 (Edagawa et al., 1998) 12
.
31
.
2 {2} (Wolf and Paufler,
1999b)
i-DyMgZn 6
.
60
.
2 (Paufler and Wolf, 2003)
i-HoMgZn 5
.
40
.
Al
73
Co
27
10
.
50
.
Al
5
Co
2
10
.
60
.
Al
3
Co 9
.
00
.
Al
13
Co
4
9
.
40
.
Al
9
Co
2
8
.
80
.
*Meyer hardness from microhardness. Load 1 N.
{
Microhardness, various loads of the order of 1 N.
{
Meyer hardness deduced from nanohardness data using a corner-of-a-cube indenter. Load 0
.
1 mN.
{2},{3], {5},{10}5surface of two-, three-, five- or 10-fold symmetry.
20 Hardness H versus contact depth h
c
for d-AlCoNi at
room temperature; squares: experimental data (after
Pauer and Wolf, 2003);solid line: model according to
Fleck et al. (1994)
c
for unimplanted and
for implanted i-HoMgZn (after Pauer and Wolf, 2003)
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ion energy 180 keV). This treatment is known to give
rise to atomic disorder. Measurements by these authors
showed that the hardness of all QC investigated at room
temperature decreased due to irradiation. This is similar
to the observations of Burnett and Page (1984) with Si.
According to Monte-Carlo simulation, the maximum
penetration depth of B
z
ions is 500 nm for i-AlPdMn
and 600 nm for i-HoMgZn (Pauer and Wolf, 2003).
Thus the indentation depth was well below the range of
implantation. Figure 24 shows the impact of implanta-
tion upon the F(h) curve of i-HoMgZn. The indenter
penetrated deeper into the implanted QC, i.e. the
hardness decreased. For hardness values, see Fig. 21.
Moreover, the ISE practically vanished. The latter result
resembles the absence of ISE due to the free volume
effect in amorphous materials which facilitates atomic
transport. Also, the crack formation probability near
indents was found to be reduced and pile-ups were
found to be less pronounced (Fig. 25), i.e. decreasing
hardness seems to be accompanied by increasing
toughness.
Pop-in
Looking more closely at Fig. 17, sudden displacement
discontinuities during loading can be observed. One in i-
HoMgZn is more pronounced at about 2200 N, others
are less well developed. This phenomenon, now known
as a pop-in event, has been found in various crystalline
materials and was attributed to the nucleation of
dislocation loops or cracks or to phase transitions under
the indentation stress (cf., e.g. Page et al., 1992). Pop-
ins were observed in QC for the rst time by Wolf et al.
(2001). Unloading/reloading cycles were performed
(Fig. 26) to check the rst appearance of inelastic
deformation.
Hardness decreased due to ion implantation, however,
pop-ins continued to occur. Having undertaken pure
elastic cycles, a further increase in load initiated the rst
pop-in indicating the transition to an inelastic deforma-
tion mode (cf. Fig. 27). As the penetration depth was
increasing discontinuously, the contact pressure p
m
(hardness) decreased in the same way (for quantitative
details cf. Fig. 27). The sharper the indenter, the deeper
was the pop-in. Figure 28 illustrates a typical series of
c
for dd-NbTaTe;
different point sets correspond to different sites
along the surface (after Pauer and Wolf, 2003)
23 Dependence of hardness H of i-YMgZn on the loading
time t using a Berkovich indenter (load 40 mN); H is
the universal hardness, which includes elastic defor-
mation; thus, H values are about 20% smaller than
the Meyer nanohardness used elsewhere in this work
(after Pauer and Wolf, 2003)
24 Comparison of multi-indentation forcedisplacement
curves (Berkovich indenter) for unimplanted and B
implanted i-HoMgZn (vefold surface); six unloading/
reloading cycles have been performed for the same
indent before nal unloading was done; staircase like
multiple pop-ins were often found in QC (after Pauer
and Wolf, 2003)
25 Comparison of Berkovich indents at room tempera-
ture in i-AlPdMn implanted (left) and unimplanted
(right); surface normal of vefold symmetry; lateral
scan width 4 mm; height scale 200 nm; no cracks
could be observed near the left indent and pile-ups
were found to be less pronounced (after Pauer and
Wolf, 2003)
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pop-ins, when a cube corner was used. Figure 29
indicates the corresponding pressure drops versus
contact depth. While the force was increasing, the
contact pressure decreased (i.e. the contact area
increased) during loading. Drops per pop-in amounted
typically to 1 GPa.
Adopting the model of dislocation nucleation and/or
motion facilitated by hydrostatic stress, it is concluded
that the rst pop-in corresponds to the maximum shear
stress to activate slip. It is approximately given by the
Tresca stress (Johnson, 1996) t
Tresca
50
.
46p
m
, which is
<5
.
8 GPa for i-YMgZn at room temperature. As a
result of the absence of strain hardening (at elevated
temperature) (cf. Brunner et al., 2000; Urban et al.,
1999, 2002), subsequent bunches of dislocations can be
activated at lower shear stress. One of the consequences
of dislocation movement could be deformation by
twinning, martensitic or related phase transitions to
meet the demands of volume change, as observed by
Fikar et al. (2001).
Influence of temperature
Measurements of microhardness of d-AlCoNi, d-
AlCuCoSi and i-AlPdMn as a function of temperature
have been performed up to <800 K (Fig. 30). Hardness
H decreased with increasing temperature T in two stages
similar to the hardness and yield stress of many
crystalline intermetallic compounds (Kirsten et al.,
1964; Schulze and Pauer, 1972). Obviously, two
distinct mechanisms predominate at lower (l) and higher
(h) temperatures. The transition in H(T) occurs at
homologous temperatures (T/T
m
)
0
<0
.
6 (Wolf and
Pauer, 1999a,b, 2001). Assuming thermally activated
processes below and above (T/T
m
)
0
, the ratio of slopes
[dH/dT]
l
/[dH/dT]
h
gives an indication of the ratio of
activation volumes v. For i-AlPdMn, it was found that
[dH/dT]
l
/[dH/dT]
h
5v
h
/v
l
<0
.
12. If the low temperature
process was governed by a cluster friction mechanism
and the high temperature process by recovery-controlled
deformation (Messerschmidt et al., 2000), then a factor
of 10 in the activation volumes seems reasonable.
Uniaxial macroscopic deformation experiments on d-
AlCoNi (Feuerbacher et al., 1997) and i-AlPdMn (Geyer
et al., 2000) without hydrostatic pressure, however, have
not yet been done at T/T
m
(0
.
7.
26 Loaddisplacement curve of a multi-indentation test
on a vefold surface of i-YMgZn using a sphero-
cone indenter; loading/unloading/reloading cycles
with increasing maximum force lead to the occur-
rence of pop-ins and, simultaneously, inelastic hys-
teresis (after Pauer and Wolf, 2003)
27 Contact pressure p
m
5F/A
c
versus contact depth h
c
derived from Fig. 26 near rst pop-in; note that
h
c
,total displacement; as a result of the pop-in, pres-
sure drops from 13 to 8 GPa (after Pauer and Wolf,
2003)
28 Loaddisplacement curve for i-YMgZn, when a
cube-corner indenter is used; a series of pop-in
events has developed with increasing load (after
Pauer and Wolf, 2003)
29 Contact pressure versus contact depth calculated
from Fig. 28 (after Pauer and Wolf, 2003)
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Crack formation
When indented by a microhardness tester at room
temperature, most quasicrystals, like other brittle
materials, develop cracks starting at the corners of the
impression pyramid. A statistical analysis of crack
directions near indents on surfaces of both two- and
vefold rotational symmetry of Al
70
Pd
23
Mn
7
revealed
that cracks exhibit a shear like habit and prefer an
overall propagation along planes of two-, three- and
vefold symmetry rather than following the plane of
maximum stress (Deus et al., 1997). However, looking
more closely at the crack paths, meandering phenomena
appeared (Wolf and Pauer, 1999a). They are particu-
larly frequent in the case of cracks with cleavage planes
of twofold symmetry perpendicular to the surface. Their
propagation direction suddenly changed after typical
lengths of 50100 nm. The angular alteration proved to
be a multiple of 72u thus permitting to continue
propagation along a plane of the same symmetry
(Wolf et al., 1997; Wolf and Pauer, 1999b). Smaller
lateral changes in the order of 1 nm could not be
excluded due to the limited resolving power of the
method. The rough appearance of cleavage planes has
been predicted in principle by Trebin (1999) from two-
dimensional numerical simulations. They showed that
cracks can propagate by emitting dislocations which
leave a phason wall of reduced surface energy in their
trail. This trail avoids structural clusters.
The occurrence of Palmquist type microcracks at the
corners of microindents has been used to evaluate the
mode I critical stress intensity factor (fracture tough-
ness) of i-AlPdMn. The value K
Ic
51
.
26 MPa m
1/2
(Deus
et al., 1997) is an order of magnitude smaller than that of
conventional aluminium alloys (e.g. K
Ic
517 MPa m
1/2
for AlLiCuMgZr (Brandes and Brook, 1992), but
comparable to other crystalline intermetallic and
quasicrystalline phases such as, e.g. K
Ic
51 MPa m
1/2
(Wittmann et al., 1991) and 1
.
40
.
1 (Mukhopadhyay
et al., 2001) for d-AlCuCoSi; K
Ic
51
.
010
.
09 MPa m
1/2
(Liu et al., 2003), 0
.
800
.
08 MPa m
1/2
(Murthy et al.,
1999) and 0
.
81 MPa m
1/2
(Li et al., 2004) for d-AlCoNi.
A strong inuence of surface symmetry upon the
morphology of impressions has been reported by Wolf
et al. (1997, 2000) and Wolf and Pauer (1999b,c).
Moreover, while the surface near an indent on an
icosahedral QC showed typical pie chart like pile-ups, it
was found rather smooth on decagonal QC. In the case
of microhardness indents, the apparent volume of the
piled-up elevations was about 3040% larger than the
volume of the impression. This is obviously due to
lateral cracking and subsurface defect formation.
Contrary to that, the volume balance for spherical
indentation under the same conditions proved negative,
i.e. about 70% of the displaced material was missing
(Wolf et al., 2000). There is evidence for long-range
transport of matter from the indent towards the outer
regions thus elevating the overall surface level of the
impression environment and making precise AFM
topology difcult. A proof of the conservation of
volume after plastic deformation, however, could not
yet be given. Violations, if any, might be due to phase
transitions. It is interesting to point out that Reibold
et al. (2005) have demonstrated the existence of
nanocrystals near the nanoindent through high resolu-
tion electron microscopy. Mukhopadhyay et al. (2006a)
have discussed that in the absence of active dislocations
in quasicrystals, the plasticity during nanoindentation
can be related to the nucleation and growth of shear
bands (i.e. localised deformation) which is observed in
AFM images as well as reected in a loaddisplacement
diagram in the form of discontinuities (i.e. pop-in effect).
Thus it is reasonable to argue that deformation during
room temperature nanoindentation proceeds via shear
band formation and subsequent phase transformation.
However, more detailed studies in this direction are
required to understand this aspect from the stability and
crystallography of this complex structure.
Bulk metallic glasses
Indentation techniques have been employed to deter-
mine the mechanical properties of thin ribbons of
metallic glasses (Sargent and Donovan, 1982). Now a
new generation of metallic glasses unlike thin ribbons
can be fabricated in bulk form by conventional foundry
practices (Inoue, 2000; Johnson, 2002). Extensive
indentation studies on various types of bulk metallic
glasses (BMG) have been pursued in order to explore
their structural applications. Like crystalline materials,
the constraint factor for correlating hardness with yield
stress also seems to be interesting in the case of BMG.
The applicability of the MohrCoulomb versus the von
Mises criteria for plastic deformation during indenta-
tion is discussed by several workers. In the load
displacement indentation curve, many interesting
features in the form of serrations, ripples, displacement
bursts, discontinuities, pop-ins (all these features are
identical but differ in terms of scaling) have been
reported. The importance of shear bands for plastic
deformation are emphasised. Several studies also indi-
cate the possibility of phase transformation during
indentation.
Recently, Schuh and Nieh (2004) have surveyed the
indentation tests on bulk metallic glasses and reported
on the hardness measurements as well as the onset of
plasticity, the role of shear banding, structural changes
beneath the indenter and the rate dependent effects
measured by nanoindentation. It has been reported that
yield strength W
y
can be approximated following Tabors
30 Meyer hardness versus temperature of d-Al
73
Co
13
Ni
14
and i-Al
70
Pd
21
Mn
9
between room temperature and
600uC (load F51 N) as derived from Vickers tests
(surface orientation in parentheses) (after Pauer and
Wolf, 2003)
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relation (Tabor, 1986)
H~Ks
y
(45)
where K is dependent on the indenter shape as well as on
the mechanical properties of the material being
indented, especially on the strain hardening character-
istics. The value of K is found to be close to 3 in most of
the amorphous materials including glassy materials and
bulk metallic glasses (Fig. 31). From Fig. 31, a simple
linear relationship can be justied, though there is a
scatter which needs to be understood from the
mechanics of plastic deformation of glassy materials. It
can be mentioned that metallic glasses are non-strain
hardenable materials and therefore they can be regarded
as rigid perfectly plastic material. The slip-line eld
theory applicable for perfectly rigid plastic material
suggests a simple relation between hardness and yield
strength. The experimental results shown in Fig. 31 are
based on the Vickers or Berkovich indenters, and the
relevant numerical slip-line eld analysis for various
conical indenter can be expressed as (Lockett, 1963).
H~
s
y
3
p 1
:
41z2
:
72h (46)
where h is the half angle of the cone-shaped indenter in
radians. Introducing the value of 2570u for Vickers or
Berkovich indenters in equation (2) and comparing with
equation (45), the value K52
.
7 is obtained which is
close to the empirical value 3. Dao et al. (2001) have
considered this problem in much more detail using
nite element simulations and obtained the following
relationship
H~
2N
1
B
s
y
N
2
zln
E
r
s
y
_ _ _ _
(47)
where B, N
1
, N
2
are numerical constants, and E
r
is the
reduced modulus. It appears that, for metallic glasses,
E
r
/W
y
can be approximated to 45. Setting N
1
and N
2
equal to 9
.
4509 and 21
.
2433, respectively, B can be
obtained as 24
.
5. Considering all constants of equa-
tion (47) and comparing with equation (45), the value of
K is obtained as 2
.
1, which is a lower bound of the
experimental data. It is observed from experimental and
various theoretical work that the constraint factor is
lower than the value for crystalline material. Therefore
the material is harder than the crystalline material with
the same yield strength. The reason has been argued on
the basis that the glassy material is pressure-sensitive
and the normal stress on a shear plane plays an
important role, and it delays the yielding which causes
the shallower indentation compared to that predicted by
the von Mises criterion. Therefore the MohrCoulomb
criterion appears to be more applicable for the glassy
material. This can be expressed as
t
y
~k{as
n
(48)
where t
y
is the shear stress on the slip plane at yield, s
n
is
the normal stress acting on the shear plane and k and a
are system-specic constants that dene the shear
strength and the atomistic friction coefcient of the
glass, respectively. Vaidyanathan et al. (2001) performed
the simulations run for the von Mises and Mohr
Coulomb criteria and showed the comparison with the
experimental data (Fig. 32). It is clear from this work
that the von Mises criterion predicts greater depth at a
particular load whereas the MohrCoulomb criterion
predicts a lower depth which agrees well with the
experimental data with a50
.
13. Though these results are
supporting the MohrCoulomb criterion, still more
studies are required in this direction. Recently,
Ramamurty and co-workers (Patnaik et al., 2004; Jana
et al., 2004a,b; Ramamurty et al., 2005) have studied the
deformation characteristics and recognised with the help
31 Plot of hardness and yield stress for various types of
metallic glasses; most of the data can be seen to lie
closely near the slope K53, though some theoretical
values of K are somewhat lower than the trend; data
from various metallic glasses are compiled and
plotted by Schuh and Nieh (2004)
32 Comparison of theoretical and experimental data from
the work of Vaidyanathan et al. (2001) for Berkovich
indentation on Zr-based bulk metallic glass; experi-
mental data are found to agree well with those calcu-
lated by the MohrCoulomb yield criterion (after
Schuh and Nieh, 2004)
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of their experimental evidence that the von Mises
criterion is inappropriate for metallic glasses even
though some earlier reports supported this model
(Kimura and Masumoto, 1983; Bruck et al., 1994). It
has been suggested that a MohrCoulomb type criterion
which takes into account the normal stress across the
slip plane in addition to the local shear stress is better
suited. They have attributed this aspect to the high
constraint factor of metallic glasses such as Zr-based
glass. They have also extended the expansion cavity
model and found that this model agrees well with their
FEM results. It is shown that the high plastic constraint
factor exhibited by metallic glasses at large indentation
strains is an outcome of their pressure-sensitive plastic
deformation.
In metallic glasses, a few very small and isolated pop-
in events were observed by Wang et al. (2000) in a Zr-
based glass, after which the phenomenon was reported
in many other alloys (Golovin et al., 2001; Schuh et al.,
2002; Schuh and Nieh, 2003; Nieh et al., 2002; Greer
et al., 2004; Greer and Walker, 2002; Wright et al.,
2001). In all these alloys, the displacement bursts are
very small in the range of 125 nm and appear to occur
with higher frequencies at a low indentation rate
(Fig. 33). However, Vaidyanathan et al. (2001) did not
observe the displacement burst which could be due to
the high loading rate during indentation. Various BMGs
such as Cu-based (Cu60Zr20Hf10Ti10), Zr-based
(Zr65Al10Ni10Cu15), Pd-based (Pd40Ni10Cu30P20),
and La-based (La55Al25Cu10Ni5Co5) were studied
(Schuh and Nieh, 2003).
It is now understood that the plastic deformation of
BMG is dependent upon structural dynamics. Homo-
geneous and heterogeneous deformation have been
discussed in Zr and La based BMG in terms of the
kinetic aspects of plastic deformation. Heterogeneous
deformation (localised deformation) occurs at room
temperature by the formation of localised shear bands,
followed by rapid propagation of these bands and
catastrophic fracture. It is known that in compression
tests, the BMGs exhibit essentially no strain hardening,
and plastic ow is serrated, with many small load drops.
Figure 34 shows the formation of shear bands which are
commonly observed on the surface and beneath the
surface while indenting bulk metallic glasses (Jana et al.,
2004a). The nature of shear bands also depends on the
indentation rate, which can be clearly seen in Fig. 35
(Jiang and Atzmon, 2003). Wright et al. (2001) and
Golovin et al. (2001) used nanoindentation for the study
of serrated ow in BMGs and observed discrete
displacement burst (pop-ins) which they attributed to
the emission of shear bands. It is also observed that a
lower strain rate promotes more prominent serrations or
displacement bursts. Chinh et al. (2004) observed the
plastic instability as serrated ow in bulk metallic
glasses. They noted that the phenomenon is similar to
that in crystalline alloys and manifested itself as discrete
steps in the loaddepth indentation curve (Schuh and
Nieh, 2003; Dao et al., 2001; Vaidyanathan et al., 2001;
Kim et al., 2002; Wright et al., 2001; Jiang and Atzmon,
2003; Benameur et al., 2002; Nieh et al., 2002; Golovin
et al., 2001). In crystalline solids, the physical basis for
the appearance of plastic instabilities is the negative
strain rate sensitivity originating mainly from the
interaction with the precipitates.
As loading rate is increased by several orders of
magnitude, the nature of serrated ow changes sub-
stantially from step like Ph curves at the lowest rates, to
a very smooth parabolic curve at the highest rates
(Fig. 36). At rates in between these extremes, Ph curves
exhibit serrations that appear more as uctuations or
ripples than as discrete, horizontal displacement bursts.
33 Example of indentation loading (Ph) curves for a
variety of metallic glasses illustrating that discrete
pop-ins or ow serrations are common to many
amorphous alloys; origin of each curve has been off-
set for clarity, and several pop-in events have been
denoted by arrowheads (after Schuh and Nieh, 2004)
a As-cast alloy subjected to indentation load of 2500 g;
b As cast alloy subjected to indentation load of 2000 g,
exhibiting semi-circular shear band morphology
34 Morphology of subsurface deformation zones under-
neath Vickers indenter (after Jana et al., 2004a)
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During nanoindentation with a constant loading rate,
the displacement rate is a non-linear function of time t,
as is the indentation strain rate dened by 1/h(dh/dt). At
the outset of each experiment, the strain rate is very high
but decreases with depth as 1/h approaches an approxi-
mately constant value at very large depths. The trends in
strain rate are not smooth and monotonic but exhibit
many short peaks that appear to increase in size as the
indentation proceeds. These short bursts of rapid
displacement correspond to the pop-in events exhibited
in the Ph curve. Furthermore, the magnitude of the
peaks is strongly affected by the indentation strain rate.
These effects are shown for other types of BMGs such as
Zr-based and Pd-based systems.
Golovin et al. (2001) have earlier observed that
localised (inhomogeneous) plastic ow of metallic
glasses can be accompanied by noticeable serrations in
the stressstrain curves. They have reported the results
of nanoindentation tests of bulky glassy PdCuNiP. The
strain serrations of the indenter can occur both towards
and against the applied force. It is known that
nanocrystallisation can form in shear bands produced
during severe bending or high energy ball milling of thin
ribbons of a metallic glass. Kim et al. (2002) have
demonstrated experimentally that highly conned and
controlled local contact at the ultrane scale in the form
of quasi-static nanoindentation of a bulk glassy metal
alloy at room temperature can cause nanocrystallisation.
However, other studies did not show any phase
transformation except for a subtle change in the TEM
contrast, which may be due to the lower strain rate or to
hydrostatic pressure. Recently, Mukhopadhyay et al.
(2006b) showed the evolution of nanocrystals during
indentation of Cu-based metallic glasses. It was also
reported that the propensity of nanocrystallisation is
much more prominent near the indent region compared
to that of regions far from the indent. However, this
aspect of phase transformation from the kinetic point of
view for nucleation and growth of nanocrystals during
the indentation period requires further theoretical and
experimental investigation.
Nanomaterials
Some interesting work on nanomaterials employing
micro/nanoindentation techniques is discussed.
Attempts are not made to discuss nanostructured thin
lm studies, except to cite a few examples. Recently,
Mirshams and Parakala (2004) reported nanoindenta-
tion experiments on electrodeposited nanocrystalline
(size ,19 nm) and commercially produced microcrystal-
line (,21 mm) Ni with three geometrically different
indenters. The highest value was obtained from the
conical indenter and the lowest from the Berkovich
indenter. The hardness measurements obtained from
Berkovich and cube-corner indenters showed a good
correlation with the strain gradient plasticity model. The
ISE was found to be strongly dependent on the indenter
geometry and less on indentation depth. There was
negligible strain rate dependence (within the range of
0
.
050
.
15 s
21
) of hardness to deeper depths and a
signicant increase in the hardness due to the decrease
in grain size. The hardness obtained by Berkovich and
cube-corner indenters has been shown to justify the
mechanism based strain gradient plasticity approach.
Their results also indicated that the microstructural
length scale parameter is small in nanocrystalline
material and therefore the strain gradient length is
higher in nanocrystalline nickel to produce the same
stress in microcrystalline material. The present study
suggested that a more detailed study is needed for the
analysis of deformation mechanism for conical indenter.
35 AFM illumination image of indents produced at pene-
tration rates of a 100 nm s
1
and b 1 nm s
1
on amor-
phous Al
90
Fe
5
Gd
5
(after Jiang and Atzmon, 2003)
36 Indentationdepth load curve of a Pd40Ni20P
BMG measured at different loading rates (after Schuh
et al., 2002)
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Schwaiger et al. (2003) examined strain rate sensitivity in
a nanocrystalline Ni sample (grain size ,40 nm) using
the nanoindentation technique with different loading
rates and observed that nanocrystalline (nc) pure nickel
was found to exhibit a positive strain-rate sensitivity in
ow stress, an effect that was not observed in ultrane
crystalline (ufc) and microcrystalline (mc) nickel. This
rate sensitivity was conrmed by the depth sensing
nanoindentation and tensile testing. The strain rate
sensitivity was observed to be related to the grain size.
The indentation hardness at 1 mm depth increased from
5
.
7 GPa at a strain rate of 0
.
01 s
1
to 6
.
4 GPa at a strain
rate of 0
.
1 s
1
. A similar trend was observed at higher
loads: the hardness increased by almost 10% when the
loading rate was increased from 3
.
8 to 186
.
1 mN s
1
.
Shaz et al. (2002) have investigated the microhardness
measurement of TiZrNi nanoquasicrystalline (40 nm)
materials. The indentation experiments were carried out
at 25, 50, 100 and 200 g load, which show the reverse
indentation size unlike the micrometre size material.
SEM observation clearly brings out the presence of
shear bands but no cracking was found (Fig. 37). As has
been shown earlier, microquasicrystalline and single
quasicrystalline samples always show microcracking
(Murty et al., 1999; Mukhopadhyay et al., 2001). In
the present system, because of the formation of
nanoquasicrystalline phases, the hardness as well as
ductility has increased. The microhardness of nanoqua-
sicrystalline alloy shows several interesting features. The
average hardness of the alloy was found to be around
3
.
6 GPa. The absence of cracks around the indented
area suggests a superior toughness of the material. This
is further supported by the evolution of shear bands, a
signature of localised deformation. The hardness was
found to increase with load initially and then to
decrease. This may be due to the easy ow of materials
in nanocrystalline/nanoquasicrystalline material by
grain boundary sliding or to phase transformation.
Localised ow indicates the evolution of shear bands
during indentation loading, analogous to deformation
of metallic glasses (Sargent and Donovan, 1982).
However, this is an interesting feature and may require
further study. Mukhopadhyay et al. (2004) have
synthesised nanoquasicrystalline phases in the
Mg
32
(AlZn)
49
intermetallic alloy and compared the
microhardness data obtained from the nanoquasi-
crystalline and microcrystalline phases of the same
composition. The microhardness values of the nano-
quasicrystalline phases are reported to be more than
those of the microcrystalline phases. They found that the
indentation size effect is more prominent in nanophase
material compared to that of microphase material
(Fig. 38). The propensity of cracking is also less in
nanomaterials.
The applicability of the HallPetch equation to
materials with grain sizes smaller than 1 mm is a
question of signicant technological importance in view
of the recent advances in materials processing techniques
such as rapid solidication, vapour deposition and
sputtering, producing ultrane grain sizes. Experi-
mental studies have indicated that the rening of grain
sizes to the nanometre scale can improve mechanical
properties. For example, an increase from 0
.
9 GPa in
the hardness of nickel was observed when the grain size
was decreased from 12
.
5 mm to 12 nm (Hughes et al.,
1986). Similarly, an increase from 0
.
5 to 2
.
5 GPa was
achieved in nanocrystalline copper by reducing the grain
size from 50 mm to 6 nm (Nieman et al., 1989). The
observed increase in hardness with grain size which can
37 a Microindentation at 200 g; absence of cracks shows
better toughness of material; b magnied image of
shear bands developed during indentation; c SEM of
microindentation of microcrystalline version of TiZr
Ni alloy, showing no shear bands (after Shaz et al.,
2002)
38 Plot showing microhardness varying with load in
Mg
32
(AlZn)
49
for a RSP foil; b as cast; variation of
hardness with load (indentation size effect) is greater
in RSP foils containing nanophase materials (after
Mukhopadhyay et al., 2004)
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be explained by the HallPetch equation has also been
reported by other workers (Valiev et al., 1992; Jang and
Koch, 1999). An important aspect of strengthening by
microstructural renement is that the strength increase
need not be at the expense of ductility. However, it is
also well documented in the literature that below a
certain grain size, the HallPetch slope may decrease
and even become negative (Fig. 39) (Chokshi et al.,
1989; Lu et al., 1990; Fougere et al., 1992). The type of
processing method used for varying the grain size, such
as heat treatment as well as the presence of imperfec-
tions such as triple junctions or porosity (Palumbo et al.,
1990; Wang et al., 1995) have been cited among the
possible causes for observed inverse HallPetch beha-
viour. Recently, Farhat et al. (1996) investigated hard-
ness of nanocrystalline aluminium of various sizes
ranging from 15 to 100 nm, using the ultra-microhard-
ness indenter and observed that the experimental data
are well represented by the HallPetch relationship.
From the present study, it can be concluded that the
grain boundaries may be providing strengthening down
to grain sizes as small as 15 nm.
Nanophase TiAl, with grain sizes in the range of 10
20 nm, was synthesised by magnetron sputtering in an
inert gas atmosphere and consolidated, in situ, under
vacuum, and Vickers microindentation tests were
carried out by Chang et al. (1993). The Vickers micro-
hardness of these samples at room temperature and at
230uC revealed an inverse HallPetch relationship at
small grain sizes, 1030 nm, and the usual HallPetch
behaviour at larger grain sizes. A small component of
indentation creep was also observed. The maximum
hardness is four times larger than that of a cast TiAl
specimen of the same composition. The Vickers hard-
ness was also observed to decrease rapidly with
temperature above 200uC. Schuh and Nieh (2003) have
investigated the HallPetch breakdown regime by
conducting hardness testing in nanocrystalline pure Ni
and NiW alloys. They observed the breakdown of the
HallPetch relationship near d514 nm and d57 nm in
the case of nanocrystalline Ni and NiW alloy and
suggested a diffusional creep mechanism is responsible
for this inverse relationship.
Recently, Veprek et al. (2000) developed multiphase
nanocomposite coatings (320 mm thick) consisting of
nanocrystalline TiN, amorphous Si
3
Ni
4
and amorphous
and nanocrystalline TiSi
2
, nc-TiN/a-SiNx/a- and nc-
TiSi
2
on steel substrate by the chemical vapour
deposition (CVD) technique. The load independent
Vickers microhardness from 80 to .105 GPa was
measured by the loaddepth sensing techniques for
applied loads between 30 and 200 mN and veried by
measuring the size of the remaining plastic indentation
using SEM. It has been observed that the ultrahardness
of 80100 GPa depends on the amount of a- and nc-
TiSi
2
phases. Veprek (1999) has reported that when the
grain size decreases below 10 nm, the inverse HallPetch
relation is observed. It has been concluded that a high
hardness with a high fracture toughness and elastic
recovery is a simple consequence of such nanostructure.
As pointed out by Koch and Narayan (2001), there
are many problems associated with measurement of
hardness as a function of grain size for nanocrystalline
materials. If the grain size is varied by annealing the
nest grain samples for grain growth, it is possible that
other structural and/or compositional effects may occur
on annealing. Most of the experiments that report the
inverse HallPetch effect have samples which exhibit
clear artefacts or are at least questionable. However,
there are reports where no obvious artefacts or other
problems exist. They have identied at least three such
apparently artefact free examples of the inverse Hall
Petch effect in hardness tests (Figs. 40 and 41).
Computer simulations also predict softening at grain
sizes below some critical value. Both the simulations
show this critical grain size to be of the order of 10 nm
or smaller. While it has been difcult to assess the
hardness of the smallest nanocrystalline samples unam-
biguously, it appears that the inverse HallPetch effect is
real. Models which describe the deformation of nanos-
cale materials should use only the few experimental sets
of data that are clearly artefact free to test their
predictions (Fig. 42) (Koch and Narayan, 2001).
Obviously, many more investigations are required to
establish the inverse HallPetch behaviour in nanocrys-
talline materials and its mechanism.
Phase transitions during hardness tests
Early observations of morphologic features of scratches
on glass by Klemm and Smekal (1941) led Madelung
(1942) to conclude that local melting could arise due to
the highly localised introduction of mechanical energy
39 Hardness versus grain size, d
0
.
5
for nanocrystalline
Cu and Pd (after Chokshi et al., 1989)
0
.
5
for nanocrystalline
(Fe,Co)33Zr67 alloys (after Alves et al., 1996)
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into the solid surface. Although rst-order phase
transitions of this type will probably not occur during
indentation at conventional speed, pressure-induced
structural phase transitions, which have become known
for numerous materials, should nevertheless play a role
in hardness tests, in particular when loaddisplacement
curves are considered. In order to initiate a certain phase
transition, the (hydrostatic or deviatoric) pressure
beneath the indenter should exceed the critical value
for the phase transition but should not do so for the
spontaneous nucleation of dislocations in the parent
phase. If the latter condition is violated, plastic strain
will diminish the stress quickly below the critical value,
which in turn may be lowered under deviatoric stresses
(Gilman, 1993). This implies that the presence of
dislocations and their ability to move under the stress
eld of the indent will have an impact upon the
occurrence of phase transitions, too. Since the hardness
is of the order of the average contact pressure beneath
the indent, materials that undergo a phase transition
during indentation might be anticipated knowing their
phase transition pressures.
It is, therefore, not surprising that semiconductors
were the materials where genuine phase transitions had
been directly observed for the rst time. These solids
exhibit both a very low initial dislocation density and a
high Peierls stress for moving dislocations. Indeed,
Gridneva et al. (1972) concluded from an athermal
region of the temperature dependence of hardness of Si
and Ge that a phase transformation had occurred, and
Eremenko and Nikitenko (1972) reported on the
formation of the high pressure phase VII in silicon
when indented at temperatures of 400700uC. According
to Hu et al. (1986), this phase appeared under
hydrostatic pressures of 40 GPa. Comparing average
pressures achieved during hardness measurements with
phase transition pressures, Gerk and Tabor (1978) drew
the conclusion that a metallic phase of Ge, Si and
diamond must have been formed beneath the indenter.
A phase transition of single-crystalline Si and Ge
through an electrically conducting state to a metastable
amorphous phase after unloading Vickers and
Knoop indentations (loading-unloading rate
16
.
67 N s
21
, maximum loads 0
.
10
.
5 N) has been
detected by Clarke et al. (1988) using electron diffraction
and electrical conductivity measurements. The authors
argued that remanent stresses inside the indented
material give rise to this amorphous phase. After
scratching, a small amorphous region was developed
surrounded by a region of high dislocation density
(Minowa and Sumino, 1992). Using a spherical indenter,
Williams et al. (1999) observed the transition of Si to a
-tin structure at about 13
.
3 GPa which compares
favourably with 12
.
5 GPa found under hydrostatic
pressure (Hu et al., 1986). It seems worth mentioning
that transition pressures observed with indentation
experiments are not to be equated with equilibrium
pressures because of kinetic effects. They may be
overestimated on increase in Si, for example, by a
minimum of 2 GPa (Hu et al., 1986).
Phase transformations alter the shape of the load
penetration depth curve. They may show up in a pop-in
along the loading curve (Williams et al., 1999; Bradby
et al., 2000, 2001, 2003) and/or a pop-out and/or an
elbow (Page et al., 1992; Novikov et al., 1996; Williams
et al., 1999; Domnich et al., 2000; Bradby et al., 2001,
2003; Zarudi et al., 2003; Ho et al., 2004) on the
unloading branch. Whereas pop-ins often also indicate
the nucleation of dislocations (e.g. Lorenz, 2001; Lorenz
et al., 2003), pop-outs and elbows seem to be more
specic of a phase transition. They occur due to a
sudden expansion of the volume, which has no counter-
part in plastic slip. Figure 43 gives an example indicat-
ing that loading/unloading rates and maximum loads
determine which of these features will appear.
Because of the small volumes involved with indentation,
various techniques have been applied to prove that a phase
transformation is correlated with those mechanical fea-
tures. These are mainly transmission electron microscopy/
electron diffraction studies (Eremenko and Nikitenko,
1972; Clarke et al., 1988; Wu et al., 1999; Bradby et al.,
2000, 2001; Mann et al., 2000, 2002; Ge et al., 2003; Zarudi
et al., 2003; Haberl et al., 2004), Raman microspectro-
metry (Kailer et al., 1997; Lucazeau and Abello, 1997;
Domnich et al., 2000; Bradby et al., 2001; Mann et al.,
2002; Ge et al., 2003; Zarudi et al., 2003), differential
scanning calorimetry (Riontino and Massazza, 2004),
acoustic emission (Mann et al., 2000) or electrical
resistance measurements (Clarke et al., 1988; Mann et al.,
2000, 2002; Bradby et al., 2003; Ho et al., 2004).
While silicon is by far the dominant goal of phase
transformation studies connected with indentation,
0
.
5
for electrodeposited
Ni (after Erb, 1995)
0
.
5
for nanocrystalline
Zn made by laser ablation or mechanical attrition
(after Koch and Narayan, 2001)
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other materials have been studied. Pop-in and elbow
shaped parts of the loadpenetration curve along with
hysteresis have been observed with quasicrystalline
i-Y
10
Mg
30
Zn
60
by Wolf and Pauer (2001), Wolf et al.
(2001) and Pauer and Wolf (2003) (Fig. 26). Also,
other authors reported on pop-ins with quasicrystals
(AlCuFe: Dub et al., 2001, 2002; TiZrNi: Azhazha
et al., 2004). Although the deformation behaviour of
quasicrystals is generally less well understood than that
of crystalline materials, there are direct and indirect
indications of phase transformations occurring in this
type of solid under localised load. The former refer to i-
AlCuFe, where a scratch-induced phase transition
from the quasicrystalline to a bcc phase was detected
using electron diffraction (Wu et al., 2000; Dong et al.,
2001). Nanocrystallisation in quasicrystals has been
reported by Reibold et al. (2005) while indenting the
AlNiCo decagonal single quasicrystals. They found
that the phase transformation is quite likely due to the
volume reduction during this indentation. Phase trans-
formations of the martensitic type, giving rise to the
shape-memory effect, have been examined using both
spherical and pyramidal indenters. The deformation of
spherical indents (tip radius 213 mm, indents (8 mm) on
NiTi was almost completely reversed by heating (Ni
et al., 2002). At indentation depth less than 100 nm,
recovery was found to be almost complete (Shaw et al.,
2003).
Automated ball indentation (ABI) and
field indentation microprobe (FIM)
technique
The industrial applications of nanohardness measure-
ments were reviewed by Michler and Dommann (2001).
Here, in situ indentation techniques are discussed for
evaluating mechanical properties in order to assess the
degradation and hence the remaining life of high
temperature components in a thermal power plant, the
oil/gas industry, nuclear industry, aerospace and chemi-
cal industries. Monitoring the progressive changes in
mechanical properties has been mandatory from the
point of view of ensuring the structural integrity of the
components and safety of the operation. Therefore,
nondestructive methods for mechanical characterisation
are required for any materials aging and life manage-
ment programme.
A eld indentation microprobe (FIM) apparatus was
developed and patented by Haggag and Nanstad (1989)
and Haggag et al. (1989, 1990) to evaluate nondestruc-
tively the mechanical properties. The FIM consists of
two main units: an automated ball indentation (ABI)
unit for measuring the mechanical properties and a
nondestructive evaluation (NDE) unit (consisting of
ultrasonic transducers and a video camera) for deter-
mining the physical properties such as crack size,
material pile-up around indentation, residual stress
presence and orientation. The main components of the
FIM apparatus are shown schematically in Fig. 44. The
tripod arrangement adjusts the ball indenter to be
perpendicular to the surface of the structure or test
specimen. The load can be applied by hydraulic,
pneumatic, mechanical, or any other means. The ABI
test is based on multiple indentations (at the same
penetration location) of a polished metallic surface by a
spherical indenter (in the order of 1 mm diameter). The
data are collected during the test and these are analysed
automatically by the computer attached to the equip-
ment. The applied loads and associated displacements
(depth of penetration of the indenter into the test
a Pop-out appears in unloading curve at slower load-
ing/unloading rates (,1 mN s
1
) and higher maximum
loads (50 mN); b Elbow is formed at faster rates
(3 mN s
1
) and lower loads (30 mN); c Mixed behaviour
is also possible
43 Impact of phase transitions upon shape of load
displacement curves as obtained by nanoindentation
of Si (after Domnich et al., 2000)
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specimen) are measured using a load cell and a linear
variable differential transducer (LVDT). The load
displacement data (Fig. 45) from each unloading
sequence are tted with a rst-degree polynomial and
the t extrapolated to obtain the displacement corre-
sponding to zero load. These displacements and the
maximum cycle load and displacement values from each
indentation sequence are used to determine the hardness
and yield strength, to produce the true-stress/true-
plastic-strain curve, and to estimate fracture toughness.
The ABI analyses are based primarily on elasticity and
plasticity theories and some empirical correlations as
described by Haggag and Nanstad (1989) and Haggag
et al. (1989, 1990). The agreement between ABI-derived
data and those from standard ASTM uniaxial tensile
and fracture toughness tests was demonstrated to be
satisfactory. The authors have suggested that this
technique could also be extended for high temperature
studies as well as indentation fatigue, fracture and creep.
The mechanical properties determined by the FIM
apparatus include elastic modulus, yield strength,
Lu ders strain, strain-hardening exponent, Brinell hard-
ness, true-stress/true-plastic strain curve up to 20%
strain, and presence of residual stress. The fracture
toughness is also estimated using the ABI measured ow
properties and a modied critical fracture strain model.
Furthermore, the shift in the ductile-to-brittle transition
temperature for steel plates and welds, for example, due
to neutron irradiation embrittlement, can be estimated
from the ABI measured changes in the materials yield
strength and ow properties.
Zarzour et al. (1996) carried out microindentation
hardness tests on HY-100 weldments by automated ball
indentation on the weldments and obtained information
from the ABI tests in various regions of the heat affected
zone (HAZ). The results provide a relationship between
grain size and corresponding stressstrain data across
the HAZ. Byum et al. (1997) investigated the through-
the-thickness variations of mechanical properties in
SA508 Gr.3 pressure vessel steels using the automated
ball indentation (ABI) test technique and evaluated
mechanical properties, such as the yield strength,
ultimate strength, ow curve and hardness from
indentation loaddepth curves. Malow et al. (1998)
conducted ABI tests on nanocrystalline (nc) iron which
was produced by mechanical attrition and compacted
into near fully dense samples followed by isothermal
annealing at 800 K resulting in grain sizes between 15
and 24 nm. The ABI method proved useful in examining
the mechanical properties of nc iron compared to that of
conventional hardness testing methods. Stressstrain
curves were obtained which indicated a low strain
hardening at high ow stresses around 3 GPa and a
room temperature strain-rate sensitivity. The deforma-
tion pile-up around the indentations exhibited intense
plastic deformation in localised shear bands.
Murty et al. (1998) investigated the tensile and
fracture properties of ASTM grade A36 steel using a
nondestructive StressStrain Microprobe system (SSM),
developed on the basis of automated ball indentation
(ABI) technique on as-received, and cold worked
materials at several temperatures in the range and at a
constant strain rate. From their study, they observed a
close agreement with the expected tensile and fracture
properties, and concluded that ABI is a reliable
nondestructive technique for determining tensile and
fracture properties of materials. Murty et al. (1999) have
studied the gradients in mechanical and fracture proper-
ties of SA-533B steel welds using the ball indentation
technique. The local stressstrain behaviours of different
microstructural zones of the weld were determined.
Gradients in the strength of the base metal, weld metal
and the different positions in the heat affected zone were
observed to be consistent with the changes in the
microstructure. Mathew et al. (1999) have carried out
ABI tests on service aged cast stainless steel components
and identied the embrittlement as well as increase in
44 Schematic diagram showing basic components of
eld indentation microprobe (FIM) apparatus (after
Haggag et al., 1989)
45 Samples of ABI test results (load versus depth using
a 0
.
76 mm diameter ball indenter) on 316L stainless
steel (SS) base metal (after Haggag et al., 1989)
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strength and decrease in toughness due to aging. They
have further investigated the effect of aging on mechan-
ical behaviour of Alloy 625 using the non-destructive
StressStrain Microprobe (SSM) system based on an
automated ball indentation (ABI) technique, and invol-
ving multiple indentations by a small spherical indenter
at a single penetration location under strain-controlled
conditions and evaluated mechanical properties such as
yield strength, ultimate tensile strength, strength coef-
cient and strain hardening exponent. These studies
demonstrate that ABI can be used as a non-destructive
technique to determine changes in mechanical properties
of nickel base alloy components due to aging. Seok and
Murty (2000) using ABI tests have explained the
decrease in fracture resistance (JR) curves in SA516
steel due to increased strain hardening and generation of
tensile residual stress at the crack tip during cyclic
loading. Murty and Mathew (2004) have studied the
applicability of an automated technique based on ball
indentation for laboratory and eld applications for
determining the mechanical and fracture properties of
materials. Das et al. (2004, 2005a,b) have exploited this
ball indentation technique extensively to study the
mechanical properties of many engineering and service
aged materials. They have observed that the pile-up
around the indent is an important parameter. Based on
the pile-up height, they have proposed a unique
classication scheme for materials.
From all these reports, it is becoming clear that ball
indentation techniques can be used as a NDT tool for
evaluating the mechanical properties of aged compo-
nents so that the extension of their life can be assessed.
From these studies, it should be emphasised that the ball
indentation technique has good potential for direct
industrial application and hence research in this direc-
tion should be pursued.
Concluding remarks
Indentation hardness obtained at micro and nano level
testing exhibits a large mismatch. The differences in
hardness are generally attributed to the indenter shape
effect, indentation size effect as well as to the pile-up
effect, and hence it deserves further study for quantita-
tive understanding. The instrumentation for collecting
the data without visual observation through AFM is
easy to use and automated, but the property evaluated
from such data may not be sufciently accurate.
Therefore, the need for visual observation has been
emphasised to have a better correlation between the
microhardness and nanohardness. The strain gradient
plasticity theory is quite successful for explaining the
ISE in ductile materials, but there is an inherent
difculty to deal with nanoscale deformation. The
RISE, which cannot be explained using SGP theory,
needs to be investigated in a more analytical manner.
The issue of indentation size effect will continue to
dominate the eld of indentation until the mechanics
and mechanism of the deformation under indentation at
various length scales are fully understood. Theoretical
understanding of the material ow in quasicrystals, bulk
metallic glasses and nanomaterials must rst be devel-
oped. Therefore, the issue of mechanical deformation
using indentation techniques in new materials is worth
pursuing for resolving many unsolved problems. The
industrial use of indentation techniques for determining
the remaining life of components in service has proved
to be indispensable compared to other conventional
techniques. However, semiempirical approaches for the
assessment of brittleness need to be established on the
basis of more fundamental analysis.
Acknowledgements
The authors would like to thank Professors
S. Ranganathan, P. Ramachandra Rao, S. Lele,
K. Chattopadhyay, S.N. Ojha, G.V.S. Sastry,
U. Ramamurty, N. Chakraborty, I. Manna, B.S.
Murty, and Dr T. Sudarshan and Dr R.K. Mandal,
Dr M. Chandrasekhar and Dr V.S. Sarma for their keen
interest and useful discussions. The authors would also
like to thank Dr V.C. Srivastava, Mr G. Narayana,
Thakur Prasad, Sunil Pal, G. Subba Rao, Andre Belger
for supplying useful references and stimulating discus-
sions. One of the authors (NKM) thanks the Alexander
von Humboldt Foundation, Germany, for a research
fellowship during which period a part of the work was
completed. Partial financial support from the
Department of Science and Technology (DST), India
is also gratefully acknowledged.
References
1. Acharya, A., Bassani, J.L. (2000): J. Mech. Phys. Solids, 48, 1565
1595.
2. Alves, H., Ferreira, M., Koster, U., Muller, B. (1996): Mater. Sci.
Forum, 225226, 769774.
3. Androussi, Y., Vanderschaeve, G., Lefebvre, A. (1989): Philos.
Mag. A, 59, 11891202.
4. Ashby, M.F. (1970): Philos. Mag., 21, 399424.
5. Atkinson, M. (1995a): J. Mater. Sci., 30, 17281732.
6. Atkinson, M. (1995b): J. Mater. Res., 10, 29082915.
7. Attinger, C. (1947): Ind. Diam. Rev., 7, 264.
8. Auerbach, F. (1890): Nachr. v. d. Ko nigl. Gesellsch. d.Wiss. zu
Go ttingen, No.16, 518541.
9. Auerbach, F. (1891): Ann. Phys. Chem., 43, 61100.
12. Auerbach, F. (1900): Ann. Phys., 4.F., 3, 108115.
13. Azhazha, V., Dub, S., Khadzhay, G., Merisov, B., Malykhin, S.,
Pugachov, A. (2004): Philos. Mag., 84, 983990.
14. Babini, G.N., Bessosi, A., Glassi, C. (1987): J. Mater. Sci., 22,
16871693.
15. Baker, S.P., Ross, C.A., Townsend, P.H., Volkert, C.A.,
Boegesen, P. (eds.) (1995): Thin films: stresses and mechanical
properties V, MRS Symp. Proc. 356, Pittsburgh, PA, Materials
Research Society.
16. Baker, S.P., Cook, R.F., Coecoran, S.G., Moody, N.R. (eds.)
(2000): Fundamentals of nanoindentation and nanotribology II,
MRS Symp. Proc. 649, Pittsburgh, PA, Materials Research
Society.
17. Banerjee, R., Feltham, P. (1974): J. Mater. Sci., 9, 14781482.
18. Bekker, I. (1829): Aristotelis meteorologica, Berolini Typis
Academicis.
19. Benameur, T., Hajlaoui, K., Yavari, A.R., Inoue, A., Rezgui, B.
(2002): Mater. Trans. JIM, 43, 2617.
20. Berkovic, E.S. (1951): Ind. Diam. Rev., 11, 129132.
21. Bernhardt, E.O. (1941): Z. Metallkd., 33, 135.
22. Bhaduri, S.B., Sekhar, J.A. (1987): Nature, 327, 609610.
23. Bhushan, B., Li, X. (2003): Int. Mater. Rev., 49, 125142.
24. Bishop, R.F., Hill, R., Mott, N.F. (1945): Proc. Phys. Soc., 57,
149.
25. Biswas, S.K., Venkatesh, K., Bobji, M.S., Sebastian, K.S. (1996):
Trans. Indian Inst. Met., 49, 725738.
26. Blau, P.J., Lawn, B.R. (eds.) (1986): Microindentation techniques
in materials science and engineering, ASTM STP 889,
Philadelphia, PA, USA, ASTM.
27. Bobji, M.S., Biswas, S.K. (1999): J. Mater. Res., 14, 22592268.
28. Boldt, P.H., Weatherly, G.C., Embury, J.D. (1992): Mater. Sci.
Eng., A155, 251255.
P
u
b
l
i
s
h
e
d

b
y

M
a
n
e
y

P
u
b
l
i
s
h
i
n
g

(
c
)

I
O
M

C
o
m
m
u
n
i
c
a
t
i
o
n
s

L
t
d
29. Boussinesq, J. (1885): Applications des Potentials a letude de
equilibre et du movement des solides elstiques, Paris, Gauthier-
Villars.
30. Bradby, J.E., Williams, J.S., Swain, M.V. (2003): Phys. Rev. B, 67,
085205-19.
31. Bradby, J.E., Williams, J.S., Wong-Leung, J., Swain, M.V.,
Munroe, P. (2000): Appl. Phys. Lett., 77, 37493751.
32. Bradby, J.E., Williams, J.S., Wong-Leung, J., Swain, M.V.,
Munroe, P. (2001): J. Mater. Res., 16, 15001507.
33. Brandes, E.A., Brook, G.B. (1992): Smithells metals reference
book, 7th edn, 1523, Oxford, Butterworth-Heinemann.
34. Bresson, L. (1994): in Lectures on quasicrystals, (ed. F. Hippert,
D. Gratias), 549559, Les Ulis, Les editions de physique.
35. Brinell, J.A. (1900): Baumaterialienkunde 5, 276280, 294297,
317320, 392394, 412415.
36. Brookes, C.A. (1983): in Science of hard materials, (ed. R.K.
Viswanadham, D.J. Rowcliffe, J. Gurland), 181197, New York,
Plenum Press.
37. Brown, L.M., Khan, M.Y., Chaudhri, M.M. (1988): Philos. Mag.
A., 57, 187196.
38. Bruck, H.A., Christman, T., Rosakis, A.J., Johnson, W.L. (1994):
Scripta Metall., 30, 429434.
39. Brunner, D., Plachke, D., Carstanjen, H.D. (2000): Phys. Status
Solidi (a), 177, 203217.
40. Bu ckle, H. (1965): Mikroha rtepru fung und ihre anwendung,
Stuttgart, Berliner Union Verlag.
41. Bull, S.J., Page, T.F., Yoffe, E.H. (1989): Philos. Mag. Lett., 59,
281288.
42. Burnett, P.J., Page, T.F. (1984): J. Mater. Sci., 19, 845860.
43. Byum, T.S., Hong, J.H., Haggag, F.M., Farrel, K., Lee, E.H.
(1997): Int. J. Pressure Vessels Piping, 74, 231238.
44. Calvert, F.C., Johnson, R. (1859): Ann. Phys. Chem., 108, 575
582.
45. Cammarata, R.C., Nastasi, M.A., Busso, E.P., Oliver, W.C. (eds.)
(1997): Thin films: stresses and mechanical properties VII, MRS
Symp. Proc. 505, Pittsburgh, PA, Materials Research Society.
46. Castaing, J., Veyssie`re, P., Kubin, L.P., Rabier, J. (1981): Philos.
Mag. A, 44, 14071413.
47. Chang, H., Altstetter, C.J., Averback, R.S. (1993): J. Mater. Res.,
7, 29622990.
48. Chen, C.C., Hendrickson, A.A. (1973): in The science of hardness
testing and its research applications, (ed. J.H. Westbrook, H.
Conrad), 274289, Metals Park, OH, American Society for
Metals.
49. Cheng, Y.-T., Cheng, C.-M. (1998a): Philos. Mag. Lett., 77, 39.
50. Cheng, Y.-T., Cheng, C.-M. (1998b): J. Mater. Res., 13, 1059.
51. Cheng, Y.-T., Cheng, C.-M. (1998c): J. Appl. Phys., 84, 1284
1291.
52. Cheng, Y.-T., Cheng, C.-M. (1998d): Philos. Mag. Lett., 78, 115.
53. Cheng, Y.-T., Cheng, C.-M. (1998e): Appl. Phys. Lett., 73, 614
616.
54. Cheng, Y.-T., Cheng, C.-M. (1999): J. Mater. Res., 14, 3493.
55. Cheng, Y.-T., Li, Z., Cheng, C.-M. (2002): Philos. Mag A, 82,
18211829.
56. Chernikov, M.A., Ott, H.R., Bianchi, A., Darling, T.W. (1998):
Phys. Rev. Lett., 80, 321324.
57. Chinh, N.Q., Gubicza, J., Kovacs, Z., Lendvi, J. (2004): J. Mater.
Res., 19, 3145.
58. Chokshi, A.H., Rosen, A., Karch, J., Gliter, H. (1989): Scripta
Metall. Mater., 23, 16791684.
59. Clarke, D.R., Kroll, M.C., Kirchner, P.D., Cook, R.F., Hockey,
B.J. (1988): Phys. Rev. Lett., 60, 21562159.
60. Dao, M., Chollacoop, N., VanVlieti, K.J., Venkatesh, T.A.,
Suresh, S. (2001): Acta Mater., 49, 38993918.
61. Das, G., Ghosh, S., Sahay, S.K., Ranganath, V.R., Vaze, K.K.
(2004): Z. Metallkd., 95, 11201127.
62. Das, G., Ghosh, S., Ghosh, S., Sahay, S.K. (2005a): Mater. Lett.,
59, 22462251.
63. Das, G., Ghosh, S., Ghosh, S., Ghosh, R.N. (2005b): Mater. Sci.
Eng. A, 408, 158164.
64. De Guzman, M.S., Nuebauer, G., Flinn, P., Nix, W.D. (1993):
Mater. Res. Symp. Proc., 308, 603618.
65. Deus, C., Wolf, B., Paufler, P. (1997): Philos. Mag. A, 75, 1171
1183.
66. Domnich, V., Gogotsi, Y., Dub, S. (2000): Appl. Phys. Lett., 76,
22142216.
67. Dong, C., Wu, J., Zhang, L., Dubois, J.-M., Brunet, P., Zhou, Q.,
Wang, D., Zhang, H. (2001): Mater. Res. Soc. Symp. Proc., 643,
K7
.
5
.
1K7
.
5
.
11.
68. Drory, M.D., Bogy, D.B., Donley, M.S., Field, J.E. (eds.) (1995):
Mechanical behaviour of carbon and other forms of carbon,
MRS Symp. Proc. 383, Pittsburgh, PA, Materials Research
Society.
69. Dub, S.N., Milman, Yu.V., Lotsko, D.V., Belous, A.N. (2001):
J. Mater. Sci. Lett., 20, 10431045.
70. Dub, S.N., Novikov, N., Milman, Yu.V. (2002): Philos. Mag., 82,
21612172.
71. Dutta, A.K., Chattopadhyay, A.B., Ray, K.K. (2001): J. Mater.
Sci. Lett., 20, 917919.
72. Edagawa, K., Suzuki, T., Takeuchi, S. (1998): Proc. 6th Int. Conf.
on Quasicrystals, (ed. S. Takeuchi, T. Fujiwara), 517520,
Singapore, World Scientific.
73. Elmustafa, A.A., Stone, D.S. (2002): Acta Mater., 50, 36413650.
74. Elmustafa, A.A., Stone, D.S. (2003): J. Mech. Phys. Sol., 51, 357
381.
75. von Engelhardt, W., Haussu hl, S. (1960): Kolloid-Zeitschr., 173,
2035.
76. Erb, U. (1995): Nanostructured Mater., 6, 533538.
77. Eremenko, V.G., Nikitenko, V.I. (1972): Phys. Status Solidi (a),
14, 317330.
78. Exner, F. (1873): Untersuchungen u ber die Ha rte an
Krystallfla chen. K.k. Hof- u. Staatsdruckerei, Vienna.
79. Farhat, Z.N., Ding, Y., Northwood, D.O., Alpas, A.T. (1996):
Mater. Sci. Eng., A206, 302313.
80. Faulkner, A., Tang, K.C., Sen, S., Arnel, R.D. (1998): J. Strain
Anal., 33, 411418.
81. Feltham, P., Banerjee, R. (1992): J. Mater. Sci., 27, 1626.
82. Feuerbacher, M., Bartsch, M., Grushko, B., Messerschmidt, U.,
Urban, K. (1997): Philos. Mag. Lett., 76, 369375.
83. Fikar, J., Bonneville, J., Rabier, J., Baluc, N., Proult, A., Cordier,
P., Stretton, I. (2001): Mater. Res. Soc. Symp. Proc., 643, K7
.
4
.
1
K7
.
4
.
6.
84. Fischer-Cripps, A.C. (2004): Nanoindentation, 2nd edn, New
York, Springer.
85. Fleck, N.A., Muller, G.M., Ashby, M.F., Hutchinson, J.W.
(1994): Acta Metall. Mater., 42, 475487.
86. Fleischer, R.L. (1994): in Intermetallic compounds. Principles
and practice, (ed. J.H. Westbrook, R.L. Fleischer), Vol. 2, 237
256, John Wiley & Sons.
87. Fleury, E., Lee, J.H., Kim, S.H., Song, G.S., Kim, J.S., Kim,
W.T., Kim, D.H. (2001): Mater. Res. Soc. Symp. Proc., 643,
K2
.
1
.
12
.
1
.
6.
88. Fougere, G.E., Weertman, J.R., Weigel, R.W. (1992): Scripta
Metall. Mater., 26, 18791883.
89. Francois, P., Lefebvre, A., Vanderschaeve, G. (1988): Phys. Status
Solidi (a), 109, 187192.
90. Frankenheim, M.L. (1829): De crystallorum cohaesione, Diss.
Vratislaviae.
91. Frankenheim, M.L. (1831): Z. Phys. Math., 9, 94106, 194208,
332357.
92. Franz, R. (1850): De corporum duritie eamque metiendi
methodo, Diss. inaug. Bonnae 1850. Also in: Ann.d. Physik u.
Chemie, 80, 3755.
93. Fro hlich, F., Grau, P., Grellmann, W. (1977): Phys. Status Solidi,
42, 7989.
94. Gane, N., Cox, J.M. (1971): Philos. Mag. A, 881891.
95. Gane, N. (1970): Proc. R. Soc. A, 317, 367391.
96. Gao, H., Huang, Y., Nix, W.D. (1999a): Naturwissenschaften, 86,
507515.
97. Gao, H., Huang, Y., Nix, W.D., Hutchinson, J.W. (1999b):
Theory J. Mech. Phys. Solids, 47, 12391263.
98. Ge, D., Domnich, V., Gogotsi, Y. (2003): J. Appl. Phys., 93, 2418
2423.
99. Gerberich, W.W., Gao, H., Sundgren, J.-E., Baker, S.P. (eds.)
(1996): Thin films: stresses and mechanical properties VI, MRS
100. Gerberich, W.W., Tymiak, N.I., Grunlan, J.C., Horstemeyer,
M.F. (2002): J. Appl. Mech., Trans. ASME, 69, 433442.
101. Gerk, A.P., Tabor, D. (1978): Nature 271, 732733.
102. Geyer, B., Bartsch, M., Feuerbacher, M., Urban, K.,
Messerschmidt, U. (2000): Philos. Mag. A, 80, 11511163.
103. Ghosh, S., Das, S., Bandyopadhayay, T.K., Bandyopadhyay,
P.P., Chattopadhyay, A.B. (2003): J. Mater. Sci., 38, 15651572.
104. Giacometti, E., Baluc, N., Bonneville, J., Rabier, J. (1999): Scripta
Mater., 41, 989994.
105. Giannakopoulos, A.E., Suresh, S. (1999): Scripta Mater., 40,
11911198.
106. Gilman, J.J. (1993): Philos. Mag. B, 67, 207214.
P
u
b
l
i
s
h
e
d

b
y

M
a
n
e
y

P
u
b
l
i
s
h
i
n
g

(
c
)

I
O
M

C
o
m
m
u
n
i
c
a
t
i
o
n
s

L
t
d
107. Glazov, V.M., Vigdorovic, V.N. (1962): Mikrotverdost Metallov.
Gos.Naucn.-techn. zd.Lit. C
ern. C vetn. Metall., Moscow.

108. Glazov, V.M., Vigdorovic, V.N. (1971): Microhardness of metals
and semiconductors, New York, Consultants Bureau.
109. Golovin, Yu.I., Ivolgin, V.I., Khonik, V.A., Kitagawa, K.,
Tyurin, A.I. (2001): Scripta Mater., 45, 947952.
110. Golovin, Yu.I., Tyurin, A.I., Farber, B.Ya. (2002): Philos. Mag.
A, 82, 18571864.
111. Gong, J., Li, Y. (2000): J. Mater. Sci., 35, 209213.
112. Gong, J., Miao, H., Zhao, Z., Guan, Z. (2001): Mater. Sci. Eng.
A, 303, 179186.
113. Grailich, J., Pekarek, F. (1854): Sitzungsber. d. kaiserl. Akademie
d. Wiss., Math.-Naturw. Cl., Vienna, 13, 410436.
114. Grau, P., Berg, G., Meinhard, H., Mosch, S. (1998): J. Am.
Ceram. Soc., 81, 15571564.
115. Greer, A.L., Walker, I.T. (2002): Mater. Sci. Forum, 386388, 77.
116. Greer, A.L., Castellero, A., Magde, S.V., Walker, I.T., Wilde,
J.R. (2004): Mater. Sci. Eng. A, 37577, 11821185.
117. Gridneva, I.V., Milman, Yu.V., Trefilov, V.I. (1972): Phys. Status
Solidi (a), 14, 177182.
118. Grigorovic, V.K. (1976): Tverdost i mikrotverdost metallov. Izd.
Nauka, Moscow.
119. Grodzinski, P. (1951): Mikroskopie 6, 118120; J. Sci. Instrum.,
28, 117121.
120. Haberl, B., Bradby, J.E., Swain, M.V., Williams, J.S., Munroe, P.
(2004): Appl. Phys. Lett., 85, 55595561.
121. Haggag, F.M., Nanstad, R.K. (1989): in Innovative approaches
to irradiation damage and failure analysis, (ed. D.L. Marriott,
T.R. Mager, W.H. Bamford), PVP Vol. 170, 4146, New York,
American Society of Mechanical Engineers.
122. Haggag, F.M., Nanstad, R.K., Braski, D.N. (1989): Innovative
approaches to irradiation damage and failure analysis, (ed. D.L.
Marriott, T.R. Mager, W.H. Bamford), PVP Vol. 170, 101107,
New York, American Society of Mechanical Engineers.
123. Haggag, F.M., Nanstad, R.K., Hutton, J.T., Thomas, D.L.,
Swain, R.L. (1990): in Applications of automation technology to
fatigue and fracture testing, (ed. A.A. Braun, N.E. Ashbaugh,
F.M. Smith), ASTM 1092, 188208, Philadelphia, PA, USA,
American Society for Testing and Materials.
124. Hainsworth, S.V., Chandler, H.W., Page, T.F. (1996): J. Mater.
Res., 14, 22832295.
125. Hanneman, R.E., Westbrook, J.W. (1986): Philos. Mag., 18, 73.
126. Hau y, R.J. (1801): Traite de mineralogie, Tome Premier, 268
271, Paris, Louis.
127. Hays, C., Kendall, E.G. (1973): Metallography, 6, 275282.
128. Hertz, H. (1882): Verh. d. phys. Gesellsch. in Berlin, 1, 6769;
(1882): J. Reine Angew. Math., 92, 156.
129. Hill, R., Lee, E.H., Tupper, S.J. (1947): Proc. R. Soc. A, 188, 273
289.
130. Hirst, W., Howse, M.G.J.W. (1969): Proc. R. Soc. A, 311, 429
444.
131. Ho, S.-T., Chang, Y.-H., Lin, H.-N. (2004): J. Appl. Phys., 96,
35623564.
132. Hu, J.Z., Merkle, L.D., Menoni, C.S., Spain, I.L. (1986): Phys.
Rev. B, 34, 46794684.
133. Huang, Y., Gao, H., Nix, W.D., Hutchinson, J.W. (2001): Anal. J.
Mech. Phys. Solids, 48, 99128.
134. Hughes, G.D., Smith, S.D., Pande, C.S., Johnson, H.R.,
Armstrong, R.W. (1986): Scripta Metall., 20, 9397.
135. Huygens, C.H.R. (1690): Traite de la lumie`re, 70, Gressner &
Schramm, Lipsiae.
136. Inoue, A. (2000): Acta Mater., 48, 279306.
137. Jaggar, T.A. (1898): Z. Kristallogr., 29, 262275.
138. Jana, S., Bhowmick, R., Kawamura, Y., Chattopadhyay, K.,
Ramamurty, U. (2004a): Intermetallics, 12, 10971102.
139. Jana, S., Ramamurthy, U., Chattopadhyay, K., Kawamura, Y.
(2004b): Mater. Sci. Eng. A, 37577, 11911195.
140. Jang, J.S.C., Koch, C.C. (1999): Scripta Mater., 24, 599.
141. Jannettaz, P., Goldberg, M. (1895): Assoc. franc. p. lavanc. d. sc.
9 Aug, Abstract in: Z. Kristallogr., 28 (1897) 103.
142. Jiang, W.H., Atzmon, M. (2003): J. Mater. Res., 18, 755757.
143. Johnson, W.L. (2002): JOM, 54, 4043.
144. Johnson, K.L. (1996): Contact mechanics, Cambridge,
Cambridge University Press.
145. Johnson, K.L. (1970): J. Mech. Phys. Solids, 18, 115126.
146. Joslin, D.L., Oliver, W.C. (1990): J. Mater. Res., 5, 123126.
147. Journal of Materials Research (special issue) (1999): 14, 2196
2350; (2004): 19, 1396.
148. Juskin, N.P. (1971): Mechaniceskie svojstva mineralov, Izd.
Nauka, Leningrad.
149. Kailer, A., Gogotsi, Y.G., Nickel, K.G. (1997): J. Appl. Phys., 81,
30573063.
150. Kang, S.S., Dubois, J.M. (1992a): Europhys. Lett., 18, 4551.
151. Kang, S.S., Dubois, J.M. (1992b): Philos. Mag. A, 66, 151163.
152. Kaupp, G., Naimi-Jamal, M.R. (2004): Z. Metallkd., 95, 297305.
153. Kick, F. (1885): Das Gesetz der proportonalen Windersta nde und
Wissenschaftsanwendung, Leipzig, Felix, referred to in C. Hays
and E.G. Kendall, Metallography, 6 (1973) 275282.
154. Kiely, J.D., Jarausch, K.F., Houston, J.E., Russel, P.E. (1999):
J. Mater. Res., 14, 22192227.
155. Kim, J.-J., Choi, Y., Suresh, S., Argon, A.S. (2002): Science, 295,
654657.
156. Kimura, H., Masumoto, T. (1983): in Amorphous metallic
alloys, (ed. F.E. Luborsky), 187, London, Butterworth & Co.
Ltd.
157. Kirsten, C.H., Paufler, P., Schulze, G.E.R. (1964): Mtber. Dt.
Akad. Wiss., Math.-Naturw. Kl., 51, Heft 5, Akademie-Verlag
Berlin, 124.
158. Klemm, W., Smekal, A. (1941): Naturwissenschaften, 29, 688690.
159. Knoop, F., Peters, C.G., Emerson, W.B. (1939): Natl. Bur. Stand.,
23(1), 39.
160. Koch, C.C., Narayan, J. (2001): Mater. Res. Soc. Symp. Proc.,
634, B5
.
1
.
1B.5
.
1
.
11.
161. Ko ster, U., Liu, W., Liebertz, H., Michel, M. (1993): J. Non-
Cryst. Solids, 153&154, 446452.
162. Kupsch, A., Meyer, D.C., Gille, P., Paufler, P. (2001):
Z. Kristallogr., 216, 607610.
163. Lawn, B.R., Howes, V.R. (1981): J. Mater. Sci., 16, 27452752.
164. Lee, S.M., Kim, B.H., Kim, W.T., Kim, D.H. (2001): Mater. Res.
Soc. Symp. Proc., 643, K2
.
6
.
1K2
.
6
.
6.
165. Li, H., Bradt, R.C. (1991): Mater. Sci. Eng. A, 142, 5161.
166. Li, H., Bradt, R.C. (1993): J. Mater. Sci., 28, 917926.
167. Li, H., Bradt, R.C. (1996): J. Mater. Sci., 31, 10651070.
168. Li, H., Ghosh, A., Han, V.H., Bradt, R.C. (1993): J. Mater. Res.,
8, 10281032.
169. Li, X., Zhang, L., Gao, H. (2004): J. Phys. D: Appl. Phys., 37,
735757.
170. Lim, Y.Y., Chaudhuri, M.M. (1999): Philos. Mag A, 79, 2979
3000.
171. Linne, C. (1768): Systema naturae, Tom. III, Holmiae.
172. Linne, C. (1793): Systema naturae, Tom. III, 13th edn, J.F.
Gmelin, Lipsiae.
173. Lips, E.M.H. (1937): Z. Metallkd., 29, 339340.
174. Lips, E.M.H., Sack, J. (1936): Nature, 138, 328329.
175. Liu, X.B., Yang, G.C., Fan, P. (2003): J. Mater. Sci. Lett., 22,
611613.
176. Lockett, F.J. (1963): J. Mech. Phys. Solids, 11, 345.
177. Lorenz, D. (2001): Thesis, Martin-Luther Universita t Halle-
Wittenberg.
178. Lorenz, D., Zeckzer, A., Hilpert, U., Grau, P., Johansen, H.,
Leipner, H.S. (2003): Phys. Rev. B, 67, 172101-14.
179. Lu, K., Wei, W.D., Wang, J.T. (1990): Scripta Metall. Mater., 24,
23192323.
180. Lucazeau, G., Abello, L. (1997): J. Mater. Res., 12, 22622273.
181. Ludwik, P. (1908): Die Kegelprobe, Berlin, Springer.
182. Ma, Q., Clarke, D.R. (1995): J. Mater. Res., 10, 853863.
183. Madelung, E. (1942): Naturwissenschaften, 30, 223224.
184. Malow, T.R., Koch, C.C., Miraglia, P.Q., Murty, K.L. (1998):
Mater. Sci. Eng., 252, 3643.
185. Malzbender, J. (2003): J. Eur. Ceram. Soc., 23, 13551359.
186. Mann, A.B., Van Heerden, D., Pethica, J.B., Bowes, P., Weihs,
T.P. (2002): Philos. Mag. A, 82, 19211929.
187. Mann, A.B., Van Heerden, D., Pethica, J.B., Weihs, T.P. (2000):
J. Mater. Res., 15, 17541758.
188. Marsh, D.M. (1964): Proc. R. Soc. Lond. A, 279, 420.
189. Martens, A. (1898): Handbuch der Materialienkunde fu r den
Maschinenbau, Vol. I, 241, Berlin, Springer.
190. Marx, V., Blake, H. (1997): Acta Mater., 45, 37913800.
191. Mathew, M.D., Murty, K.L., Rao, K.B.S., Mannan, S.L. (1999):
Mater. Sci. Eng. A, 24, 159166.
192. Mcelhaney, K.W., Vlassak, J.J., Nix, W.D. (1998): J. Mater. Res.,
13, 13001306.
193. Mencik, J., Swain, M.V. (1994): Mater. Forum, 18, 277288.
194. Messerschmidt, U., Bartsch, M., Geyer, B., Feuerbacher, M.,
Urban, K. (2000): Philos. Mag. A, 80, 11651181.
195. Meyer, E. (1908): Z. d. Ver. Deutscher Ingenieure, 52, 645654,
740748, 835844.
196. Michel, M. (1992): Diploma thesis, University of Dortmund.
197. Michler, M., Dommann, A. (2001): Z. Metallkd., 92, 10351039.
198. Minowa, K., Sumino, K. (1992): Phys. Rev. Lett., 69, 320322.
P
u
b
l
i
s
h
e
d

b
y

M
a
n
e
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(
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u
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i
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L
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d
199. von Mises, R. (1913): Nachr.v. d. Konigl. Gesellsch.d.Wiss. zu
Gottingen, math.-phys. Klasse 582592.
200. Mirshams, R.A., Parakala, P. (2004): Mater. Sci. Eng. A, 372,
252260.
201. Mitsche, R. (1948): Osterr. Chem. Z., 49, 186.
202. Mohs, F. (1812): Versuch einer Elementar-Methode zur natur-
historischen Bestimmung und Erkennung der Foilien, Erster
Theil, 910, Vienna, Camesinische Buchhandlung.
203. Mohs, F. (1822): Grund-Ri der Mineralogie, Erster Theil, 374
382, Dresden, Arnoldische Buchhandlung.
204. Moody, N.R., Gerberich, W.W., Burnhan, N., Baker, S.P. (eds.)
(1998): Fundamentals of nanoindentation and nanotribology,
MRS Symposium Proc. 522. Pittsburgh, PA, Materials Research
Society.
205. Mott, B.W. (1956): Micro-indentation hardness testing, London,
Butterworth Scientific Publications.
206. Mukhopadhyay, N.K. (2005): J. Mater. Sci. 40, 241244.
207. Mukhopadhyay, N.K., Bhatt, J., Pramanick, A.K., Murty, B.S.,
Paufler, P. (2004): J. Mater. Sci., 39, 51555159.
208. Mukhopadhyay, N.K., Sarma, V.S., Sankaran, S. (2005): Trans.
Ind. Inst. Metals, 58, 809818.
209. Mukhopadhyay, N.K., Weatherly, G.C., Embury, J.D. (2001):
Mater. Sci. Eng. A, 315, 202210.
210. Mukhopadhyay, N.K., Belger, A., Paufler, P., Gille, P. (2006a):
Philos. Mag., 86, 9991006.
211. Mukhopadhyay, N.K., Belger, A., Paufler, P., Kim, D.H. (2006b):
Mater. Sci. Eng. A, to be published.
212. Mulhearn, T.O. (1959): J. Mech. Phys. Solids, 7, 8596.
213. Muraki, N., Katagiri, G., Sergo, V., Pezzotti, G., Nishida, T.
(1997): J. Mater. Sci., 32, 54195423.
214. Murthy, G.V.S., Ray, A.K., Minz, R.K., Mukhopadhyay, N.K.
(1999): J. Mater. Sci. Lett., 18, 255258.
215. Murty, K.L., Mathew, M.D. (2004): Nuclear Eng. Design, 328,
8186.
216. Murty, K.L., Miraglia, P.Q., Mathew, M.D., Shah, V.N.,
Haggag, F.M. (1999): Int. J. Pressure Vessels Piping, 76, 361369.
217. Murty, K.L., Mathew, M.D., Wang, Y., Shah, V.N., Haggag,
F.M. (1998): Int. J. Pressure Vessels Piping, 75, 831840.
218. Ni, W., Cheng, Y.-T., Grummon, D.S. (2002): Appl. Phys. Lett.,
80, 33103312.
219. Nieh, T.G., Schuh, C.A., Wadsworth, J., Li, Y. (2002):
Intermetallics, 10, 11771182.
220. Nieman, G.W., Weertman, J.R., Siegel, R.W. (1989): Scripta
Metall., 23, 20132018.
221. Nix, W.D., Gao, H. (1998): J. Mech. Phys. Solids, 46, 411425.
222. Novikov, N.V., Dub, S.N., Milman, Yu.I., Gridneva, I.V. (1996):
J. Superhard Mater., 18, 32.
223. Oliver, W.C., Pharr, G.M. (1992): J. Mater. Res., 7, 15641583.
224. Oliver, W.C., Pharr, G.M. (2004): J. Mater. Res., 19, 320.
225. Onitsch, E.M. (1947): Mikroskopie, 2, 131.
226. Ozakan, C.S., Cammarata, R.C., Freund, L.B., Gao, H. (eds.)
(2001): Thin films: stresses and mechanical properties IX, MRS
227. Page, T.F., Oliver, W.C., McHargue, C.J. (1992): J. Mater. Res.,
7, 450473.
228. Palumbo, G., Erb, U., Aust, K.T. (1990): Scripta Metall. Mater.,
24, 23472350.
229. Patnaik, M.N.M., Narasimhan, R., Ramamurty, U. (2004): Acta
Mater., 52, 33353345.
230. Paufler, P., Wolf, B. (2003): in Quasicrystals, (ed. H.-R. Trebin),
501522, WileyVCH.
231. Peng, Z., Gong, J., Miao, H. (2004): J. Eur. Ceram. Soc., 24,
21932201.
232. Pethica, J.B., Taylor, D. (1979): Surf. Sci., 89, 182.
233. Petty, E.R. (1971): in Techniques of metals research, (ed. R.F.
Bunshah ),Vol. 5, Part 2, 157221, John Wiley.
234. Pfaff, F. (1883): Sitzungsber. d. math.-phys. Classe d. k.b.
Akademie d. Wiss. Mu nchen 13, 5568 and 372; Abstract in
Z. Kristallogr., 1885, 10, 528531.
235. Pfaff, F. (1884): Sitzungsber. d. math.-phys. Classe d. k.b.
Akademie d. Wiss. Mu nchen 14, 255; Abstract in Z. Kristallogr.,
1885, 10, 531532.
236. Philosophical Magazine A (special issue) (1996): 74; (2002): 82,
18072231.
237. Pohlenz, F., Hermann, K., Seemann, R., Menelao, F. (2001):
Z. Metallkd., 92, 931.
238. Poole, W.J., Ashby, M.F., Fleck, N.A. (1996): Scripta Mater., 34,
559564.
239. Po schl, V. (1909): Die Ha rte der festen Ko rper und ihre
physikalisch-chemische Bedeutung, Dresden, Steinkopff.
240. Prandtl, L. (1920): Go ttinger Nachr. Math. Phys. KL. 74, 37;
(1920): Nachr. v.d. Ko nigl. Gesellsch.d.Wiss. zu Go ttingen,
math.-phys. Klasse, 7485.
241. Prandtl, L. (1921): Z. Angew. Math. Mech., 1, 1520.
242. Qui, X., Huang, Y., Nix, W.D., Hwang, K.C., Gao, H. (2001):
Acta Mater., 49, 39493958.
243. Quinn, J.B., Quinn, G.D. (1997): J. Mater. Sci., 32, 43314346.
244. Ramamurty, U., Jana, S., Kawamura, Y., Chattopadhyay, K.
(2005): Acta Mater., 53, 705717.
245. Ray, A.K., Das, G., Mukhopadhyay, N.K., Bhattacharya, D.K.,
Dwarakadasa, E.S., Parida, N. (1999): Bull. Mater. Sci., 22, 25
32.
246. Reaumur, R.A.F. de (1722): Lart de convertir le fer forge en
acier, et lart dadoucir le fer fondu, Paris, Michel Brunet.
247. Reibold, M., Belger, A., Mukhopadhyay, N.K., Gille, P., Paufler,
P. (2005): Phys. Status Solidi (a), 202, 22672276.
248. Ren, X.J., Hooper, R.M., Griffiths, C., Henshall, J.L. (2002):
Philos. Mag. A, 82, 21132120.
249. Reynolds, G.A.M., Golding, B., Kortan, A.R., Parsey, J.M.
(1990): Phys. Rev., B41, 11941195.
250. Riontino, G., Massazza, M. (2004): Philos. Mag., 84, 967981.
251. Rockwell, S.R. (1922): Trans. Am. Soc. Steel Treat., 2, 1013.
252. Rosiwal, A. (1896): Verhandl. d. k. k. geolog. Reichsanst. Wien,
17, 475.
253. Rother, B., Dietrich, D.A. (1994): Phys. Status Solidi, 142, 389
407.
254. Rother, B. (1995): J. Mater. Sci., 30, 53945398.
255. Sainfort, P., Dubost, B. (1988): in Quasicrystalline materials, (ed.
Ch. Janot and J.-M. Dubois), Singapore, World Scientific, 361
371.
256. Sakai, M. (1993): Acta Metal. Mater., 41, 17511758.
257. Samuels, L.E. (1986): in Microindentation techniques in materi-
als science and engineering, ASTM STP 889, (ed. P.J. Blau, B.R.
Lawn), Philadelphia, PA, USA, ASTM.
258. Samuels, L.E., Mulhearn, T.O. (1957): J. Mech. Phys. Solids, 5,
125.
259. Sangwal, K. (2000): Met. Chem. Phys., 63, 145152.
260. Sangwal, K. (1989): J. Mater. Sci., 24, 1128.
261. Sargent, P.M. (1986): in Microindentation techniques in materi-
als science and engineering, AST STP 889, (ed. P.J. Blau, B.R.
Lawn), 160174, Philadelphia, PA, ASTM.
262. Sargent, P.M., Donovan, P.E. (1982): Scripta Metall., 16, 1207
1212.
263. Sauthoff, G. (1995): Intermetallics, 501, Weinheim, VCH.
264. Schuh, C.A., Nieh, T.G. (2003): Acta Mater., 51, 8799.
265. Schuh, C.A., Nieh, T.G. (2004): J. Mater. Res., 19, 4657.
266. Schuh, C.A., Nieh, T.G., Kawamura, Y. (2002): J. Mater. Res.,
17, 16511654.
267. Schulze, G.E.R., Paufler, P. (1972): Abhandlg. Sachs. Akad. Wiss.,
Math.-Naturwiss. Kl., 51, Heft 5, Akademie-Verlag Berlin, 124.
268. Schwaiger, R., Moser, B., Dao, M., Chollacoop, N., Suresh, S.
(2003): Acta Mater., 51, 51595172.
269. Seebeck, A. (1833): Pru fungs-Programm des Co lnischen
Realgymnasiums, Berlin.
270. Seok, C.S., Murty, K.L. (2000): Int. J. Pressure Vessels Piping, 77,
303311.
271. Shaw, G.A., Stone, D.S., Johnson, A.D., Ellis, A.B., Crone, W.C.
(2003): Appl. Phys. Lett., 83, 257259.
272. Shaz, M.A., Mukhopadhyay, N.K., Mandal, R.K., Srivastava,
O.N. (2002): J. Alloys Comp., 342, 4952.
273. Sklerometrija (1968): Izd. Nauka, Moscow.
274. Smith, R., Sandland, G. (1925): J. Iron Steel Inst., 111, 285294.
275. Sneddon, I.N. (1965): Int. J. Eng. Sci., 3, 4757.
276. Spoor, P.S., Maynard, J.D. (2001): in Handbook of elastic
properties of solids, liquids, gases, Vol. II (ed. M. Levy) 125141,
San Diego, CA, Academic Press.
277. Stelmashenko, N.A., Walls, M.G., Brown, L.M., Milman, Y.V.
(1993): Acta Metall. Mater., 41, 28552865.
278. Sterzel, R., Hinkel, C., Haas, A., Langsdorf, A., Bruls, G.,
Assmus, W. (2000): Europhys. Lett., 49, 742747.
279. Swadener, J.G., Misra, A., Hoagland, R.G., Nastasi, M. (2002):
Scripta. Mater., 47, 343348.
280. Tabor, D. (1951): The hardness of metals, Oxford, Clarendon
Press.
281. Tabor, D. (1986): in Microindentation techniques in materials
science and engineering, ASTM STP 889, (ed. P.J. Blau, B.R.
Lawn), 129159, Philadelphia, PA, USA, ASTM.
282. Takeuchi, S., Iwanaga, H., Shibuya, T. (1991): Jpn. J. Appl. Phys.,
30, 561562.
P
u
b
l
i
s
h
e
d

b
y

M
a
n
e
y

P
u
b
l
i
s
h
i
n
g

(
c
)

I
O
M

C
o
m
m
u
n
i
c
a
t
i
o
n
s

L
t
d
283. Tanaka, K., Mitarai, Y., Koiwa, M. (1996): Philos. Mag., A73,
17151723.
284. Tertsch, H. (1949): Die Festigkeitserscheinungen der Kristalle,
171257, Vienna, Springer-Verlag.
285. Timoshenko, S., Goodier, J.N. (1951): Theory of elasticity, 2nd
edn, New York, McGraw Hill.
286. Trebin, H.-R. (1999): Mater. Res. Soc. Symp. Proc., 553, 337343.
287. Tymiak, N.I., Daugela, A., Wyrobek, T.J., Warren, O.L. (2004):
Acta Mater., 52, 533563.
288. Turley, D.M., Samuels, L.E. (1981): Metallography, 14b, 275294.
289. Turner, T. (1886): Proc. Philos. Soc. Birmingham, 5, 282312.
290. Upit, G.P., Varchenya, S.A. (1973): in The science of hardness
testing and its research applications, (ed. J.H. Westbrook, H.
Conrad), 135146, Metals Park, OH, ASTM.
291. Urban, K., Feuerbacher, M., Wollgarten, M. (2002): In
Quasicrystals, (ed. J.-B. Suck, M. Schreiber, P. Ha ussler), 305
318, Berlin, Springer-Verlag.
292. Urban, K., Feuerbacher, M., Wollgarten, M., Bartsch, M.,
Messerschmidt, U. (1999): In Physical properties of quasicrys-
tals, (ed. Z.M. Stadnik), 361401, Berlin, Springer-Verlag.
293. Vaidyanathan, R., Dao, M., Ravichandran, G., Suresh, S. (2001):
Acta Mater.,49, 37813789.
294. Valiev, R.J., Chmelik, F., Bordeaux, F., Kapeiski, G., Bandelet,
B. (1992): Scripta Metall. Mater., 24, 855.
295. Vanderwal, J.J., Zhao, P., Walton, D. (1992): Phys. Rev., B46,
501502.
296. Veprek, S. (1999): J. Vac. Sci. Technol. A, 17, 2401.
297. Veprek, S., Niederhofer, A., Moto, K., Bolom, T., Mannling,
H.D., Nesladek, P., Dollinger, G., Bergmaier, A. (2000): Surf.
Coatings Technol., 133134, 152159.
298. Vitovec, F.H. (1986): in Microindentation techniques in materials
science and engineering, ASTM STP 889, (ed. P.J. Blau, B.R.
Lawn), 175185, Philadelphia, PA, USA, ASTM.
299. Vinci, R., Kraft, O., Moody, N., Besser, P., Shaffer, E. (eds.)
(1999): Thin films: stresses and mechanical properties VIII, MRS
300. Wang, J.G., Choi, B.W., Nieh, T.G., Liu, C.T. (2000): J. Mater.
Res., 15, 798807.
301. Wang, N., Wang, Z., Aust, K.T., Erb, U. (1995): Acta Metall.
Mater., 43, 519528.
302. Wei, Y., Wang, X., Zhao, M. (2004): J. Mater. Res., 19, 208217.
303. Werner, G.A. (1774): Von den a uerlichen Kennzeichen der
Foilien, Leipzig, S.L. Crusius.
304. Westbrook, J.H. (1967): in Environment-sensitive mechanical
behaviour, (ed. A.R.C. Westwood, N.S. Stoloff), 247, New York,
Gordon and Breach.
305. Westbrook, J.H., Conrad, H. (eds.) (1973): The science of
hardness and its research applications, Metals Park, OH, ASTM.
306. Williams, J.S., Chen, Y., Wong-Leung, J., Kerr, A., Swain, M.V.
(1999): J. Mater. Res., 14, 23382343.
307. Wittmann, R., Urban, K., Schandl, M., Hornbogen, E. (1991):
J. Mater. Res., 6, 11651168.
308. Wolf, B., Paufler, P. (1999a): Phys. Status Solidi (a), 172, 341
361.
309. Wolf, B., Paufler, P. (1999b): Surf. Interface Anal., 27, 592
599.
310. Wolf, B., Paufler, P. (1999c): Microsc. Anal., Nov., 2527.
311. Wolf, B., Paufler, P. (2001): Proceedings of the NATO Advanced
Study Institute on Fundamentals of tribology and bridging
the gap between the macro- and micro/nanoscales, vol. 10 (ed.
B. Bhushan), Keszthely, Hungary, August 2000, Academic
Publishers, Dordrecht, 549556.
312. Wolf, B., Bambauer, K.-O., Paufler, P., 2001, Mater. Sci. Eng.,
A298, 284295.
313. Wolf, B., Deus, C., Paufler, P. (1997): Surf. Interface Anal., 25,
561568.
314. Wolf, B., Swain, M., Kempf, M., Paufler, P. (2000): J. Mater. Sci.,
35, 723734.
315. Wollgarten, M., Saka, H. (1997): in New horizons in quasicrys-
tals, (ed. A.I. Goldman, D.J. Sordelet, P.A. Thiel, J.M. Dubois),
World Scientific.
316. Wollgarten, M., Saka, H., Inoue, A. (1999): Philos. Mag. A, 79,
21952208.
317. Wright, W.J., Saha, R., Nix, W.D. (2001): Mater. Trans. JIM, 42,
642649.
318. Wu, J.S., Brien, V., Brunet, P., Dong, C., Dubois, J.M. (2000):
Philos. Mag. A, 80, 16451655.
319. Wu, Y.Q., Yang, X.Y., Xu, Y.B. (1999): Acta Mater., 47, 2431
2436.
320. Yan, Y., Zhang, Z., Wang, R. (1994): Philos. Mag. Lett., 69, 123
130.
321. Yokoyama, Y., Inoue, A., Masumoto, T. (1993): Mater. Trans.
JIM, 34, 135145.
322. Yu, W., Blanchard, J.P. (1996): J. Mater. Res., 11, 23582367.
323. Zarudi, I., Zhang, L.C., Swain, M.V. (2003): Appl. Phys. Lett., 82,
10271029.
324. Zarzour, J.F., Konkel, P.J., Dong, H. (1996): Mater. Character.,
37, 195209.
325. Zhang, T.Y., Xu, W.H. (2002): J. Mater. Res., 17, 1715.
326. Zhang, T.Y., Xu, W.H., Zhao, M.H. (2004): Acta Mater., 52, 57
68.

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