Acta Materialia 55 (2007) 4277–4286

www.elsevier.com/locate/actamat

Fracture toughness of carbides in tool steels evaluated

by nanoindentation
a,*
Daniel Casellas , Jaume Caro a, Sı́lvia Molas a, José M. Prado a, Isaac Valls b

a
CTM – Technological Centre, Avda Bases de Manresa, 1, 08242 Manresa, Spain
b
ROVALMA S.A., Apol.lo 51, PI Can Parellada, 08228 Terrassa, Spain

Received 29 March 2006; received in revised form 27 March 2007; accepted 29 March 2007
Available online 25 May 2007

Abstract

In this study, the hardness and fracture toughness of different primary carbides present in tool steels have been evaluated by nano-
indentation. Toughness was evaluated by the indentation method using Laugier’s equation, after experimentally assessing its applicabil-
ity. The results obtained allow different types of carbides to be discerned, in terms of hardness and toughness, which ranges from 2.2 to
3.7 MPa m1/2. It has been found that M7C3 carbides exhibit a marked fracture resistance anisotropy, which is lower in the direction par-
allel to its larger edge. This anisotropy is related to the crystalline texture. The relationship between hardness and toughness of the ana-
lysed carbides can be used as a guideline for the selection of the most appropriate type of carbide that the microstructure should contain
in order to optimize the wear behaviour and the fracture resistance of a tool steel.
 2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Toughness; Nanoindentation; Carbides; Microstructure; Steel

1. Introduction act as a fracture initiation site, breaking under applied

The processes forming high-strength materials require
the use of high-performance tool steels, since the applica-
tion of high pressures produces accelerated wear of the
forming tools, sometimes even leading to their catastrophic
and premature failure. Wear has traditionally been over-
come by increasing hardness, which inevitably leads to a
decrease in toughness, but this strategy cannot be applied
to high-pressure forming operations, where tools must be
tough enough to withstand the high loads involved. This
fact means that the hardness–toughness relationship in tool
steels must be optimized through accurate microstructural
design.
Carbides play an important role in the mechanical
response of tool steels, since they act as hard particles
and dictate the wear resistance. The dimensions and mor-
phology of carbides must be controlled, since they often
*
Corresponding author. Tel.: +34 93 877 7373; fax: +34 93 877 7374.
E-mail address: daniel.casellas@ctm.com.es (D. Casellas).
stress and leading to failure [1,2]. Thus, the properties of
carbides affect both the wear and fracture resistance of tool
steels. Accordingly, the relationship between the wear and
fracture resistance of tool steels should be optimized con-
sidering the mechanical properties that govern the wear
and fracture resistance, i.e. the hardness and fracture
toughness of the carbides. A detailed knowledge of this
relationship is crucial in order to develop high-performance
tool steels.
However, there is a lack of knowledge about the
mechanical behaviour of carbides in tool steels, mainly
due to the experimental difficulties associated with its mea-
surement. Warren evaluated the fracture properties by the
hertzian indentation of metallic carbides, obtained by sin-
tering [3]. However, the composition, and thus the proper-
ties, of these monolithic carbides may differ considerably
from those of carbides found in tool steels. To our knowl-
edge, only Berns [4] has reported values (of about
2.6 MPa m1/2) of microhardness for some chromium and
niobium primary carbides in tool steels.

1359-6454/$30.00  2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.actamat.2007.03.028
4278 D. Casellas et al. / Acta Materialia 55 (2007) 4277–4286
The present paper shows that nanoindentation is a suit-
able technique for the mechanical characterization of
micrometer-sized carbides in tool steels, in terms of hard-
ness, elastic modulus and fracture toughness. While hard-
ness and elastic modulus can be routinely measured by
nanoindentation [5], the evaluation of fracture toughness
of hard phases has received little attention. Fracture tough-
ness (KC) can be readily measured in hard materials by
inducing cracks at the corners of the indentation, a method
known as indentation microfracture (IM) [6–11]. The
application of IM is especially suited to the primary car-
bides in tool steels, where it is aimed at obtaining by nan-
oindentation a relevant mechanical parameter in tool steel
microstructural design, such as the KC of the hard and brit-
tle phase of the microstructure (i.e. the carbides).
In light of the above, the aim of this study is twofold:
first, to evaluate the fracture toughness of primary carbides
in tool steels, and secondly, to shed light on the KC of
small, second-phase particles using the IM method by nan-
oindentation, through an accurate assessment of the appli-
cability of some available expressions.
2. Fracture toughness measurement through nanoindentation
Small surface cracks of controlled size and shape can be
induced in most hard materials by the application of sharp
indenters. The final morphology of the indentation cracks
depends on the indentation load, the tip indenter geometry
and the toughness of the material. Halfpenny or radial
cracks, which are connected underneath the hardness
impression (Fig. 1a), are the most common crack configu-
ration for brittle materials [6], while Palmqvist cracks
(Fig. 1b) are developed at low indentation loads or in
high-toughness materials (such as hard metal [7] or zirconia
ceramics [8]). Transition between both crack configurations
takes place when the indentation load is increased.
The cracks emanating from the corners of a Vickers or
Berkovich indenter are arrested when the residual stress
driving force at the crack tip is in equilibrium with the
KC. Thus, KC can be readily measured in brittle materials
by measuring these indentation cracks. Several expressions
are available to determine KC by the IM method, depend-
a b c edges of the pyramid are more easily constructed to meet
Fig. 1. (a) Radial cracks emanating from a Vickers indenter impression;
(b) Palmqvist cracks emanating from a Vickers indenter impression and (c)
cracks emanating from a Berkovich indenter impression.
ing on the indenter geometry and crack morphology [6,7,9].
One of the most widely used expressions for radial cracks is
the relationship proposed by Anstis et al. [6]:
 n
E P
KC ¼ A ð1Þ
H c3=2
where P is the indentation load, c is the crack length, E is
the Young’s modulus and H is the hardness. The constants
A and n have been empirically determined by Anstis et al.
as A = 0.016 and n = 0.5 [6].
For Palmqvist crack configurations many expressions
have been developed to calculate KC. Among others, the
expressions proposed by Niihara et al. [7] and Laugier [9]
are commonly used. Niihara et al. proposed the following
expression:
 2=5
E P
KC ¼ w pffiffi ð2Þ
0:927H a ‘
where a is the half-diagonal of the indentation impression,
‘ is the crack length (see Fig. 1b) and w is a material con-
stant, estimated by Niihara et al. to be 0.0089 for WC–Co
materials. The expression developed by Laugier is:
a1=2  E 2=3 P
K C ¼ xV ð3Þ
‘ H c3=2
xV was determined as 0.015 by fitting Eq. (3) to data previ-
ously generated by Anstis et al. [6] using a Vickers indenter.
The applicability of expression (1) is limited to half-
penny cracks. This crack system is easily applied to the
symmetrical geometry of Vickers indenters (Fig. 1a). How-
ever, the nonsymmetrical nature of Berkovich indenters
does not permit the radial cracks to join beneath the hard-
ness impression based upon halfpenny cracking (Fig. 1c),
and the application of Eq. (1) is doubtful. Moreover,
another major difference between Vickers and Berkovich
indenters is the number of radial cracks. Ouchterlony has
investigated this effect [10] and based on their results KC
values may be obtained with the three-sided Berkovich
indenter by Eq. (3) with a little modification of xV
(xV = 0.016). The comparison of the measurements of KC
with Vickers and Berkovich indenters is extensively
detailed in the work of Dukino and Swain [11].
The Berkovich indenter is generally used in small-scale
nanoindentation studies and has the advantage that the
at a single point, rather than the inevitable line that occurs
in the four-sided Vickers pyramid. However, in many pre-
vious studies where KC was evaluated by nanoindentation
using Berkovich indenters, the most commonly used
expression is Eq. (1), whose applicability has mainly been
tested with Vickers indenters [12,13]. It is clear that accu-
rate KC measurements require that the crack morphology
be taken into account when choosing the expression to cal-
culate KC. Characterization of small second phases, like
carbides in the present work, is conducted with Berkovich
indenters at low loads that are expected to give rise to
Palmqvist-type cracks. Accordingly, Eqs. (2) and (3) are
 D. Casellas et al. / Acta Materialia 55 (2007) 4277–4286 4279

expected to provide better results than Eq. (1). Experimen-
tal results will help to assess the applicability of expressions
(1)–(3) to evaluate KC by nanoindentation.
3. Experimental
3.1. Material characterization
The study is focused on the primary carbides of different
tool steels, with noticeable differences in chemical composi-
tion and thus with very different types of carbides. The
studied steels were a conventional high chromium-high car-
bon tool steel, with denomination DIN 1.2379 or AISI D2,
and a high-speed steel with denomination DIN 1.3202 or
AISI T15. These steels are widely applied in cold forming
operations and their microstructures are well studied [14–
17]. In addition, in order to have different types of carbides,
an experimental cold-work steel developed by ROVALMA
was used. Two different thermomechanical treatments were
performed on this steel that produced two microstructures
containing different primary carbides, named as steel A and
steel B. Chemical compositions of these steels are shown in
Table 1. Table 2 details the heat treatment schedule along
with the obtained hardness, on the Rockwell C scale
(HRC), for each steel.
As carbide orientation strongly affects the properties of
the tool steels, samples were extracted with the same car-
bide orientation, that is, parallel to the rolling direction.
The chemical composition of the carbides was evaluated
Indenter XP (MTS) system fitted with a Berkovich dia-
mond tip. The tip was calibrated on a fused silica sample
using the Oliver and Pharr method [5,13]. The evaluations
of H and E were conducted as a function of depth penetra-
tion into the carbide using the continuous stiffness mea-
surement (CSM) operation mode. During the CSM
operation, the AC load was controlled to give a 2 nm har-
monic displacement amplitude at 45 Hz. The samples were
allowed to thermally equilibrate with the instrument until
the drift rate was measured to be below 0.080 nm s1.
The indentations were carried out at a constant strain rate
of 0.050 s1 up to a maximum load of 400 mN. A Poisson’s
ratio of 0.25 was supposed for all the samples.
Expressions (1)–(3) were applied to evaluate KC by using
Berkovich indenters at an indentation load range from 0.2
to 0.5 N. Crack length was measured by scanning electron
microscopy (SEM).
4. Results
The nanoindentation results are shown in Fig. 2, reveal-
ing the existence of carbides with different hardness. Aimed
at rationalizing these differences, carbides were identified
a 400
Young's modulus (GPa)

by energy-dispersive X-ray microanalysis (EDAX). Due 350

to experimental limitations, the amount of carbon was
not determined using this technique. Carbide identification
300
and in-plane texture measurements (pole-figure) were per-
formed by X-ray diffraction (XRD) using a Philips Mate-
MC (steel 1.3202)
rial Research Diffractometer system with a four-circle 250 M6C (steel 1.3202)
goniometer and parallel beam optics.
M7C3 (steel 1.2379)
3.2. Micromechanical evaluation 200
10 15 20 25 30 35
Hardness (H), elastic modulus (E) and KC of carbides Hardness (GPa)
were measured by means of nanoindentation using a Nano-
b 400
Table 1
Chemical composition of the studied steels (in wt.%)
Young's modulus (GPa)

350
Steel C Cr Mo V W Co
1.2379 1.5–1.6 11.0–12.0 0.6–0.8 0.9–1.0 – –
1.3202 1.5–1.6 3.7–5.0 1.0 max 4.5–5.2 11.7–13.0 4.7–5.2 300
Steel A, B 0.9–1.2 6.5–8.5 – 2.5–3.0 1.1–1.4 –
MC-III
250 MC-II
Table 2 MC-I
M7C3 (steel A)
Heat treatments applied to the studied steels and obtained hardness
Steel Austenizing (quench in oil) Tempering HRC 200
10 15 20 25 30 35
1.2379 1050 C for 30 min 400 C for 2h (·2) 57.0 ± 0.5
1.3202 1250 C for 5 min 550 C for 2h (·3) 66.2 ± 0.3 Hardness (GPa)
Steel A 1060 C for 35 min 540 C for 2h (·3) 61.3 ± 0.1
Fig. 2. Nanoindentation results of E and H: (a) carbides in 1.2379 and
Steel B 1090 C for 60 min 540 C for 2h (·3) 61.5 ± 0.2
1.3202 steels and (b) carbides in steels A and B.
4280 D. Casellas et al. / Acta Materialia 55 (2007) 4277–4286

Table 3 4
Chemical composition of the metal part of carbides (in wt.%) Equation (3)
Steel Carbide Fe Cr V Mo W Equation (2)
3 Equation (1)

KC (MPa m )
1.2379 M7C3 40–45 46–51 6.0–6.5 2–3 –

1/2
1.3202 MC 2–4 3–5 50–75 1.0 20–45
1.3202 M6C 26–31 3–5 3.5–4.5 1.5–2.5 58–62
2
Steel A MC-I 2–6 8–10 50–70 – 7–12
Steel A M7C3 35–45 35–45 10–20 – 2–4
Steel B MC-II 2–3 8–10 60–70 – 7–12
Steel B MC-III 2–3 8–10 70–80 – 3–6
1

by means of their chemical composition as well as their
crystal structure obtained from XRD. The results are
shown in Table 3.
In 1.2379 tool steel, there is only one type of primary
carbide, the M7C3, as it is well established for this steel
[1]. The microstructure of high-speed steels always presents
MC and M6C [14–17], which have been also identified in
the 1.3202 steel (Table 3). The MC carbide has a face-cen-
tred cubic (fcc) structure and is often found in tool steels. It
mainly dissolves V, with incorporation of W and small
amounts of Cr and Fe. It has been reported that MC is
the carbide phase with the greatest composition variability
[15,16]. This assertion is also supported by the results
obtained here, where the vanadium content varies from
50% to 70% (Table 3). The M6C carbide has a complex
fcc structure and it is a W-rich carbide with a considerable
content of Fe and moderate amounts of Cr and V. The
chemical composition of M6C is quite stable [16,17], as is
also shown in the 1.3203 steel, where M6C carbides exhibit
little variation of W and Fe content (see Table 3).
In steel A there are two types of primary carbides. The
soft ones are M7C3 but with higher contents of V and W
than those found in the 1.2379 steel. As has been well
established, these elements are used to replace Cr in the
crystalline structure of the carbide [14]. The hard carbide
in steel A has been identified as an MC type, with a differ-
ent amount of W than the MC carbide found in 1.3202
steel. Again, this MC carbide in steel A shows considerable
variability in its content of V (Table 3). Steel B was treated
at temperatures that induce the dissolution of the M7C3,
and promote the nucleation of more MC carbides and
the growth of the pre-existing ones. As a result, steel B only
contains MC carbide with a different composition (see
Table 3).
Fracture toughness has been evaluated for each set of
carbides using Eqs. (1)–(3). The results obtained are shown
in Fig. 3, where clear differences in the calculated KC can be
seen depending on the expression used. More than 20 car-
bides of each set were indented, but the experimental diffi-
culties associated with the small dimensions of carbides
yields only about five valid measurements (asymmetrical
cracks as well as indentations too close to carbide edge
were rejected) for each type of carbide. Figs. 4 and 5 show
indented carbides in the 1.3202 steel and steels A and B,
respectively. All the carbides analysed exhibit cracks ema-
nating from the indentation corners, without chipping, at
0
C3 C-
I - II - III C C
M7 AM MC MC -M6 2-M
7 9 -
L L B L B
0 2 0
3 E E E 2 2
1.2 ST
E
ST
E
ST
E 1 .3 1 .3
Fig. 3. Values of fracture toughness evaluated with expressions (1)–(3).
the applied load levels. Only the M7C3 in steel A does
not develop cracks, owing to its low hardness (14.5 GPa).
It is reported that lowering hardness increases the thresh-
old load for generating cracks from the indentation corners
[18]. Considering the same toughness of the M7C3 found in
1.2379 steel, the threshold indentation load calculated by
the expression given for Lawn and Marshall is doubled
(larger than 0.5 N) [18]. However, the relatively small size
of these carbides, about 5–10 lm, together with their hard-
ness, hampers the application of loads higher than 0.5 N,
as they give rise to indentations larger than the carbide.
On the other hand, results obtained in 1.2379 steel show
a marked dependence on the carbide orientation. Primary
carbides in tool steel are elongated as a consequence of
the forging steps during fabrication. Results show that
the cracks emanating from the indenter corners propagate
more easily in the direction parallel to the larger edge of the
carbide, following the elongated shape of the carbide. This
effect is clearly shown in Fig. 6. In most cases, cracks only
appear in the direction parallel to the major axis of the car-
bide, independently of the indenter orientation (see arrows
in Fig. 6b). Carbides in this steel are large enough to give
better experimental results than steels with small carbides,
allowing more than 25 valid measurements to be obtained.
Considering that using a three-sided diamond tip (Berko-
vich) the orientation of the indenter may be critical to see
anisotropy effects, the indenter orientation has been kept
constant with respect to the carbide direction during mea-
surements. Moreover, to see the effect of indenter orienta-
tion, some measurements were conducted tilting the
indenter with respect to the carbide direction. Results indi-
cated that cracks still propagate parallel to the carbide’s
large edge, as shown in Fig. 6b and c. All these measure-
ments allow two sets of KC values to be discriminated,
one smaller than 1 MPa m1/2 and the other between 1.3
and 4.5 MPa m1/2 (see Fig. 7). The KC data lower than
1 MPa m1/2 was calculated from cracks that propagate par-
allel to the carbide’s larger edge; meanwhile, the other data
set was calculated from cracks that run perpendicular to
 D. Casellas et al. / Acta Materialia 55 (2007) 4277–4286
Fig. 4. Indented carbides in 1.3202 steel: (a, b) M6C and (c) MC.
the carbide’s larger edge. Such results allow us to state that
fracture resistance in M7C3 carbides is highly anisotropic
and clearly depends on the direction of the carbide.
5. Discussion
5.1. Fracture toughness measurements
Fig. 3 shows the marked effect of the expressions used to
compute KC from indentation crack lengths. The expres-
4281
Fig. 5. Indented carbides in steels A and B: (a) MC type I; (b) MC type II;
and (c) MC type III.
sions tested have been shown to give accurate results in
ceramics and hard metals, using both Berkovich and Vick-
ers indenters. However, they have been applied mostly to
bulk materials, without restrictions on the load applied
or the crack length. In the present investigation the dimen-
sions of the carbides (10–20 lm) require the use of low
loads in order to produce small cracks, shorter than
5–10 lm, within the carbide. At this crack extension the
4282 D. Casellas et al. / Acta Materialia 55 (2007) 4277–4286

Fig. 6. (a) Indented M7C3 in 1.2379 steel. (b, c) Effect of indenter tilting in M7C3. Cracks propagate parallel to the carbide’s larger edge (see white and
black arrows).

application of expressions (1), (2) or (2) could give rise to
considerable differences in the calculated value of KC, as
shown in Fig. 3. In Fig. 8 the KC obtained with the three
different expressions is plotted as a function of crack
length. From this plot it is clear that at short crack lengths
Laugier’s expression gives the highest values of KC (2.4
times larger than Anstis’s expression for M6C carbides in
1.3202 steels, as shown in Fig. 8). According to these com-
ments, it is clear that the accurate evaluation of KC with
short cracks, as occurs in nanoindentation tests at low
loads, requires the proper selection of the expression used
to calculate it.
From a geometrical point of view, and considering that
a Berkovich indenter was used in the nanoindentation tests,
expression (3) seems to be the most appropriate, as postu-
lated in Section 2. This expression has been successfully
proved in a wide range of ceramic materials using Berko-
vich indenters to induce cracks from indentation corners
[11]. However, the differences between the results obtained
with expressions (1)–(3) indicate that its applicability
should be assessed. Moreover, it should be considered that
the IM method uses a constant (A, w and xV of Eqs. (1)–(3)
respectively) that is empirically adjusted in order to repro-
duce the fracture toughness of a set of different brittle
 D. Casellas et al. / Acta Materialia 55 (2007) 4277–4286 4283

0.15 1.2379 steel a

Frequency

0.10

0.05

0.00
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
1/2
KC (MPa m )

Fig. 7. Scatter in the values of the KC of M7C3 in 1.2379 steel.

b 1.2 Fracture toughness of Si single

crystals in the (100) plane
1.1

1.0

KC (MPa m )
1/2
0.9

0.8

0.7

0.6

0.5
Fig. 8. KC values calculated by the expressions (1)–(3) at P = 0.2 N and

al

al

l
)

a
(2
(1

a = 2.8 lm (corresponding to the M6C carbides of the 1.3202 steel). (3

et
et

et
n

n
io

io

tio

n
ed
Xi

he
t

t
ua

ua

ua

Br

C
Eq

Eq

Eq

materials. Calibration of this constant for a wide range of

materials may reduce the accuracy of the results obtained c 8
[19]. In this sense, methods that do not use an empirical 7
constant, such as those based on the propagation and frac-
6
ture of large cracks, are expected to give more accurate
results. Thus, in order to assess the applicability of expres- 5
sions (1)–(3) in the calculation of KC with short indentation 4 Si (100)
M7C3 (steel 1.2379)
cracks, the IM method was applied to a material whose KC 3
MC-III
is well known by using low loads. The results were com- MC-II
2
pared with the KC values obtained with a method based MC (steel 1.3202)
on large cracks that are assumed to be more accurate. 1 M6C (steel 1.3202)
The chosen material to perform this comparison was Si, 0
0 1 2 3 4 5 6 7 8
because its KC has been well reported (for measurements
conducted by large crack testing methods, see Refs. [20–
22]) and it may be easily obtained as a single crystal (since Fig. 9. (a) Nanoindentation at 0.2 N in Si on the plane (1 0 0). (b)
the applied loads are too low, a single crystal is preferred to Comparison between KCs calculated in Si (1 0 0) with expressions (1)–(3)
avoid uncertainties relating to the interaction between and those obtained with large crack testing methods [18–20]. (c) Relation
between the half-diagonal impression (a) and the indentation crack length
crack propagation and grain boundary and grain orienta-
(l) in the studied materials.
tion). However, Si single crystals present a marked anisot-
ropy of properties [21,23], which implies that comparisons
may be done considering that measurements were con- Fig. 9b together with the values of KC obtained with large
ducted on the same crystallographic plane. The indented crack testing methods [20–22]. It can be seen that Niihara
plane in the present study was the (1 0 0) plane, and the val- and Laugier’s expression (using the modified factor
ues of KC were selected from the literature. xV = 0.016, as proposed by Dukino and Swain [11]) gives
Fig. 9a shows the nanoindentation results on Si (1 0 0) at values of KC within the range of the values of Si reported
0.2 N. The results obtained using Eqs. (1)–(3) are plotted in with large crack testing methods. However, Niihara et al.
4284 D. Casellas et al. / Acta Materialia 55 (2007) 4277–4286

set the applicability of expression (2) within the range MC (steel 1.3202) MC-I MC-II MC-III
0.4 < a/l < 1. Fig. 9c plots the relation between a and l in M6C M7C3 (steel 1.2379) M7C3 (ref. 4)
5 NbC (ref. 4) ZrC (ref. 3) VC (ref. 3)
the analysed carbides and Si (1 0 0). It is clear that almost
all the data for carbides lie outside this range. Thus, all
4
these comments allow us to point out that the evaluation

Kc(MPa m )
1/2
of KC by nanoindentation should be conducted using the 3
expression proposed by Laugier, with xV = 0.016. This
assertion is especially relevant at low applied loads, when 2
cracks are shorter than 10 lm, which usually occurs in nan-
oindentation of small particles. 1

5.2. Fracture toughness of carbides 0

14 16 18 20 22 24 26 28 30 32
H (GPa)
The results obtained are summarized in Table 4, which
shows clear differences in the mechanical behaviour of dif- Fig. 10. Hardness and fracture toughness of different carbides. Arrows for
ferent carbides in tool steels. These differences are obvi- M7C3 present in 1.2379 steel indicate that KC may be even lower.
ously related to their crystalline structure and chemical
composition. The obtained hardness values are in agree-
ment with those previously reported for similar carbides 5.0
[14,15]. Hardnesses of about 16.5 GPa are found for M6C 4.5
carbides in high-speed steels [14]. M7C3 carbides have also
4.0
been well studied in the 1.2379 steel, with values reporting KC (MPa m )
1/2

of about 18 GPa [14]. The MC carbides present high hard- 3.5

ness, about 25–30 GPa for VC [14,15], similar to the values 3.0
measured in this study (see Table 4). MC type carbides
2.5 MC (steel 1.3202)
There is little information relating to the fracture
2.0 MC-I (steel A)
toughness of carbides in tool steels. To our knowledge,
MC-II (steel B)
only Berns [4] has evaluated the KC of M7C3 and NbC 1.5 MC-III (steel B)
in tool steels by microindentation using Eq. (2). Previ-
1.0
ously, Warren evaluated the KC of bulk carbides by 0 5 10 15 20 25
hertzian indentation [3]. Reported values for these V/W
authors are shown in Fig. 10, together with the experi-
mental values obtained in the present work, with which Fig. 11. Toughness (KC) vs. composition of the MC carbides.
they are in good agreement. Moreover, and for compar-
ison purposes, the experimentally obtained values of KC function of the V/W ratio for the carbide. The figure shows
for the studied carbides lie in the range of ceramic mate- that V-rich carbides exhibit high values of KC.
rials (see, e.g. Ref. [24]). For sintered polycrystalline SiC, With regard to the marked anisotropy in fracture tough-
widely studied as a bulk material, KC ranges from 2.5 to ness detected in M7C3, the same effect has been previously
4.0 MPa m1/2 [24,25]. The fracture toughness of bulk B4C reported for other covalent materials, like SiC, TiC and
varies from 2.6 to 3.4 MPa m1/2, depending on its density Si3N4. In SiC and Si3N4 this effect is due to a marked tex-
after sintering [26]. ture development [25,27]. Meanwhile, in TiC single crys-
In order to show the dependence of toughness on com- tals, the KC ranges from 1.5 to 3.6 MPa m1/2 due to
position, the evolution of KC in MC-type carbides, present crystallographic anisotropy [28]. Considering that M7C3
in 1.3202 steel and steels A and B, is plotted in Fig. 11 as a carbides are also single crystals, the preferred orientation

Table 4
Mechanical properties measured by nanoindentation
Steel Carbide H (GPa) E (GPa) KC (MPa m1/2) Eq. (3) xV = 0.016
1.2379 M7C3 18.2 ± 2.4 294 ± 17 2.3 ± 0.8a
1.3202 M6C 18.1 ± 1.3 318 ± 15 3.3 ± 0.5
1.3202 MC 24.7 ± 1.2 338 ± 16 2.2 ± 0.4
Steel A M7C3 14.5 ± 2.5 270 ± 18 –
Steel A MC-I 25.7 ± 3.6 315 ± 23 3.7 ± 0.6
Steel B MC-II 20.3 ± 1.2 272 ± 18 2.7 ± 0.5
Steel B MC-III 26.1 ± 0.9 316 ± 20 3.7 ± 0.5
Different MC carbides in steels A and B are identified as I, II and III.
a
KC evaluated in the direction perpendicular to the larger edge of the carbide in 1.2379 steel.
 D. Casellas et al. / Acta Materialia 55 (2007) 4277–4286
Fig. 12. Pole figure at 2h = 39.44 for (024) obtained by XRD in 1.2379
steel.
of the carbides was experimentally assessed by means of
XRD. The pole-figure at 2h = 39.44 for (024) reflections
reveals that carbides are strongly in-plane textured
(Fig. 12), which supports the anisotropy in fracture resis-
tance that has been revealed experimentally. This statement
is very helpful in understanding the effect of carbide band
orientation on the mechanical behaviour of tool steels.
Considering that primary carbides act as fracture initiation
sites, it is clear that fracture resistance anisotropy in pri-
mary carbides will lead to macroscopic anisotropic behav-
iour in tool steels, as is found in forged tool steel [29].
On the other hand, the relationship between H and KC
can be used as a guideline for the selection and design of
the most appropriate type of carbide that a tool steel
should contain for a given mechanical requirement.
Accordingly, carbides showing high H and high KC are
especially suitable for applications where high wear and
fracture resistance are demanded. Forming operations of
high-strength materials implies the use of high loads during
cutting or drawing, which produces accelerated wear or
premature tool failure if the microstructural constituents
do not present high values of H and KC. In conventional
tool steel, increasing the KC by quenching–tempering heat
treatments results in a decrease in H, which hampers the
production of hard and tough microstructures. This diffi-
culty may be overcome by microstructural design, selecting
hard and tough carbides which allow high-performance
tool steel to be obtained. Fig. 10 rates the properties of
the different carbides analysed, by comparing the measured
H and KC. Carbides located at the upper right hand of the
graph fit these requirements, and are potential candidates
for incorporation into tool steels aimed at optimizing the
relationship between wear and fracture resistance.
4285
6. Summary and conclusions
The fracture toughness of different primary carbides in
tool steels has been evaluated by nanoindentation in differ-
ent tool steels. The carbides analysed are identified as MC,
M6C and M7C3, and are 10–20 lm in size. In order to
obtain valid measurements of KC the indentation cracks
should remain within the carbide, i.e. cracks should be
about 5–10 lm in length. At this crack extension the calcu-
lation of KC by the IM method strongly depends on the
expression used. Accordingly, it is clear that the accurate
evaluation of KC with short cracks requires the proper
selection of the expression used to calculate it. Thus, the
applicability of different expressions has been experimen-
tally assessed, indicating that the evaluation of KC by nan-
oindentation should be conducted using the expression
proposed by Laugier, with xV = 0.016. This assertion is
especially relevant at low applied loads, where cracks are
shorter than 10 lm, as usually occurs in nanoindentation
testing of small second-phase particles.
The results obtained allow different types of carbides to
be discerned, in terms of toughness and hardness. More-
over, the in situ evaluation of the KC of carbides present
in tool steels is especially relevant considering the lack of
knowledge relating to this property. Quantification of H
and KC of carbides is essential in order to design micro-
structures that optimize both wear behaviour and fracture
resistance, aimed at developing high-performance tool
steels. In this sense, the best combination of hardness and
toughness has been found in MC carbides with a high V
content.
Indentation tests have also revealed a clear anisotropy
effect on the fracture resistance of the primary M7C3 car-
bide present in 1.2379 steel. This anisotropy is related to
the crystalline texture measured by XRD.
Acknowledgements
This work was partially financed by the Catalan Gov-
ernment’s Ministry of Employment and Industry, through
Grant No. CT05-1-1001, and the Spanish MEC, through
Grant No. DPI2006-12279. The authors express their grat-
itude to M. Marsal for her technical assistance during SEM
observations and P. Bassas for XRD measurements.
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