Aspects of Strain and Strength Measurement in Miniaturised Testing For Engineering Metals and Ceramics

25 YEAR PERSPECTIVE
Aspects of strain and strength measurement

in miniaturised testing for engineering metals
and ceramics
J. D. Lord*1, B. Roebuck1, R. Morrell1 and T. Lube2
Testing in the microregime is relevant to many technological issues, including, for example,
evaluating the performance of established plant or new components through removal of small
scale samples; assessing point to point variation in welded structures; characterising expensive
advanced alloys that typically are only available in small quantities; and testing of subsized
components. The use of miniature testpieces requires attention to the scale of the underlying
microstructure relative to the overall testpiece dimensions, and presents challenges to the
measurement of stress and strain in small volumes. The subject is extensive and the emphasis of
the current paper is on a discussion of issues associated with the measurement of strength and
strain, particularly with the latter assessed using non-contact optical techniques based on digital
image correlation. The current article thus concentrates on the testing situation at the intermediate
scale (in the range 0?5–5 mm) where testpieces are small compared with the size of engineering
components and in the range where representative mechanical behaviour of the underlying
microstructure must be considered. Metrology issues are addressed through specific case
studies concerning; microuniaxial tests; small punch tests; subsized ceramic strength tests and
the microindentation technique. Particular attention is paid to the uncertainties in measurement
arising from the use of microscale tests to provide quantifiable levels of confidence in the ability of
such tests to discriminate material behaviour.
Keywords: Microscale tests, Mechanical properties, Small punch tests, Digital image correlation, Microindentation, Strain measurement, Review
Introduction and scope lifetimes by aging, i.e. the mechanical characteristics of

structural materials change with time or use, or through
With the drive for improved reliability and sustainability other changes in the loading and operating cycle. An
engineering components and structures are expected to understanding of the change in mechanical properties of
remain longer in service, possibly for years or decades structural components is therefore necessary for opti-
beyond their original design lifetimes. They will experi- mising operating procedures, inspection intervals, repair
ence high fluctuating loads and temperatures and strategies and lifetime assessments. The remanent life of
operate under environmental conditions that degrade structures is often assessed using destructive tests on
long-term properties. Exposure to elevated temperatures specimens obtained from actual components, especially
for long times results in damage processes that impair as the local microstructures are determined by the prior
mechanical properties. The requirements for environ- manufacturing and performance history. In most cases
mental sustainability make it economical to extend the material is scarce (or only available in thin section) and
lifetime of existing components rather than build new tests on ‘miniaturised’ specimens allow a more extensive
plant. Thus, reducing uncertainty in the calculation of test programme to be carried out. Indeed, in some cases
the remanent life of plant is critical, and design this may be the only solution. Miniature testpieces are
procedures must ensure that failure does not occur important for use in predicting remanent life of plant
during the extended component life. Components and and equipment but only provided that the data
structures are designed with significant safety margins generated can be proven to be reliable. The character-
but these can be reduced throughout their service isation of the mechanical behaviour of high temperature
and other advanced alloys is particularly challenging.
Consider for example the gas turbine, where there is
1
National Physical Laboratory, Teddington, Middlesex, TW11 0LW, UK considerable effort on alloy development and the
2
Institut für Struktur- und Funktionskeramik, Montanuniversität Leoben, refurbishment of aging turbine parts. Typical Ni based
A8700, Austria alloys are costly and often only available in limited
*Corresponding author, email jerry.lord@npl.co.uk quantities, especially during the development of new
ß 2010 Crown copyright

Published by Maney on behalf of the Institute
Received 27 May 2009; accepted 16 November 2009
DOI 10.1179/026708309X12584564052012 Materials Science and Technology 2010 VOL 26 NO 2 127
Lord et al. Aspects of strain and strength measurement in miniaturised testing for engineering materials and ceramics
alloy grades. The alloys are often used in thin sections to strength and toughness, through to macroscale effects
with the wall thicknesses of a typical turbine blade often of direct concern to the engineer, for evaluating the most
being only a few millimetres and new techniques need to appropriate constitutive behaviour for use in finite
be developed and evaluated for assessing the degrada- element (FE) modelling of structural components. The
tion of thin walled turbine blades after service exposure. nanoscale in particular has attracted much attention in
Clearly microscale testing has a role to play in this recent years, with considerable research directed at the
respect. The very high test temperatures required need techniques of nanoindentation and micropillar testing.
specific attention to the design of grips and strain A selective list of references4–27 is included for the
measurement techniques; the use of conventional interested reader as it provides complementary insight
methods can be expensive and time consuming. for many of the issues discussed in the current paper,
Another example is the development of advanced highlighting mechanistic topics such as dislocation
technical ceramics, which are being employed in a wide source characteristics, dislocation generation, multi-
range of mechanical and electronic/functional applica- plication and annihilation mechanisms and testpiece
tions, and usually as device critical components. Often preparation methods and surface conditions that under-
the size of such products, such as chip capacitors, is as pin and affect the interpretation of these very small scale
small as 1 mm. Understanding the mechanical proper- tests. Despite the research effort there are still consider-
ties of such small components, especially in relatively able metrological issues to resolve and there is scope for
weak and brittle materials, is essential to maintaining an extensive review of nanoscale testing that brings
performance. Testing for design and quality assurance together much of the recent research published in a
requires new approaches compared with the more range of Physics, Materials and Engineering journals.
traditional approaches that have been adopted for Complementary modelling studies are especially
engineering-scale components. required to evaluate crystal plasticity effects and load
Optimising the test conditions for relevant miniature sharing between different phase constituents in multi-
tests is an important objective as the requirement for phase materials.28–32
correlating the results with data generated from full size The current article concentrates, however, on the
samples. The subject matter is extensive and draws the testing situation at the intermediate scale (in the range
attention of dedicated, focused meetings; for example, 0?5–5 mm) where testpieces are small compared with the
the ASTM extended series of conferences on small scale size of engineering components and in the range where
tests, with the most recent at Reno, Nevada in 2000 and representative mechanical behaviour of the underlying
Anaheim, California in 2007.1,2 The ASTM meetings microstructure must be considered. This viewpoint
have covered a wide range of topics, and particularly document is necessarily selective due to the wide range
emphasise miniature toughness tests. As such, discussion of definitions used to describe ‘microscale’ effects. For
of toughness has been omitted from the present paper example, tensile tests for microelectromechanical sys-
and the reader’s attention is directed to the ASTM tems and very thin films have been discussed in recent
references and a recent detailed review by Hyde et al.3 reviews33,34 highlighting problems such as accurate
that also covers the assessment of creep properties. This testpiece fabrication, gripping and strain measurement.
latter review highlights a number of generic issues The emphasis in the present paper is particularly aimed
associated with using miniature tests, which include: at discussing aspects of strain measurement and
(i) the requirement to have sufficient representative associated flow stress characterisation. Specific test
volume elements within the gauge volume methods discussed include miniature uniaxial, small
(ii) the necessity to ensure the effects of constraint punch, bend and microindentation, and all are evaluated
features (such as notches, edges and corners) are with case studies of ongoing research, both at National
addressed Physical Laboratory (NPL) and elsewhere, to highlight
(iii) the increased likelihood of probabilistic events some important metrological items. Many of the issues
from small heterogeneities impinging on gross relating to specimen preparation, representative cross-
mechanical behaviour sections, resolution and accuracy of the instrumentation
(iv) the lack of standardisation supported by inter- and test equipment still merit further assessment.
national round robins to validate microscale
test procedures.
To these can be added several more topics that are
Non-contact techniques for strain
touched upon in the current article: measurements
(i) the importance of specimen geometry, prepara- Strain measurement in microscale testing is particularly
tion and surface finish challenging, as the specimen dimensions, gauge lengths
(ii) the possibility of surface residual stresses influenc- and test fixtures are small. In most cases conventional
ing measured gross mechanical behaviour extensometry and strain gauges cannot be used and
(iii) the challenge of accurate strain measurement at other techniques must be investigated. Current solutions
these length scales include the use of line scan cameras and optical tech-
(iv) the utility of mechanical modelling to optimise niques, laser and digital speckle pattern interferometry,
testpiece geometries linear variable differential transformers (LVDTs), capa-
(v) the need to assess the statistical variation in citance gauges, and the change in electrical resistance.
data. Many of these techniques do not measure strain directly,
Scale effects in the mechanical behaviour of materials but measure displacement. Some make direct measure-
have long interested the material scientists, from ments on the testpiece but others such as LVDTs and
nanoscale physical metallurgy, understanding the con- capacitance gauge probes are usually integrated with the
tribution that dislocation generation and motion makes test fixture or load train and measure displacement
128 Materials Science and Technology 2010 VOL 26 NO 2

remotely. A summary of some of candidate displace- Figure 1 shows examples of typical full field strain
ment and strain measurement techniques being consid- distributions that can be measured using non-contact
ered for miniaturised testing are shown in Table 1. A techniques, a shear band captured during the tensile
general introduction and overview of some of these testing of an aluminium alloy, and strain distribution in
techniques is given by Sharpe35 and Eaton-Evans et al.36 a weld subjected to four-point flexure. In this case there
Most of the traditional techniques measure an average is a superimposed strain due to the bending, but the
strain value over a fixed gauge length and cannot technique can highlight local differences in strain
discriminate or resolve local behaviour. A significant associated with the heat affected zone and different
advantage of using non-contact optical techniques parts of the weld.
within the test system is the potential for full field The images in Fig. 1 were measured using digital
measurement, enabling local variations and non- image correlation (DIC), which is a full field non-contact
uniformity in the strain field due to stress concentra- strain measurement technique. It was first developed in
tions, defects, different phases, or orientations of the the 1980s38,39 but has seen significant development and
grains to be identified. uptake in recent years due to the availability of higher
Non-contact optical methods have other advantages; resolution cameras and increased computer power. It is
for example, remote sensing does not affect the a versatile tool and is being used extensively in con-
compliance of the system, as it would do if strain gauges ventional experimental mechanics in a diverse range of
or transducers were attached to small samples. They also applications for characterising material behaviour,
have the potential to provide high rates of data capture measuring the evolution and uniformity of strain,
and high precision with potential resolution in the sub mapping of strain fields around features and defects,
micrometre range. For example, a gauge length of 1 mm crack tip and crack propagation studies, dynamic
would require a displacement resolution of 0?5 mm to vibrational analyses, high temperature strain measure-
ensure strain accuracy of 0?05%, i.e. typically 50–100 ment, deformation of large structures, structural health
data points in the elastic region before yield in a low monitoring and FE validation.40 Digital image correla-
strength aluminium alloy. LaVan and Sharpe37 used a tion is already being used in a range of microscale
laser interferometric system to measure both sides of a testing.41–55
small sample and obtained reasonably accurate Young’s Digital image correlation works by comparing images
modulus values for a ferrous alloy. Obvious drawbacks of a component or testpiece at different stages of
with the optical methods are the requirement for line of deformation and tracking blocks of pixels to measure
sight to the testpiece, which for some test setups may not surface displacement and build up full field two- and
be possible. three-dimensional deformation vector fields and strain
Table 1 Advantages and disadvantages of some candidate strain and displacement measurement techniques for
miniaturised test systems
Techniques Advantages Disadvantages
LVDT (linear transducers) Readily available, sub micrometre resolution Measures displacement cf. strain, requires point
point displacement. contact.
Electrical resistance Cheap and direct method with simple analysis Only possible with electrically conducting
to provide plastic strain values. Excellent at materials. Only measures plastic strain values.
high temperatures right up to solidus. Requires additional calibration if phase changes
occur during the test to alter intrinsic resistivity
values.
Capacitance gauges High resolution displacement measurement. Average displacement measurement, requires
some physical contact, drift.
Line scan cameras Cheap, high resolution measurement. Two-dimensional mapping only possible with a
scanning system.
Moiré interferometry Non-contact, full field, real time. High High level of skill required. Grating must be
resolution displacement measurement. applied to the testpiece. Sensitive to environment
and rigid body motion.
Laser interferometry High resolution displacement and strain Reflective targets required. Sensitive to vibration
measurement (5 me). and rigid body motion.
Digital speckle pattern Full field, non-contact, measurement. High Expensive, sensitive to vibration. Requires a
interferometry sensitivity and spatial resolution. Two- and diffuse surface. Not suitable for large deformations
three-dimensional measurement capability. or rigid body motion.
High temperature capability.
Digital image correlation Full field, non-contact, two- and three- Modest strain resolution (0.01 pixel/100 me)
dimensional implementations available, wide depending on camera resolution and field of view,
range of cameras and suppliers. Can be used testpiece may require some surface pattern or
on SEM images. preparation.
Photoelastic stress analysis Full field, non-contact, direct measurement of Photoelastic coatings must be applied. Limited
stress and strain. temperature range, stress level may saturate.
Thermoelastic stress analysis Full field, non-contact, small scale applications. Requires cyclic load, only applicable to linear
elastic loading.
Materials Science and Technology 2010 VOL 26 NO 2 129

1 Examples of DIC strain mapping: shear band in aluminium alloy tensile sample (left), distribution of strain in weld
under four-point bending (right)
maps. The position of the centre of the pixel blocks is property measurement. The absolute strain resolution
determined to subpixel accuracy over the whole image depends on the camera resolution, field of view, scale of
using sophisticated correlation functions, from which the image relative to the pattern on the surface, the
the vector and strain components can be calculated. uniformity of strain in the testpiece, the number of pixels
Different DIC analysis solutions have been developed to in each pixel block, and the gauge length over which the
obtain subpixel resolution based on non-linear optimi- strain is calculated. Choices must be made about the size
sation techniques, intensity interpolation, Fourier trans- of the pixel blocks (also described as ‘facets’, ‘windows’,
form analyses, gradient based methods, correlation and ‘subsets’) as this effectively defines the gauge length
coefficient curve fitting, Newton–Raphson iteration for strain measurement and has an important influence
methods, genetic algorithms and neural networks. The on the spatial resolution and accuracy of the strain and
accuracy and sensitivities of the different approaches displacement measurement. Generally for uniform dis-
reported in the literature range from 0?5 to 0?01 pixel. placement fields, larger windows give better strain
Pan et al.42 carried out a systematic study of three types accuracy, while smaller windows give better spatial
of subpixel registration algorithms using the translation resolution. Table 2 (Ref. 43) summarises the calculated
of synthetically generated images. They concluded that errors and uncertainties that might be expected with
the Newton–Raphson methods are generally the most different window sizes.
accurate, but are very computer intensive and much An advantage of analysing the images with DIC is
slower than some of the other approaches. Also the that once the images have been captured they can be
gradient based methods are better than the curve fitting reprocessed using different window sizes and DIC para-
approach in terms of accuracy and sensitivity. meters to highlight different features on the testpiece.
For many applications the DIC analysis is carried out Digital image correlation requires a random pattern
off line, so the computing power required might not be on the sample, and different approaches can be used to
an issue, but with increasingly higher resolution cameras generate this including conventional polishing and
being available the processing of large image file sizes etching of the sample to reveal grain structure and
becomes more difficult and might be a factor in choosing texture, the application of a pattern to the testpiece
which approach to take. using a fine airbrush or applying light, random scratches
As noted above, depending on the subpixel algorithms to the surface. The scale of the pattern relative to the
used, the claimed resolution for two-dimensional DIC pixel size is important, and a consideration for measure-
approaches 0?01 pixel for displacement measurement. In ments made under the microscope or SEM where the
practice however, factors associated with the experi- application of a very fine random pattern is difficult.
mental setup, such as the quality of lighting, camera Uniform illumination is also essential and a dedicated
noise, lens distortion, the scale and type of pattern or local light source should be used to ensure consistency of
coating on the testpiece etc., will degrade the images and illumination throughout the test. LED ringlights offer a
affect the accuracy of the DIC calculations, so 0?1 pixel good solution particularly in combination with a macro
is probably more realistic. This means that for a or telecentric lens.
miniature testpiece with a gauge length of 10 mm and It should be noted that using a conventional small
a camera resolution of 1 megapixel, if the gauge length scale test machine with a fixed crosshead can lead to
fills the field of view, DIC will be able to resolve difficulties with DIC as the original part of the image
displacements to between 0?1 and 1 mm resolution. For can move out of the field of view and the correlation
full field studies the strain resolution is typically 100 me, breaks down. This can be overcome using a larger field
so is good for plastic deformation studies but less of view, multiple cameras that overlap, or designing a
reliable at small strain values, and challenging for elastic test machine where both grips move and the central
Table 2 Effect of DIC ‘window’ size on calculated accuracy of displacement and strain measurements43
Accuracy of calculated strain values

Size of DIC window (pixels) Accuracy of calculated vectors (pixels) (with 50% overlap)
1286128 0.01–0.03 0.094%

64664 0.02–0.05 0.30%
32632 0.05–0.2 1.25%
16616 0.1–0.3 5.0%

2 Real time DIC measurements on miniaturised tensile 4 Comparison of strain measured by image correlation
specimen in NPL ETMT, showing linear fit to data for and resistance changes
elastic modulus calculation
loads taken during the four-point bend testing of a small
gauge length of the testpiece remains at the centre of the 40 mm long graphite beam. Because of the size of the
image. testpiece and nature of the material it was not possible to
Digital image correlation is generally used as a full apply strain gauges or an LVDT (linear transducer) to
field application, but some variants of DIC software use monitor beam deflection, so DIC was used, focusing the
the tracking of discrete markers or features for measur- cameras on the side of the specimen. In combination
ing displacement and strain. Because the processing with FE modelling, the full field displacement data have
power required is much reduced there is scope for real been used successfully to measure the elastic modulus of
time measurement of displacement and strain over the graphite and also identify local variations in
several pairs of markers on the testpiece. Measure- properties associated with the structure of the material.
ments have been made on miniaturised tensile specimens Some researchers44,45 have used DIC to examine the
in NPL’s version (the electrothermal mechanical tester, constitutive properties of weld materials, generating
ETMT) of the mechanical system used by Peterson discrete stress–strain relationships for the parent metal,
et al.41 to examine the potential of the DIC technique for heat affected zone and weld zone all from a single
measuring elastic modulus. Figure 2 shows results from testpiece, and the variation of proof stress across a
a series of tests on a stainless steel 304 alloy. Although weld46 by monitoring the strain in discrete locations of
there is some scatter and noise in the data, due in part to the sample. Further examples of using the technique to
the load control, the fit through the data gives values of measure plastic deformation and local strain distribu-
modulus of 185 and 187 GPa for the two specimens, and tions include work to correlate strain measurements with
reasonable strain resolution (10 me) below that typically grain orientation in polycrystalline Al alloys,47 the
expected for full field DIC. examination of strain distributions in dual phase
Full field non-contact techniques open up the steels,48 strain localisation in thin sheet samples49
potential for a wide range of novel measurements and and an investigation of shear band formation and
applications. Figure 3 shows the x and y displacement development in Al alloys.50 A variation of the method
maps and series of displacement profiles at increasing by Moulart et al.51 combines white light interferometry
measurements in combination with the grid method
and DIC to study strain distributions in microscale
testpieces.
Images of testpiece deformation can be obtained from
a wide variety of sources and a range of scales, including
conventional charge coupled device or consumer digital
cameras, high speed video, microscopes, macroscopes,
the SEM and atom force microscopy. Good quality
measurements in the SEM are particularly challenging
due to the limited contrast, charging of the specimen,
noise and potential drift of images, but has been applied
successfully52–54 in combination with in situ loading
stages, for studying local strain fields, microplasticity
and strain heterogeneity in Ti alloys.53
Digital image correlation has been used successfully
for tracking markers on the testpiece with the NPL
ETMT at temperatures up to 800uC without special
cameras or infrared filters (Fig. 4). At high temperatures
there is an increased likelihood that thermal currents
and airflow in front of the lens will lead to distortion of
3 Displacement fields (x: top; y: middle) and mean dis- the image and breakdown of the correlation; techniques
placement profile (with increasing load) of miniaturised are being developed based on high speed sampling to
four-point bend test on graphite overcome this. Oxidation should be avoided by testing

in vacuum or inert atmosphere as this will lead to calculate applied stresses accurately. Sharpe62 also
changes in the surface appearance and a breakdown in advocates the use of grips mounted in linear air bearings
the correlation. Normally with DIC the images are to reduce friction, particularly with low strength
compared relative to the initial (unloaded/starting) state, testpieces. Some of the work reported was on 3?5 mm
but if there large deformations or changes to the surface thick polysilicon film and 200 mm thick electroplated
condition it is possible to do the correlation between nickel samples. Gauge lengths for strain measurement
successive images and generate cumulative strain fields. are necessarily short and lead to severe problems with
Potential issues with oxidation of testpieces or surface conventional extensometry for measuring displacement
diffusion effects changing the appearance of the testpiece and changes in shape. Considerable innovation is needed
surface with time can be overcome to some extent using to derive reliable strain values.
a robust and frequent monitoring regime to ensure that Microstructural features (e.g. the distribution of grain
the correlation does not break down between images. shape, phase, orientation, texture, precipitate distribu-
This may not work in all cases however. tion) and their size relative to the dimensions of the
Recent work examining the influence of specimen testpiece can have significant effects on flow stress.
dimensions and strain measurement methods on the Hoefnagels et al.63 used a non-contact optical strain
tensile stress–strain behaviour of bulk nanostructured measurement technique to examine the influence of
materials55 showed significant differences in the grain boundaries and grain statistics in pure Al by
stress–strain behaviour and ductilities. Results showed testing a range of miniaturised testpieces of different
that the post-yield elongation increased significantly as cross-sections. Results showed widely different deforma-
the gauge length was reduced and specimen thickness tion behaviour depending on the microstructure and
increased. The authors reiterate the use of accurate number of grains present, with inhomogeneous defor-
strain measurement techniques such as DIC and laser mation and localised slip bands occurring throughout
interferometry as the strains derived solely from the the tensile test on the thinnest testpieces, and more
crosshead displacement lead to significant errors. They homogeneous behaviour with the thicker testpieces due
also note the requirement for standardised test proce- to the greater number of grains and plane strain
dures to allow meaningful comparisons of data from conditions offering a greater level of constraint at the
different laboratories. grain boundaries. For a set value of grain size, because
grains close to the surface are under less constraint than
Miniature uniaxial tests those within the central regions of the testpiece, the
Microscale uniaxial tests are not yet standardised, except global flow stress of the sample will decrease as the
for the specific requirements for testing foil materials sample width and thickness decrease.56,57,60,66 This is
given in ASTM E345-93, but have the potential to opposite in effect to that found in the nanoindentation
provide uniaxial stress–strain data that is representative and micropillar tests where single orientation behaviour
of macro behaviour. It is important to be aware, is often being measured and a reduced scale of test is
however, of a number of metrological issues that can associated with increasing strength. Typically a thick-
have a significant influence on the quality and accuracy ness to grain size ratio of less than 10–12 has a
of the results,37,41,56–73 including: sample preparation; significant effect on measured properties,56 but currently
microstructural considerationsalignment; ductility; and there are no clear recommendations available on the
resolution of load cells and transducers. number of grains that should be sampled in the testpiece
Sample preparation methods, by their nature, result in cross-section. It is an important consideration but is
testpiece surfaces that may not be representative of the often specific to, and may be even limited by, the
underlying material. The volume of affected material is particular material under investigation.
clearly dependent on the method of preparation; i.e. Even in tensile tests for large samples, ductility is
grinding, polishing, electrodischarge machining, etc. and recognised to be sensitive to testpiece geometry, and
can be a significant percentage of the testpiece cross- standards such as ASTM E8M and ISO 6892 recom-
sectional area. Any damage or defects introduced during mend proportional geometries for round specimens
preparation may have a significant influence on the where the ratio of the gauge length to area (L/A1/2) is
behaviour and premature failure. typically set at 5?64 to enable comparability in ductility
Uniaxial tensile testing poses alignment challenges for values from samples ranging in diameter from 4 to
brittle or low ductility materials at the best of times, and 12?5 mm. It is likely that similar requirements will hold
these generally become worse as the scale is reduced, for smaller samples although this has yet to be system-
with the result that uniaxial testing is rarely performed, atically evaluated. More attention has generally been
since results are often unsatisfactory. Recourse is paid to strength values as opposed to measurements of
generally made to some form of flexural testing, ductility. For example, it was noted in a study of
although one novel example of indirect tension testing nanostructured materials that the strength/hardness
is described later in the section on ceramics. Misalign- correlation was significantly affected by material ducti-
ment of small samples can be particularly important if lity and work hardening rates, especially if ductilities
elastic properties are to be measured and it is advant- were ,5%.5
ageous to measure strain on two sides of a sample if For uniaxial microtensile tests for metals the bow tie
precautions to avoid bending strains have not been shaped testpiece (Fig. 5) is often used. LaVan and
taken. Errors of up to 100% in flow stress can result at Sharpe37 showed that it has considerable advantages
plastic strains close to yield, i.e. below 1%.37 with regard to gripping when the bow tie ends are
Small testpieces require low loads to break them and located into a cut-out in the grip, even for samples as
extra care must be taken in calibrating load cells and small as 360?260?2 mm in the gauge section. The
measuring the dimension of the testpiece in order to drawing in Fig. 5 has been simplified for ease of

minimised, especially if accurate mechanical properties

close to yield are required. Sometimes the testpieces are
also waisted, since for high strength materials (Ni base
alloys, some heat treated steels) the testpieces occasion-
ally fracture in cooler regions away from the central hot
zone. Waisting the samples concentrates the stress and
temperature within the central region of about 2–3 mm
(Fig. 5). The waist geometry is fairly gentle (a 60 mm
radius diamond wheel is used) and the associated stress
concentration factors (of a few per cent) are usually
5 Various options for miniature uniaxial testpieces show- ignored in the calculation of nominal stress versus strain
ing simple parallel sided rectangular shapes (typically curves.
406261 mm), waisted testpiece geometries (width at Recent studies using an ETMT system for deforma-
centre is generally targeted at 1?2 mm) and bowtie tion tests on Ti alloys have shown41 that if high
shaped samples to allow reliable location in grips37 temperature properties are being measured, temperature
uniformity is an important issue. Some miniature test
illustration since LaVan and Sharpe used a slight taper rigs use small furnaces, induction coils or direct dc
in the gauge length to encourage failure in the centre of heating to heat the samples. Often the testpiece is
the gauge length, but this was designed to introduce only gripped outside the hot zone, so there will be a tem-
a small stress concentration. Molak et al.64 used a perature gradient in the sample, which should be kept to
similar specimen geometry to generate stress–strain a minimum within the gauge length, and will depend on
curves and remanent life data on pressure vessel steels the temperature being used. In the absence of specific
using DIC to measure the strain in the 3?8 mm gauge guidelines for miniaturised testing, recommendations for
length. temperature uniformity and tolerance based on conven-
Weld microstructures, in particular, can vary quite tional high temperature testing should be used.74
sharply over submillimetre regions and it is therefore The deformation rate is also an important parameter
useful to be able to test samples that can reflect this to measure and control in tests at elevated temperatures
variation in structure.32,37,61,65 It is necessary to be able (high homologous temperatures) where measured defor-
to cut small samples from different regions within the mation stresses are sensitive to how fast the test is
weld and to do this without affecting the microstructure conducted. Generally microscale testpieces are too small
in such a way that it significantly affects the resulting to attach conventional extensometers with precise gauge
properties that are measured. The usual method for this lengths so mechanical properties are often evaluated by
procedure is to electrodischarge machine the basic shape plotting load or stress against displacement. The dis-
and then remove the ensuing surface cast layer by placement measured is a combination of displacement
diamond grinding and/or polishing. The cast layer can due to the testpiece extension and displacement due to
be as much as 50 mm in thickness and contain defects the compliance of the test rig itself. This can be assessed
and cracks that in particular reduce measured ducti- by inserting a very stiff testpiece (either high E or large
lities.37 It should always be removed by polishing or by cross-section), that does not extend significantly, and
careful diamond grinding. It is certainly not good testing hence the corrected load/displacement curve can be
practice to test samples under the as electrodischarge determined. Alternatively, in microscale tests it has been
machine condition. Ceyhan et al.61 conducted a shown that plastic strain ep can be calculated from
systematic study of small samples of P22 and P91 steels changes in electrical resistance70–73
where they compared machined and polished with ep ~0:5 ln (Rt =Rs ) (1)
electropolished surfaces for 260?569 mm (gauge
length) tensile specimens. A laser extensometer was used where Rs is the resistance of the central gauge length
to measure strains and tests were performed at room region (typically 2–3 mm) where temperatures are uni-
temperature and 550/600uC. They found quite notice- form at the start of the test and Rt is the resistance
able differences in the measured strength between the during the test. Resistance is measured by attaching (by
different surface conditions but with no consistent gentle spot welding) two thin (0?1 mm diameter) Pt–
patterns. However, they did find a huge difference 13%Rh wires (those used for thermocouple beads)
between the result of tests on macroscopic specimens separated by a distance of ,3 mm, with which a voltage
compared with the microtensiles (a factor of 3) which is drop is measured when a dc current is passed through
not consistent with other studies of small scale the sample. Resistance can be readily measured to about
samples,2,37,41,70–73 and particularly with a recent paper 1 part in 2000 for metallic samples typically 162 mm in
on miniature samples to measure the properties of Ti cross-section. This results in a plastic strain uncertainty
alloys41 where good agreement was obtained with of ,0?05%. These uncertainties compare well with
macroscopic tests. engineering measurements of strain. Typically resistance
At NPL miniature samples tested in an ETMT values of about 0?1–5 mV are measured at room
system65,70–73 are generally electrodischarge machined temperature, from high conductivity aluminium alloys
and then lightly diamond surface ground to a nominal to poorly conducting Ni based alloys. The technique is
size of 406261 mm. The surface grinding process can applicable to most engineering materials but care needs
introduce fairly deep, highly deformed regions, typically to be taken if strain is being measured over a range of
up to 50 mm thick in a stainless steel material; and temperature where a phase transformation takes place,
perhaps half of this in aluminium alloys. Consequently, since there is an associated step change in resistivity that
dependent on sample thickness, this must be removed or needs to be calibrated. Equation (1) was derived

(a) (b)
6 a type I stress–strain curve at 280uC (Al alloy) and b type II stress–strain curve from resistance plot showing ‘pseudo’
elasticity in test at 950uC (superalloy single crystal material)
assuming constant volume during deformation and room temperature. Miniature tensile testpieces were
negligible changes in resistivity from increased disloca- prepared by electrodischarge machining and light
tion densities, and neglects elastic strains. Tests analysed diamond grinding followed by annealing at 1100uC for
by this method fall into two types, dependent on the 30 min. The testpieces were waisted (Fig. 5) in order to
material under test: provide gentle strain gradients within a single sample
Type I: the assumptions are taken in full and the curve following deformation. The tensile test was performed at
of stress against plastic strain is more or less vertical a loading rate of 10 N s21, and conducted in two parts.
initially (Fig. 6a). Proof stress is then obtained by The testpiece was first deformed in tension to a plastic
drawing a vertical line at the required offset strain. strain of ,15% and then unloaded. It was then retested
Type II: it has been observed in some tests at elevated to give a total strain of ,35%. Before the test a 36100
temperatures, particularly on single crystal Ni based array of microhardness indents was made on the surface
alloys, that stress–strain plots obtained by this method of the testpiece using a scanning microhardness test
of analysis have a pseudo elastic region (Fig. 6b), machine (see later section), at a load of 1 N and spacing
possibly because the material’s intrinsic resistivity is of 0?2 mm. The spacing of the indents was measured
dependent on applied elastic strain. Further work is after the deformation test in order to calculate local
needed to explore this latter possibility. However, the strain and its variation along the tapered testpiece.
plot can still be used to define a proof stress by drawing Plastic strain in the central 2 mm region of the testpiece
a line parallel to the ‘pseudo’ elastic region at a suitable was also measured using the resistance method. The
offset plastic strain. tensile test results are shown in Fig. 8a plotted as stress
Because the use of resistance changes for measuring against strain. Plastic strain was calculated from the
strain is unconventional, a series of comparison tests resistance data. Elastic strain was calculated assuming a
were carried out on a BCR nimonic 75 tensile reference Young’s modulus value of 195 GPa and added to the
material75 for validation and comparison purposes. The plastic strain to give a total strain value. The results are
results of the ETMT miniature uniaxial tests at 600uC shown in two parts corresponding to the first and second
are shown in Fig. 7 compared with the results of three cycles of the test.
tests on conventional macroscopic testpieces that had
used extensometers to measure strain. The agreement is
good and confirms that plastic strain measurement
through changes in resistance is an acceptable method.
It is also interesting to note that the resistance method
accurately resolves a serrated yield process in the
nimonic 75. The steps in the flow stress–strain curve
are not noise in the signal but reflect real material
behaviour. Further work is needed to develop an
understanding of the pseudo-elastic region particularly
observed in tests in some Ni superalloys. For this
purpose research is under way at NPL to develop an
optical system to measure strain in the central 2 mm of
the hot zone using non-contact strain measurement tech-
niques based on the DIC process described previously.
To further confirm the validity of the approach of 7 Comparison of miniature uniaxial tests with macro-
obtaining the plastic strain from the resistance, a waisted scopic tests at 600uC on BCR nimonic 75 reference
sample of 304 stainless steel was deformed in tension at material

(b)
(a)
(c)
8 a tensile stress–strain curve from waisted 304 stainless steel testpiece (measured from the resistance changes) and
variation of plastic strain along testpiece measured from changes in indent spacing after b initial loading to 18% strain
and c further testing to 35% strain
The variation of strain along the testpiece as measured obtained from 406261 mm rectangular testpieces of
by the spacing (initially 100 mm) of the microhardness an austenitic stainless steel at 600uC tested in the NPL
indents is shown in Fig. 8b and c respectively for the first ETMT. One sample was annealed at 1200uC for 5 min
and second parts of the deformation cycle. The strain before testing, the other sample was tested under the as
values were calculated using sequential gauge lengths of supplied condition, probably diamond ground. The
200, 400, 800 and 400, 800 and 1200 mm respectively. It process of specimen machining will generally introduce
can be seen that locally there was considerable point-to- a layer of deformed material around the edges of the
point variation although this variation is smoothed out testpiece, with different microstructures and properties
for larger values of the gauge length. from the bulk material, and may introduce residual
The local variation is not simply an uncertainty stresses in the testpiece. The extent of the damaged layer
associated with the measurement of strain but reflects and magnitude of the residual stresses can significantly
the heterogeneous variability in local deformation in a affect the bulk material behaviour, particularly in small
fairly coarse grain sized material. The central (averaged testpieces, which have not been annealed. Although the
over 3000–4000 mm) strain values of 17?5 and 35% residual stress distribution will be balanced across the
agreed well with those shown in Fig. 8a that were whole testpiece (assuming equal treatment on opposing
measured using the resistance method (which were faces), local variations at the surface, combined with the
averaged over 3 mm). presence of the highly deformed material can dominate
Another example confirming the utility of resistance the behaviour and lead to significant changes in the
changes for the measurement of plastic strain was stress–strain behaviour. For this reason it is recom-
obtained in a tensile test conducted on 304 stainless mended that careful consideration be made to the
steel at 600uC where strain was measured using DIC
concurrently with the measurement of change in resis-
tance. Figure 4 shows an excellent agreement between
the two methods, confirming that DIC has good pro-
spects as a non-contact method at elevated temperatures
and that resistance changes can be taken to be an
accurate technique for assessing strains. In further sup-
port of using resistance changes for measuring strain it
should be noted that typical increases in resistivity due
to high dislocation densities are very small (0?1 nVm for
10% strain in nickel)76 compared with the resistivities
usually measured in elevated temperature tests
(500 nVm at 600uC for steels).
The influence of the damage and residual stresses
introduced to the surface layers during specimen pre-
paration are illustrated in Fig. 9 where there are clear
differences in the shape of the stress–strain curve and 9 Effect of heat treatment and surface condition on early
yield behaviour of material tested in the as received and stages of yield in test on austenitic stainless steel
annealed conditions. The stress–strain curves have been micro tensile testpiece

machining and preparation of micro testpieces, the

extent of damage introduced should be kept to ,5% of
the cross-sectional area and residual stresses should
generally be kept to a minimum. Annealing is not always
possible or desirable as this will negate the effect of heat
treatment and generate a different material behaviour.
Small punch tests

Standard procedures for mechanical tests usually require
fairly large volumes of material that must be taken from
in-service component. Often this is not practical or
desirable and has led to the development of small punch
(SP) test techniques based on the deformation of
miniature, disc shaped, test specimens.77–84 The SP test 10 Effects of oxidation time on percentage changes in
has been widely used for assessing the effects of nominal applied stresses
irradiation on nuclear materials1,2 and assessing rem-
nant creep life.3 The SP test is carried out by applying a should be measured before the start of the test
load, with a round ended punch or ball, to one surface of programme
a small disc-shaped testpiece supported over an aper- (ix) all tests in a series should ideally be carried out
ture, typically 4 mm in diameter, to investigate its on a single test jig. Where this is not possible care
response to the applied force, either at constant should be taken that the dimensions of the jigs
displacement rate or with a constant load (pseudo used are as close as possible. In order to produce
creep). The key requirements that need to be addressed comparable data the dimension should not differ
for more widespread uptake of the SP tests were by more than 1% between rigs
discussed by Hyde et al. in their recent review of (x) if possible a small number of uniaxial tests
mechanical and creep tests using miniature specimens3 should be performed on the same material in
with an emphasis on correlating mechanical data from order to validate any expression used to correlate
SP test procedures with microstructural changes, opti- SP tests with uniaxial data
misation of the test conditions for correlation of the (xi) the tolerance on thickness needs to be tightly
results with those from full size samples, development of specified (probably to better than ¡0?05 mm) to
suitable numerical models of the SP test, and investiga- avoid the necessity for normalising data.
tion of the protocols through interlaboratory exercises. The round robin exercise gave strong support to the
Key points for SP creep tests noted in recent CEN observation that SP creep testing can be regarded as a
TWA21 round robin activities included a code of robust method and therefore a good candidate for
practice published as CWA 15627, December 2006, standardisation and eventually for industrial application
which highlights the following: to residual life analysis of plant components.
(i) the use of simplified models proposed in the The SP test under constant load produces a displace-
literature for correlating the punch load to the ment/time trace that resembles that observed under
uniaxial stress in a conventional uniaxial creep uniaxial creep. Deformation is characterised by an
test led to a significant grouping of all the SP extended period of ‘primary’ creep, followed by a region
results of the four laboratories into a single trend of approximately constant displacement rate with a final
(ii) lab-to-lab differences were mostly due to having rapidly accelerating period leading to failure. A major
utilised two different punch diameters, and apart benefit of the SP test is that it enables mechanical
from this fully rationalised difference, the results characterisation of the materials of in-service compo-
were quite coherent among the partners. nents in a minimally invasive, virtually non-destructive
manner; i.e. using only a small volume of material
The following recommendations should be adopted in
removed from the component and testing without
conjunction with those given in the CEN TWA21
necessarily a requirement for repair.
documents81,82 and the recent SP fatigue paper by
For some materials the test environment is clearly
Lacalle et al.:83
important, and SP tests are carried out, for the most
(i) load and temperature control should follow
part, in an inert argon environment, to minimise
similar guidelines to existing creep standards
oxidation effects that can change the cross-section of
(ii) preference for a punch rather than a ball for
the sample significantly and thus increase stress and
applying load
reduce ductility.
(iii) preferred testpiece to be 8 mm diameter and A series of tests were carried out at NPL to examine
0?5 mm thick h the oxidation process quantitatively and calculate metal
(iv) recommended rig geometries included loss kinetics relevant to the SP test. Data were obtained
(v) punch radius r where 1,r,1?25 mm from simple uniaxial tensile specimens held under
(vi) aperture radius, R52?00 mm with chamfer constant load at different temperatures for two power
(vii) if no prior knowledge, load is calculated from generation alloy steels (P11–CrMo and P12–CrMoV)
: : over the temperature range 560–650uC through mea-
F ~3:33sR{0 2 r1 2 h (2)
surements of resistance change that occur as metal is lost
(viii) for both forms of SP tests, the geometry of the to oxide. The metal loss kinetics can be converted to a
test jigs (i.e. ball diameter and hole diameter) graph (Fig. 10) of nominal percentage stress changes

plotted against time for a typical SP disc of original

thickness 0?5 mm. If it is assumed that only a 5% change
in stress can be tolerated then it can be seen that, even at
temperatures as low as 560uC, the loss in cross-sectional
area becomes excessive at times as short as 20 and 40 h,
for P12 and P11 respectively. Consequently, it is
recommended that, to avoid problems with data
interpretation, SP tests should always be conducted in
an inert environment (high purity argon should be
suitable).84
The SP test is considered to be a non-destructive
technique because of the small amount of material
required. Discs are usually machined to a final thickness
of ,0?5 mm, with a tolerance of no more than ¡0?5%,
with disc diameters generally 8 mm¡1%. Heating
systems are designed to provide a uniform temperature 11 Comparison of uniaxial creep data with SP disc test
distribution throughout the test section of the disc. A results for P12 steel sample
temperature measuring system usually comprises ther-
mocouples, located to determine that the testpiece
remains within the temperature limits specified for the to failure tF, and this Monkman–Grant type relation
test. The temperature control system is generally capable was the same irrespective of the load and the amount of
of maintaining the temperature constant to within pre-existing damage that the discs contained. The
¡0?25% of the target temperature throughout the test. relation varied slightly with disc thickness and punch
Typical differences in system set-up can be demon- head radius. Ball diameter and hole diameter were
strated by test rigs at NPL and at the IRC in high established as key aspects of jig geometry, as well as
temperature materials at the University of Wales, other test parameters such as load, material condition
Swansea.78–80 In the NPL system the load is applied and specimen thickness.
with a Si3N4 ceramic ball of radius 1?2 mm and the disc Over the load range 175–425 N the load dependence
is clamped circumferentially, with a thermocouple in the of time to fracture predicted by the model could be well
recess of the face of the clamp. In the IRC Swansea described by a power law equation. Plots of minimum
system the load is applied with a hemispherical ended displacement rate against failure time for the small disc
solid nimonic rod of radius 1?0 mm and the temperature test frequently show the same type of dependency as
measured with a remote thermocouple that had pre- observed in uniaxial creep tests, but with a shift along
viously been calibrated with an instrumented testpiece. the time-to-failure axis. Figure 11 shows experimental
Temperature measurement and distribution is important data obtained on minimum displacement rates (for the
because of the difficulty in putting individual thermo- small disc test) and minimum creep rates (from pre-
couples on each testpiece, and in developing good testing existing uniaxial tests held at the IRC Swansea). The
practice it is important to assess the magnitude of the results did not sit on parallel lines as some other studies
uncertainty in temperature and what difference this have suggested. It is debatable as to whether this
makes to the mechanical data. Guidelines for current similarity to a Monkman–Grant type relation is an
creep testing standards should apply equally to SP tests. intrinsic property of the small disc test or is due to the
For example, ¡3uC on 600uC would be expected to expected scatter in both the uniaxial and more especially
result in an uncertainty of about ¡25% in minimum small disc test results. An important objective was to
creep rate. develop a better understanding of this shift, its
The SP test is extremely dependent on jig geometry dependence on test conditions and when it is parallel
and the influence of key parameters has been investi- in nature. The stochastic model was therefore run 15
gated using numerical models by Evans and Evans.78 An times with variable test conditions. The resulting slope
elastic–viscoplastic FE model of the disc creep test was estimates of the Monkman–Grant type relation showed
developed that produces as an output the displacement that the differences in slope in Fig. 11 were within the
time curve up to the point of fracture. The model uses a 95% confidence interval and thus an assumption of the
realistic creep deformation law which includes strain parallel nature of the plot is not unreasonable. This
hardening, thermal softening and damage accumulation provides support to the CEN TWA recommendations
for a P12 steel. In the model the displacement/time curve for using simplified analytical models for calculating
is made a function of the following variables which form equivalent uniaxial stresses, however there is clearly
the inputs into the model: the hole diameter, the disc scope for more detailed continued studies using FE
diameter, the disc thickness, the punch head radius, the methods and analytical engineering models that can
coefficient of friction, the pre-existing damage present in accommodate the complex stress fields in the test.
the disc and the punch load. Two versions of the model Figure 12 shows experimental data supporting the
were developed. The first was a deterministic model that importance of the hole diameter on the time/displace-
did not take into account the variability observed in the ment behaviour of a service exposed P12 steel material
multiaxial creep test data for P12 steel. The second tested at 600uC and 320 N. The ball radius was identical
version built this variability into the small disc test so for each test at 1?2 mm. An increase in aperture
that confidence intervals for the model predictions were diameter of only y7% reduced the lifetime of the
also obtainable. At 575uC a relationship was found to material by more than an order of magnitude. Small
exist between the minimum displacement rate and time punch tests at NPL have showed that lifetimes at given

12 Influence of aperture (hole) diameter on SP creep test

results on P12 steel (service exposed) at 600uC and
320 N applied load
stress levels were particularly sensitive to hole sizes

within the range 3?8–4?1 mm. The diameter of the
receiving aperture can be produced by drilling with a
tolerance of ¡0?05 mm. This diameter is probably the 13 So called ‘theta’ testpiece for indirect tensile testing
most critical dimension in the test set-up and must be of brittle materials
measured before testing.
Tests also show that increasing the diameter of the specimen. The design of this testpiece was originally
indenting ball systematically increased the maximum devised in the 1950s as a way of overcoming gripping
load obtained while increasing the diameter of the problems in macroscopic testpieces, but is little used
receiving aperture had little effect on the maximum load now because of the expense of machining the complex
but seemed to increase the maximum displacement for shape, a disc with a diametral bar which is loaded in
failure. The magnitude of these effects was also orthogonal compression (Fig. 13). Machining costs are
dependent on the applied displacement rate. much reduced in miniaturised testpieces using deep
Effects of surface finish might be considered to be reactive ion milling or similar processes such as focused
important but it can be argued that, if damage is ion beam. Quinn et al.85,86 have reported tests on
continuum based, failure times would not be expected to 100 mm thick silicon wafer material in which a row of
be surface sensitive. Observations of crack initiation such testpieces 300 mm in diameter are machined. Test-
sites and propagation directions would be helpful in ing of each testpiece was achieved by sandwiching the
validating model predictions, but this might be difficult row of testpieces between supporting microscope slides,
due to the problems of choosing the correct times at and using a nanoindenter with a blunt diamond tip to
which to interrupt the test. Stress multiaxiality is also
load each testpiece in turn. Fractographic examination
recognised as a possible issue, SP tests are initially
revealed that the strengths of 450–600 MPa achieved
biaxial, and then possibly multiaxial, as strain develops;
were limited by the formation of etch pits typically 1 mm
whereas the results with which the SP data is compared
in size produced by the milling process.
are often obtained from uniaxial tests.
Beam flexural testing
Miniaturised strength tests for ceramics Traditional ceramics have been tested in large bar type
It is instructive at this point to review the development testpiece form in order to capture realistic microstruc-
of miniaturised strength tests for ceramic materials since ture through the thickness. However, the fine grain size
there have been considerable developments in this field in the majority of advanced technical ceramic materials,
in recent years. The principal driver is that many coupled with their cost and difficulties of machining,
modern applications for advanced ceramics are in small have led to the development of testing techniques, now
or very small components, particularly for the electro- standardised, based on small bar specimens, typically
nics applications where mechanical reliability is an issue. 364645 mm (Table 3). Such testpieces are already
It should be noted that strain is seldom directly small compared with most metallic and composite
measured in the test, other than occasionally indirectly materials testing. The background to the testing
through displacement in, for example, bend tests; the methodology and the potential sources of error are well
assumption being that the materials are behaving in a researched and fully documented.87,88 Typically, in a
purely elastic manner. A further issue is the wide spread correctly functioning loading jig, an accuracy of ,2% in
in strength behaviour, governed by the size of small fracture stress can be expected, computed from fracture
defects, requiring a larger number of tests and statistical force and testpiece dimensions using simple beam
assessment of test data. bending equations; which is adequate for most purposes,
such as material discrimination. Such testpiece dimen-
Tensile testing sions are now in common use for strength, elastic
Tensile testing of brittle materials is inherently difficult, modulus, fracture toughness and fatigue testing.
due to the problems of ensuring alignment. Downscaling With a broadening of applications, and especially with
testpiece sizes exacerbates the problem, because of the miniaturisation of components in the electrical and
dimensional precision needed. However, recent work has electronic fields, the need for evaluation of testpieces and
reported some success in using the so called ‘theta’ components which are smaller still has developed

strongly in recent years, and this has stimulated research to a shift in the neutral axis. This can lead to an
to evaluate suitable tests. indeterminate stress distribution unless substantial
For flexural strength testing, Lube et al.89 have quantities of test data are deconvoluted to derive the
examined the potential errors involved in reducing the stress/strain rate relationships (e.g. Chuang’s analysis).95
size of conventional testpieces, and conclude that they
rise rapidly once the testpiece loading span is less than
Biaxial flexural testing
,20 mm. Such errors accumulate from issues such as It has long been argued that biaxial testing, using, for
parallelism of surfaces, measurement errors, and align- example, a concentric ring-on-ring geometry, is highly
ment, twist and frictional errors in the loading system. advantageous for ceramic materials because it avoids the
With weaker materials there is also an increased risk of issue of edge chamfers; edges being remote from the
high local stresses under loading contacts causing highly stressed region and thus unlikely to be fracture
damage. origins.96 The biaxiality of the stress field within the
Standardised testing also requires that the long edges inner loading ring is also more probing of surface
of testpieces are chamfered. This process removes edge defects, and the average strength data are generally
damage that can arise during testpiece preparation. lower, and are considered to be more realistic than
Provided that the chamfers are small in relation to the uniaxial data. Compared with the beam flexure test,
there are other limitations for accuracy, including
testpiece cross-sectional dimensions, their effect on the
greater problems in controlling frictional effects, and a
flexural moment of inertia can be ignored. However, as
need for flat test surfaces. This geometry has been
the testpiece becomes smaller, scaling the chamfers
employed in ISO 6474 for alumina ceramics for
equivalently means that they might lose their effective-
orthopaedic devices for some years (Table 3). In this
ness, while maintaining their size means that moment of
case, it has been found to be necessary to use rubber and
inertia corrections become applicable.90,91 Such correc-
paper interlayers between testpiece and loading ring in
tions require measurement of the chamfers.
order to reduce frictional effects and take up some out-
In experiments to directly injection mould miniature of-flatness. More flexible dimensions are allowable in
(160?260?2 mm) testpieces directly in zirconia, achiev- ASTM C1499, which also permits the use of square
ing good shape precision has proved difficult.92 They are testpieces, such as electronic substrates.
too small to be remachined, and so this is probably the Attempts have been made to apply this geometry to
principal factor leading to the illustrated corner failures very thin test material, such as fuel cell laminae, but
in three-point bend testing and to a high scatter in immediately there is a problem that once the central
results. More recent work by the same group93 has deflection at fracture is more than half the thickness,
shown that the moulding technique is critical in produc- non-linearity of the force/deflection response develops,
ing rounded edges on the mouldings, with evidence that with the occurrence of so called membrane stresses in
deliberately allowing edge rounding improves strength addition to bending stresses. Kao et al.97 provided some
and reduces scatter in testing. analysis of this situation, which can be reduced to the
As noted above, strain is seldom measured directly. results in Fig. 14.96 This approach has been satisfacto-
The principal area where it has been employed at NPL is rily employed by Kübler et al.,98 for example.
in the flexural testing of long-fibre ceramic composites, Various other biaxial testing methods have been
with successful use of surface strain gauges up to strain attempted, but the one that shows most promise for
levels of typically 1–2%. scaling downward in size is the ball on three balls (B3B)
High temperature flexural strength testing using test. This geometry, which is a simplification of the
refractory test jigs has also been standardised punch on three balls method originally developed by
(Table 3). For the purposes of materials comparison, Wachtman et al.99 using a stress distribution computed
flexural creep testing has also been widely used. Strain is analytically by Kirstein and Wooley100 and applied to
typically measured from mechanically determined cur- thin ceramic substrates for electronics, has been
vature measurement, but unless the materials behave extensively researched by Börger et al.101,102 The peak
viscously i.e. the stress exponent of strain rate is unity, biaxial tensile stress is over a small area on the opposite
the maximum nominal stress is overestimated to an face to the central loading ball. Figure 15 shows the
extent dependent on that stress exponent.94 An added practical implementation of the test, which can be scaled
complication is that creep rates may be different on the appropriately to the size of the testpiece. Its advantage is
tensile side compared with the compression side, leading that non-flat, non-parallel surfaces can be used, and the
Table 3 Standardised tests for advanced technical ceramics
Testpiece type Standard Testpiece dimensions{, mm
Three or four-point flexure, bars ISO 14704 (room temperature) 3646.45 (40 span)
ISO 17565 (high temperature) 3646.35 (30 span)
EN 843-1 (room temperature) A: 262.56.25 (20 span)
EN 821-1 (high temperature) B: 3646.45 (40 span)
ASTM C1161 (room temperature) A: 1.5626.25 (20 span)
ASTM C1211 (high temperature) B: 3646.45 (span)
Ring on ring flexure of discs ISO 6474 (room temperature){ Outer ring dia.: 30; inner ring dia.:
12; testpiece, 36 (dia.)62 (thickness)
ASTM C1499 (room temperature) Flexible
{Different test spans reflect different historical developments, notably in the US and Japan, and have not yet been rationalised.
{This test is also employed in similar specifications for ceramics for orthopaedic applications other than high purity alumina.

14 Large deflection solutions for thin disc (non-

dimensional) stresses at disc centre and under load-
ing ring as function of non-dimensional force for case 16 Calibration of factor f in B3B test reveals that it is
of support to loading ring radius ratio of 2:97,99 most sensitive to ratio of thickness to disc radius,
straight line is small deflection solution mildly sensitive to ratio of ball support to disc radius,
and relatively insensitive to Poisson’s ratio
test can readily be scaled down to testpiece sizes of

typically 2 mm diameter (or square) and 100 mm thick. Fracture origins and strength statistics
Its disadvantage is that the tensile stress calibration It is probably true to say that once the accumulated
requires FE analysis. However, this has shown that for a errors in testing rise towards the scatter of strength data
restricted range of thickness to diameter ratios and of typically obtained in brittle strength testing, the relia-
values of Poisson’s ratio, simplified geometrical para- bility of intermaterial or interbatch comparative testing
meters can be used in the calculation of fracture stress may become meaningless. There are also issues as to
smax through the relationship exactly what is being measured. A change in dominance
of various fracture initiating ‘flaws’ can arise, since the
F
smax ~f(R,Ra ,t,n) (3) preparation of small testpieces eliminates the possibility
t2 of the existence of larger defects. Small testpieces with
where F is the fracture force, t is the testpiece thickness, big defects would probably not make it to the test!
and f is a dimensionless function of R, the testpiece One of the key issues in ceramic strength testing is the
diameter Ra is the support ball ring radius, and n is surface of testpieces. If testpieces are under an as fired
Poisson’s ratio. An evaluation of the parameter f is condition, the surface may be stress-free, but the geo-
shown in Fig. 16, where it can be seen that the dominant metry may not be well controlled owing to the inevitable
factor is the ratio of disc thickness to radius. The ratio of shrinkage and possible distortion in firing the original
disc to support ball ring radius has a significant factor, powder compact. In order to improve the geometry for
while Poisson’s ratio has a minor role. testing by machining, damage is introduced into the
This test has been applied to both monolithic and surface in the form of plastic deformation, microcracks
layer structure ceramics, including low temperature fired and residual stress. This damage may be directional,
electronic substrates with metallic interconnects, in the depending on the method employed. In test material in
latter case with the ability to position the region of which there is a distribution of significant internal
maximum stress at a particular feature of interest. defects, such as pores, agglomerates, cracks, etc.
(a) (b) (c)

a positioning guide in place to ensure centralisation before applying preload; b lowering of guide to leave balls and
testpiece free standing; c geometry of tensile stress distribution under loading ball
15 Ball on three balls test schematic

(a) (b) (c)

17 Weibull size scaling plots for a alumina with as fired finish, based on effective stressed surface area, and b,c for sili-
con nitride with ground finish, based on effective stressed volume and area respectively: batch E was polished; solid
lines are extrapolations from four-point bend tests, with confidence intervals (dashed lines)
strength may be determined by these ‘volume flaws’, and ð m

thus will not be particularly influenced by how the s
Veff ~ dV (4)
surface has been prepared. However, in high quality sref
materials which have no significant ‘volume defects’, where sref is the reference stress in the testpiece, usually
flaws at the surface, especially those introduced by the maximum nominal stress, and m is the Weibull
machining, control the strength properties. On a modulus, a measure of the scatter of strengths.
practical note, it becomes increasingly difficult to ensure Lube et al.89 made a comparison between standard
that true geometry (such as squareness, parallelism of 40 mm span testpieces and scaled 13 mm span testpieces
faces, etc.) is maintained by conventional machining in four-point flexure. A size scaling consistency was
processes as the size scale is reduced, owing to limita- achieved for a silicon nitride in terms of the Weibull
tions in handling and gripping. There are also increased scaling theory, but for an alumina this did not hold. It
risks of curvature induced by residual stresses, which can was reasoned that the nature of the defect distribution
only be reduced by ensuring that opposing faces receive was different for the two materials. The nature of defects
exactly the same treatment. in the weaker alumina meant that reducing the size of
Inevitably, therefore, in testing very small testpieces, a the testpiece did not change the defect distribution
balance has to be struck between the possible high error controlling the strength in the same way as in the silicon
level resulting from poor geometry, and modifying the nitride; effectively, larger critical flaws were not being
flaw population as a result of correcting the geometry to eliminated by testing a smaller effective volume or
reduce testing errors. effective surface area. It is suspected that this is because
An approach to understanding size scaling effects in critically sized flaws grow subcritically from much
brittle materials is to use the well known Weibull theory. smaller inherent microstructural defects that continue
An evaluation of this theory down to very small sizes has to be present.
been undertaken by Danzer.103 It is argued that as the However, in another more recent size scaling study, a
effective stressed volume decreases, the high density of series of B3B testpieces of different diameters fabricated
very small potentially destructive flaws means that they from a high purity alumina with an as fired surface and
must interact, and the weakest link hypothesis behind from a silicon nitride with a machined surface were
the Weibull statistical approach becomes inconsistent (A compared with the usual flexural strength tests.104,105
material showing Weibull strength behaviour has a flaw Fractographic investigation showed that the alumina
density distribution which is an inverse power law. As failed from surface flaws, while the silicon nitride failed
the size reduces, the flaw density goes to infinity, which from bulk flaws, mostly agglomerates. Figure 17 shows
is physically unrealistic.) For a typical high strength that for the alumina, the scaling theory based on stressed
ceramic, such as silicon nitride, it is predicted that this surface area is appropriate, but for the silicon nitride
will occur when the effective volume under stress is less there is a marked deviation of the B3B test results from
than typically 1024 mm3 (equivalent to a cube of side the prediction based bar flexural tests. In addition to the
,45 mm). Such volumes are approached, for example, in difference between uniaxial and biaxial stressing, with a
the miniaturised B3B test when the testpiece size is less decrease in the volume or area there is probably a
than a few mm. The ‘effective volume’ Veff is a des- change in flaw population more towards surface related
cription of the volume of the testpiece under stress s machining flaws. When testpiece surfaces were polished
which probabilistically can contribute to failure, and is to remove such flaws (batch E), the strength of small
given by discs markedly increased.

Studies such as these show that prediction of

microscale strength properties from macroscale test data
is risky, and that it is better to undertake testing on the
scale and with the surface condition intended for the
component application than to extrapolate theoretically.
Microindentation tests
The most common applications of microindentation
tests have been to map local heterogeneities, such as
those common in welds and damaged or heat treated
surfaces,106 or in tests to assess the high temperature
deformation characteristics of local variations in micro-
structure through indentation creep studies.107–115 The
indentation, or as it is sometimes known, impression 18 Stepped stress indentation creep tests at 600uC on
creep method has substantial advantages because it is CrMoV steel (courtesy Dr S. Brett, RWE npower)
relatively easy to apply and correlates reasonably well
with uniaxial data. Two kinds of indenter have generally constraint on measurement of low strain rates in tests
been selected for these tests, either circular or rectan- lasting several weeks. Typically displacement measure-
gular, and the use of both has been carefully supported ment resolutions of ,1 mm are required. However, the
by FE studies to assess the impact of geometrical impression creep test method is limited by its inability to
factors, such as indenter and specimen sizes, associated study the final (tertiary) stages of creep deformation that
with test metrology. Indenters typically have widths (or lead to fracture in tensile creep studies. There is some
diameters) of ,1 mm and are well suited for in situ evidence that minimum creep rates obtained by this
measurements of different zones in the weld. The method can be correlated with failure times in uniaxial
constraint factors associated with the indenter/punch tests by a Monkman–Grant expression but this observa-
are typically about 3 and have to be ascertained for each tion requires further experimental investigation before it
method of interest before direct comparison can be can be wholeheartedly recommended. The method does,
made with uniaxial data. The use of the reference stress however, lend itself to step or ramp experiments whereby
approach to correlate indenter displacement rates and data under several conditions can be generated from a
nominal applied stresses with their uniaxial equivalents single testpiece (Fig. 18). This is quite important because
has been summarised recently108 with a recommendation it accelerates the process of data acquisition and this is
for ‘standardising’ the test procedure using square vital since single condition tests can tie up expensive
specimens, typically 1061062?5 mm in dimension experimental kit for long periods. This use of stepped
indented with a 1 mm wide rectangular punch covering tests, whether step-up or step-down, make some assump-
the full width of the testpiece. Smaller proportional tions that the measured secondary creep rates are
specimens could be used but at some stage care has to be dependent only on levels of accumulated strain and are
taken that the indenter covers a representative element not strain history dependent. There is evidence both for
of the underlying microstructure. Indenters have to be and against this assumption116–118 and further research
strong compared with the indented material and would be very welcome. The use of miniature uniaxial
typically ceramic or superalloy compositions would be tensile testpieces is an alternative approach, since the
chosen. The deformations also need to be small stress states are relevant to the tertiary deformation stage
compared with indenter dimensions, which puts some in macroscopic testpieces that lead to fracture. Figure 19
(a) (b)
19 Comparative creep data on P11 steel (both as received, P11ar, and thermally exposed, P11exp), from miniature ETMT
testpiece with a strain/time data and b minimum creep rate/time to failure

features. A scanning microhardness indentation test

machine (SIMM) has been developed at NPL to speed
up the process of investigation,65,129 by measuring depth
sensing hardness through instrumented load and dis-
placement. Conventional automated systems generally
rely on measurements of indentation diameter after the
map has been constructed. The SIMM measures a
universal hardness, i.e. based on the measurement of
load/displacement data, and can be related to a Vickers
microhardness after suitable calibration, using the
principles outlined in the standard for instrumented
hardness tests, ISO 14577. The principle of depth
sensing hardness allows the measurement process to be
fully automated. A raster of indents can be placed by
computer control to map the variation in hardness.
20 Larson–Miller plots comparing ETMT data from uniax-
Local mechanical property information can be rapidly
ial miniature tests on P12 steel thermally exposed at
obtained from a measurement of nominal microindenta-
200 or 250uC with macroscopic data at lower stresses
tion hardness. Typically an array of 1006100 indents
provided by E.ON
takes ,10 h, i.e. ,4 s/indent. The machine currently
operates in the micro to mesoscale range, 0?02–20 N)
shows typical creep data from a P11 steel from the NPL with a load resolution of 2 mN and a depth sensing
ETMT system, but even here there are issues associated resolution of 20 nm, using a specially designed capaci-
with the development of damage (cracks or internal tance displacement sensor. Hardness maps can be
porosity) in testpieces of small cross-section. ETMT obtained using the high speed indenter up to 60 times
results are compared with Larson Miller data from faster than nanoscale machines working at the micro-
macroscopic tests provided by E.ON on a P12 steel119 in scale. This allows mapping of a significant surface area
Fig. 20. This would be fruitful area for further research, and may be used both in a quality control context as
particularly linking the studies to thermomechanical well as for research and development. Some examples of
fatigue failures120 as well as creep, and incorporating the utility of the test system are shown in Fig. 21 which
complementary damage mechanics and FE studies. shows maps of a weld produced in a superduplex
Many material components, especially when heat stainless steel and a spot welded aluminium alloy sheet
treated or welded, have heterogeneous structures and material. Both maps were obtained in a fully automated
the underlying variation in properties is crucial to nature with more than 10 000 indents placed in a regular
improving performance. Understanding the spatial array. Typical indent sizes were 10–20 mm and were
variation of local mechanical properties in materials spaced at between 50 and 100 mm intervals.
with graded compositions, complex coatings or inho- Conventional microhardness values are calculated
mogeneous structures can lead to a more cost effective using the standard Vickers formula
application of these technologies. Often these graded
structures are assessed with microindentation tests, HV ~ð2P sin hÞ=d 2 ~ð1:8544PÞ=d 2 ~P= 26:42h2 (5)
usually as a line scan with 10–20 indents being typical,121
although new automated instruments are increasingly where P is the indent load in kgf, d is the corner to
being applied to characterise weld structures in parti- corner diameter of the indentation in mm and h is the
cular.122 The low number of indents is a consequence of angle between the indenter face and the vertical (136u/
2568u). The depth of the indentation h is equal to
the effort required to make measurements of the size of
the indentation. In a recent review of depth sensing d= 2|21=2 tan h &d=7. Vickers microhardness is
nanoindentation tests4 attention was drawn to the defined as the ratio of applied load to contact area
overall concept of hardness since results depend on between indenter and sample under load. The depth
many factors, including indenter geometry, rate of sensing hardness H(SIMM) is defined by Pmax/A (i.e.
indentation, material microstructure and specific details 2P/d2), where A is the projected area of contact, and this
of the deformation response. These comments are is calculated from
equally applicable to indentations on the microscale
H(SIMM)~F =(24:5h2c ) (6)
(typically 1–100 mm in indent diameter) where indents
can be within individual phases or grains, across where hc is the indentation contact depth under load.
boundaries, and often sample unseen subsurface fea- The hardness at each point is determined using the
tures. The trend towards the calculation of uniaxial following method on the load/displacement curves.
constitutive mechanical response (either stress–strain or First, the surface is found by fitting a polynomial to
creep) from depth sensing data was noted.4,123–128 the initial 5% of the loading curve, followed by
However, Luo et al.124,125 have highlighted the difficul- measurement of the depth at maximum load. A linear
ties of calculating the coefficients in these expressions fit to the top 20% of the unloading curve is then
from indents of a single geometry and noted that the use extrapolated down to zero load, to give the unloading
of more than one indenter geometry may be necessary to zero. The indentation contact depth under load hc can
obtain a unique solution to the fitting of a suitable con- then be determined. Thus, for relatively high loads
stitutive expression for uniaxial deformation behaviour. (generally above ,2 N for metallic materials), where
At the microscale an important factor is the spread in small discrepancies in the diamond indenter geometry
data from indents that sample different microstructural are not a problem, from equations (5) and (6) the

21 Examples of microindentation hardness maps in welded superduplex steel plate (left) and spot welded aluminium
alloy sheet (right)
hardness obtained by SIMM is related to the conven- point to point variation, as microindentation indents are
tional microhardness by often within individual grains and therefore highlight
orientation differences in deformation response.
HðSIMMÞ~0:93 HV (7) Depth sensing microhardness measurements on a 316
For loads less than ,1 N, small imperfections in the stainless steel were compared with values obtained in a
indenter tip geometry can give rise to significant conventional microhardness machine. The calibration
discrepancies with regard to hc, usually manifested as procedure involved measurement of SIMM indents in
an indentation size effect with increased values of the centre of the samples (away from the influence of
nominal hardness compared with that which would be residual stress and surface deformation effects) by
expected from a perfect geometry. These discrepancies optical microscopy, for direct comparison with the
generally have to be calibrated by experiment. In these depth sensing values. A standard Leitz Miniload micro-
circumstances the nominal SIMM hardness values are hardness machine was used to place five indents in the
significantly higher than the conventional microhardness centre of an annealed sample at a range of loads (0?5,
HV value. 0?2, 0?1, 0?05, 0?025 and 0?01 kgf; equivalent to 4?9,
Gradients in microhardness can be used to map 1?96, 0?98, 0?49, 0?25 and 0?1 N). The diameter of the
differences in internal deformation.129 Microhardness indents was measured using an optical image analysis
mapping measurements show that the technique pro- system at a magnification of 6500 to improve resolution
vides good repeatability in plots of mean values of of the smallest indents, which were ,20 mm in size. The
linescans through work hardened surface layers SIMM indents were also measured using the same
(Fig. 22), but it must be noted that there is considerable optical system and used to calculate HV (optical) values
22 Microhardness indent arrays (,20 mm spacings) through two ground surfaces of stainless steel sample mounted back
to back; and associated microhardness map of one of arrays

23 Load dependence of microhardness (left) and indent diameters (right) for conventional and SIMM measurements in
316 stainless steel
for comparison with the depth sensing values and the in the 316 stainless steel alloy of grain size ,30 mm all
conventional HV microhardness values. The individual indents below ,1?0 N will be within individual grains
values of conventional microhardness are plotted against and should therefore be interpreted appropriately depen-
load in Fig. 23 to illustrate the level of scatter. It is likely dent on the position and number of indents.
that this scatter reflects local differences in plasticity It is worth noting that depth sensing hardness values
arising from grain to grain orientation differences since are often quoted as Martens Hardness in units of
the grain size of the material is ,20 mm and thus greater N mm–2 and thus a factor of 9?81 greater than the
than or equal to most of the indent sizes. SIMM depth sensing values discussed here, where
The SIMM was then used to place 363 indent arrays correspondence with conventional Vickers microhard-
with indents separated by 100 mm at loads of 2, 1, 0?5, 0?2, ness numbers was sought.
0?1, 0?05 and 0?02 N. The SIMM microhardness values
(Fig. 23) show a much stronger dependence on load than Generic issues and future needs
the conventional microhardness values. The results for While it is clear that the challenge of miniature test
both SIMM and conventional microhardness tests are method development has been addressed by a number of
also plotted as indent diameters against load in Fig. 23. A different approaches (SP tests, bend tests, microuniaxial
linear fit through the log–log plot for the conventional tests, microindentation tests) there are some common
microhardness values gives a slope very close to 0?5, as features that are worth noting and areas where future
would be expected from HV51?844P/d2. However, the research activities would be welcomed. The following
load dependence of the indent diameter calculated from points can be summarised from the present paper.
the depth sensing microhardness values has an exponent 1. Digital image correlation is a powerful non-contact
of 0?635. This is thought to be due to a rounding of the tip method for quantifying strain distributions and local
or a chip from the bottom of the SIMM Vickers indenter, heterogeneities associated with different phases, grain
of magnitude 0?5 mm. Thus microhardness maps orientations and textures in the testpiece and further
obtained below ,1 N on typical engineering materials intensive research is expected.
should be used in a comparative sense, in that each 2. Measurement uncertainties clearly increase as test-
indenter has to be individually calibrated with respect to piece size decreases; consequently, it is good practice to
the material of interest and the specific load applied to
generate fully calibrated maps.
The depth sensing hardness data show a greater
sensitivity to the applied load than conventional mea-
surements and this may be an advantage in profiling
plasticity gradients. A typical microhardness profile
through a diamond ground surface is shown in Fig. 22
where it can be seen that the deformed surface layer was
about 100–200 mm thick as discussed in the section on
uniaxial microtensile test characterisation. Furthermore,
statistical measurements of load dependence of indent
diameter can provide useful guidelines on the size of area
probed by specific SIMM indents. A series of reference
plots of indent diameter for average microhardness values
for a range of engineering materials is shown in Fig. 24,
and this can be used for assessing the statistical relevance 24 Representative reference plots of SIMM indent diameters
of particular indents at selected load values. For example, as function of load in various engineering materials

pay specific attention to statistical measures of uncer- 5. I. Brooks, P. Lin, G. Palumbo, G. D. Hibbard and U. Erb:
‘Analysis of hardness-tensile strength relationships for electro-
tainty, choice in the number of specimens examined, and
formed nanocrystalline materials’, Mater. Sci. Eng. A, 2008, A491,
evaluation of how uncertainties in input data, from experi- 412–419.
ment or analysis, propagate through model predictions. 6. E. Demir, D. Raabe, N. Zaafarani and S. Zaefferer: ‘Investigation
3. The testpiece dimensions used should contain repre- of the indentation size effect through the measurement of the
sentative microstructures of the material being examined. geometrically necessary dislocations beneath small indents of
different depths using EBSD tomography’, Acta Mater., 2009, 57,
4. Specimen preparation techniques should be con- 559–569.
sidered carefully and aimed at minimising damage and 7. M. Rester, C. Motz and R. Pippan: ‘Indentation across size scales
residual stresses in surface layers. Quantification of this – A survey of indentation-induced plastic zones in copper {111}
damage due to different preparation methods would be single crystals’, Scr. Mater., 2008, 59, 742–745.
very useful. 8. M. D. Nix and H. Gao: ‘Indentation size effects in crystalline
materials: A law for strain gradient plasticity’, J. Mech. Phys.
5. The utility of finite element studies to assess the Solids, 1998, 46, (3), 411–425.
importance of geometrical features so that tests can be 9. M. Zhao, W. S. Slaughter, M. Li and S. X. Mao: ‘Material-length-
optimised for the determination of key parameters. scale-controlled nanoindentation size effects due to strain-
Typical examples were outlined in the small punch test gradient plasticity’, Acta Mater., 2003, 51, 4461–4469.
and microindentation sections. Additional research on 10. J. B. Pethica, R. Hutchings and W. C. Oliver: ‘Hardness
measurement at penetration depths as small as 20 nm’, Philos.
other test geometries is needed. Mag. A, 1983, 48A, (4), 593–606.
6. Validation with full scale tests should be used 11. F. Diologent, R. Goodall and A. Mortensen: ‘Surface oxide in
where possible to quantify potential size effects. replicated microcellular aluminium and its influence on the
7. The use of reference materials for validation, plasticity size effect’, Acta Mater., 2009, 57, 286–294.
particularly of finite element model predictions, is 12. A. Iost and R. Bigot: ‘Indentation size effect: Reality or artefact?’
J. Mater. Sci., 1996, 31, 3573–3577.
encouraged. 13. T. Chudoba, P. Schwaller, R. Rabe, J.-M. Breguet and J. Michler:
8. For oxidation sensitive materials it is essential to ‘Comparison of nanoindentation results obtained with Berkovich and
conduct elevated temperature miniature tests in an inert cube-corner indenters’, Philos. Mag., 2006, 86, (33–35), 5265–5283.
environment, such as high purity argon or a vacuum. 14. X. D. Hou, A. J. Bushby and N. M. Jennett: ‘Study of the
The use of miniaturised test methods is expected to interaction between the indentation size effect and Hall–Petch
effect with spherical indenters on annealed polycrystalline
grow quickly and contributions in the fields of copper’, J. Appl. Phys. D, 2008, 41D, 074006–074012.
durability, fatigue (including thermomechanics), ele- 15. J. R. Greer: ‘Bridging the gap between computational and
vated temperature and dynamic testing will be very experimental length scales: a review on nano-scale plasticity’,
welcome and expected to provide the required engineer- Rev. Adv. Mater. Sci., 2006, 13, 59–70.
ing insights that will promote safe, efficient and 16. J. R. Greer, W. C. Oliver and W. D. Nix: ‘Size dependence of
mechanical properties of gold at the micron scale in the absence of
sustainable use of resources and contribute to cost strain gradients’, Acta Mater., 2005, 53, 1821–1830.
effective practices in both materials and equipment. In 17. R. Maab, S. van Petegem, J. Zimmermann, C. N. Borca and
addition to the laboratory based systems described, the H. van Swygenhoven: ‘On the initial microstructure of metallic
future demand and challenges lies in transferring some micropillars’, Scr. Mater., 2008, 59, 471–474.
of the methodologies to provide real time, in situ 18. H. Bei, S. Shim, G. M. Pharr and E. P. George: ‘Effects of pre-
strain on the compressive stress–strain response of Mo-alloy
measurement of properties on components in the field. single-crystal micropillars’, Acta Mater., 2008, 56, 4762–4770.
19. D. Kiener, C. Motz and G. Dehm: ‘Micro-compression testing: a
Acknowledgements critical discussion of experimental constraints’, Mater. Sci. Eng.
A, 2009, A505, 79–87.
Metrology research on materials testing at NPL is 20. C. P. Frick, B. G. Clark, S. Orso, A. S. Schneider and E. Arzt: ‘Size
supported by the UK Government’s National Measure- effect on strength and strain hardening of small-scale111 nickel
compression pillars’, Mater. Sci. Eng. A, 2008, A489, 319–329.
ment System Programme. Members of various industrial
21. S. I. Rao, D. M. Dimiduk, T. A. Parthasarathy, M. D. Uchic,
advisory groups are thanked for their steer in develop- M. Tang and C. Woodward: ‘Athermal mechanisms of size-
ing appropriate test methods and providing suitable dependent crystal flow gleaned from three-dimensional discrete
engineering materials for test method development. dislocation simulations’, Acta Mater., 2008, 56, 3245–3259.
Colleagues M. G. Gee, M. Stewart, M. S. Loveday 22. C. Motz, D. Weygand, J. Senger and P. Gumbsch: ‘Micro-
bending tests: a comparison between three-dimensional discrete
and M. Brooks at NPL are acknowledged for their
dislocation dynamics simulations and experiments’, Acta Mater.,
contributions to some of the unique test methods 2008, 56, 1942–1955.
described in the paper. The authors would also like to 23. J. Senger, D. Weygand, P. Gumbsch and O. Kraft: ‘Discrete
acknowledge that the final content and structure of the dislocation simulations of the plasticity of micro-pillars under
paper were constructively influenced through detailed uniaxial loading’, Scr. Mater., 2008, 58, 587–590.
24. D. Kiener, W. Grosinger, G. Dehm and R. Pippan: ‘A further step
comments during the refereeing process.
towards an understanding of size-dependent crystal plasticity: in
situ tension experiments of miniaturized single-crystal copper
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Aspects of Strain and Strength Measurement in Miniaturised Testing For Engineering Metals and Ceramics

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25 YEAR PERSPECTIVE

Aspects of strain and strength measurement

Introduction and scope lifetimes by aging, i.e. the mechanical characteristics of

ß 2010 Crown copyright

128 Materials Science and Technology 2010 VOL 26 NO 2

Techniques Advantages Disadvantages

Materials Science and Technology 2010 VOL 26 NO 2 129

Accuracy of calculated strain values

1286128 0.01–0.03 0.094%

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minimised, especially if accurate mechanical properties

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machining and preparation of micro testpieces, the

Small punch tests

136 Materials Science and Technology 2010 VOL 26 NO 2

plotted against time for a typical SP disc of original

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12 Inﬂuence of aperture (hole) diameter on SP creep test

stress levels were particularly sensitive to hole sizes

138 Materials Science and Technology 2010 VOL 26 NO 2

Table 3 Standardised tests for advanced technical ceramics

Testpiece type Standard Testpiece dimensions{, mm

Materials Science and Technology 2010 VOL 26 NO 2 139

14 Large deﬂection solutions for thin disc (non-

test can readily be scaled down to testpiece sizes of

(a) (b) (c)

140 Materials Science and Technology 2010 VOL 26 NO 2

(a) (b) (c)

strength may be determined by these ‘volume flaws’, and ð m

Materials Science and Technology 2010 VOL 26 NO 2 141

Studies such as these show that prediction of

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features. A scanning microhardness indentation test

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Materials Science and Technology 2010 VOL 26 NO 2 147

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