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Journal of the European Ceramic Society

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Original Article

A detailed analysis of the determination of fracture toughness by

nanoindentation induced radial cracks
Yuning Guo, Thorsten Staedler⁎, Julian Müller, Steffen Heuser, Benjamin Butz, Xin Jiang⁎
Institute of Materials Engineering, University of Siegen, Paul-Bonatz-Str. 9-11, 57076, Siegen, Germany

AR T ICLE INFO ABSTRAC T

Keywords: The correlation between the choice of reference material and model utilized in determining fracture toughness
Fracture toughness from indentation-induced radial cracks was critically investigated with six commonly used reference materials.
Radial crack Initially, the empirical constants in Anstis’s and Laugier’s equations were calculated, compared and analyzed.
Nanoindentation According to the values of the constants, the reference materials were categorized into three groups. This
Reference materials
classification was further verified by evaluating the corresponding constants of 13 additional equations. To
Diamond/SiC composite film
account for the classification, FIB technique was employed to examine the crack morphology in the reference
materials – Si (100) features an almost Half-penny-shaped crack while the cracks in SiC (0001) display nearly as
a rectangle, both far from the assumptions employed by the models. Subsequently, an improved and more
reliable procedure to determine fracture toughness is proposed. Finally, with this procedure, the fracture
toughness of a diamond/SiC composite film is determined to be 11.1 ± 1.1 MPa m1/2.

1. Introduction
The determination of fracture toughness from the length of in-
dentation induced radial cracks is a widely used strategy, the origin of
this concept dates back to 1957 when Palmqvist [1,2] proposed an
empirical relation between crack length and the maximum applied
load. In 1980, Lawn, Evans and Marshall (LEM) proposed a fracture
toughness equation based on elastic-plastic fracture mechanics, Eq. 1
[3], where E, H, Pmax, c and χ are elastic modulus, hardness, maximum
indentation load applied, total crack length, and a dimensionless con-
stant, respectively. It should be noted here, that in order to render the
indentation-based fracture toughness discussed in this work compliant
with modern standards and nomenclature, KIF (indentation fracture
toughness) will be used instead of KIC in all original fracture toughness
equations throughout this work. In 1981, Anstis employed a number of
reference materials including mono-, polycrystalline and amorphous
ceramics, which covered a large regime of fracture toughness values
ranging from 0.74 to 12 MPa m1/2, and carried out corresponding tests
with a Vickers indenter to derive the dimensionless constant in Eq. 1
and ended up with a value of χ = 0.016 ± 0.004. Thereafter, this
equation is frequently referred to as Anstis’s equation. It is based on a
Half-penny crack type and the boundary condition that c≫a is sug-
gested (c is the total crack length, whereas, a denotes the crack length
measured from the center to the corner of the remaining imprint, see
Fig. 1(a)). [4]. In 1987, Laugier [5,6] found that ceramics typically
display a Palmqvist type (Fig. 1(b)) instead of Half-penny type crack
morphology and modified Anstis’s equation by adding the term (l/a)−1/
2
to Anstis’s equation (c/a ≥ 1.3), see Eq. 2 (l represents the crack
length measured from the corner of the remaining imprint of the in-
denter to the end of the crack). He argued that Anstis’s equation is able
to reliably describe Palmqvist crack to some extent as the additional
term often only features a minor impact on the relationship. Both An-
stis’s and Laugier’s equations allow us to estimate fracture toughness
from directly measurable parameters (e.g. E, H, Pmax, c, l and a). In
addition to Anstis’s and Laugier’s equations, a diversity of equations
dealing with fracture toughness determination from radial crack length
have been proposed in the 1980s, which are based on Anstis’s equation.
However, these equations only exhibit slight changes to the exponent n
in the (E/H)n part and additional changes to the dimensionless con-
stant. A systematic work reviewing these equations has been carried out
by Ponton et al. [7], in which they summarized nineteen equations from
different references into 7 generic equations.
KIF = χ (E/H)1/2 Pmax c−3/2 (1)
KIF = χv (E/H)2/3 (l/a)−1/2 Pmax c−3/2 (2)
In recent years, the validity of fracture toughness determination
from radial cracks has triggered intense debate. Quinn and Morell et al.
[8–10] argued that the fracture toughness equations have various

⁎
Corresponding authors.
E-mail addresses: thorsten.staedler@uni-siegen.de (T. Staedler), xin.jiang@uni-siegen.de (X. Jiang).

https://doi.org/10.1016/j.jeurceramsoc.2019.10.013
Received 27 June 2019; Received in revised form 2 October 2019; Accepted 4 October 2019
Y. Guo, et al.
Fig. 1. (a) Half-penny crack and (b) Palmqvist crack created by a three-sided
Berkovich indenter.
confinement/problems in practical applications, such as the complexity
invoked by multiple crack types of the corresponding system (radial,
median, lateral, etc.), the uncertainty with respect to details of the
stress field beneath the indenter, and the sometimes inaccurate and
unreliable fracture toughness results based on this method. Thus, the
Vickers indentation fracture toughness technique should no longer be
acceptable for fracture toughness testing of ceramic materials. None-
theless, Marshall et al. [11] contradicted referring to the aspects that
the stress field beneath the indenter is generally well defined and
documented, and that the indentation fracture toughness method is
based on rigorous Griffith-Irwin equilibrium fracture mechanics.
Moreover, the indentation patterns are unique fingerprints of the me-
chanical behaviors of one material. Therefore, indentation fracture
toughness is still a valid method. Admittedly, there are still many issues
and shortcomings in the equations associated with fracture toughness
determination:
I) The most prominent issue is that none of the equations is universal
for all materials, thus the calculated fracture toughness varies a lot
from equation to equation although a fixed crack length is used.
This was demonstrated, for example, by Schiffmann [12] as he
examined four radial crack based equations (including Anstis’s and
Laugier’s equations) using a Cube corner indenter. It turned out that
none of the equations examined was suitable for all the materials
investigated (Si, fused silica, sapphire and several film systems). To
shed some light on this question, Ponton [13] investigated the
performance of nineteen equations with respect to various mate-
rials and suggested the optimum equations for each class of mate-
rial. However, the fundamental reason behind the non-universal
phenomenon is not explained and the choice of the most appro-
priate equation for an unknown material system still remains un-
solved.
II) With regard to the empirical constant contained within each frac-
ture toughness equation, it is generally believed that they are re-
lated to indenter geometry or centerline-to-face angle. The acqui-
sition of the constants is usually based on a method analogous to
the one proposed by Anstis, a linear fitting of experimental data
received from several reference materials whose elastic modulus,
hardness and fracture toughness are already known. However, the
Table 1
Summary of some important parameters utilized in references to derive empirical constants.
Year Researcher Indenter type Crack morphology Equation used
1981 Anstis [4] Vickers Half-penny Eq. 1
1987 Laugier [6] Vickers Palmqvist Eq. 2
1994 Harding [17] Cube-corner Radial cracks Eq. 1
2012 Cuadrado [16] Berkovich Palmqvist Eq. 1
Eq. 2
Cube-corner Palmqvist Eq. 2
number of reports dedicated to the procedure of deriving the con-
stants is limited. Table 1 summarized some important parameters
(e.g. indenter type, equation used, crack morphology and reference
materials) utilized in the corresponding references to derive the
empirical constants. Nevertheless, based on Quinn’s argument [8]
that any request of an universal empirical constant should end up in
vain, along with some additional issues regarding practical appli-
cations, it is reasonable to doubt, that taking and applying any of
the equations to an unknown system without any former adjust-
ments (in particular to the empirical constant) is a scientifically
valid approach. Pharr et al. [14] reported that different reference
materials yield in various constants, deviating from Anstis’s 0.016
for Vickers and Berkovich indenters. Besides, the fact that Anstis’s
constant (χ = 0.016 ± 0.004) was derived for tests carried out
under oil atmosphere should also be taken into consideration.
III) It is to date well-accepted that crack morphology is crucial in
choosing the appropriate equation. Generally, for a material with
Half-penny crack morphology, Anstis’s equation is preferred while
Laugier’s equation is more suitable for materials showing Palmqvist
cracks. Moreover, numerous factors contribute to the actual details
of crack morphology, including, but not limited to, residual stress,
indenter geometry, indentation load, material properties, densifi-
cation and environmental conditions. However, in the original
works, which derived the corresponding constants, the crack mor-
phology within the reference materials never has been carefully
examined nor considered. Cuadrado et al. [15,16] employed FIB
tomography to identify the crack morphology in their reference
materials (Si (100), SiC and soda lime glass), which were probed by
a Cube-corner indenter. Nevertheless, issue number one (none of
the equations is universally valid) still remained unanswered and
no guidelines or criterions have been derived to propose a standard
procedure to acquire fracture toughness.
IV) There is still confusion about the observation, that for a given
equation, the fracture toughness of some materials is always un-
derestimated (e.g. SiC, sapphire), while other materials fracture
toughness is overestimated.
In conclusion, to answer the questions above and to better under-
stand the fracture toughness mechanism itself, the existing equations to
determine fracture toughness from radial crack length need to be
carefully examined from the perspective of the empirical constant.
Moreover, in this work, the final crack morphology is considered as
output, while all other factors mentioned above, which affect crack
morphology, are regarded as input of a virtual black box. Guided by an
investigation of six commonly used reference materials and an ex-
amination of the crack morphology within some of the reference ma-
terials by FIB, we provide an answer to those questions – the im-
portance of choosing the appropriate reference materials. Finally, a new
or an improved procedure that could tackle these issues is proposed.
2. Experimental
In this work, all mechanical properties were measured by na-
noindentation (Hysitron TI 950 TriboIndenter, Hysitron Inc.). Single
Constant Reference material
0.016 ± 0.004 Si3N4, Al2O3, glass ceramic, glass
0.015 Data from Anstis
0.036 Fused quartz, Ge (111), pyrex, Sapphire (111), Si (100), Si (111), SiC, Si3N4, Soda
lime glass, spinel (100)
0.026 ± 0.001 Si (100), SiC (0001), soda-lime glass
0.022 ± 0.001
0.057 ± 0.002
Y. Guo, et al.
Table 2
Hardness and elastic modulus of the six reference materials.
Material Elastic modulus* (GPa) Hardness (GPa) Poisson ratio
[21–23]
Si (100) 174.05 ± 3.00 11.49 ± 0.17 0.28
Si (111) 166.21 ± 3.02 11.30 ± 0.20 0.27
Soda lime glass 76.96 ± 1.03 6.51 ± 0.11 0.22
SiC (0001) 538.98 ± 13.12 39.59 ± 1.26 0.19
Sapphire 427.19 ± 2.04 28.82 ± 1.06 0.29
Fused quartz 71.35 ± 0.74 8.89 ± 0.12 0.17
crystalline silicon with two orientations (Si (100) and Si (111)), soda-
lime glass, single crystalline silicon carbide (SiC (0001)), sapphire and
fused quartz were chosen as reference materials to study fracture
toughness and its correlation to the equations utilized for determina-
tion.
Prior to accessing fracture toughness, a Berkovich indenter with a
maximum load of ˜10 mN was employed to evaluate hardness and
elastic modulus of the reference materials. The results of each material
were derived from an average of more than 50 measurements and are
listed in Table 2. Loading and unloading rate were held constant for
each sample. The analysis of the load-displacement curves was based on
the method proposed by Oliver and Pharr [17]. The initial contact was
determined by assuming a tip rounding and fitting the first few nan-
ometers (˜10 nm) of the load-displacement curves with a P = C·(h’-h0)3/
2
relationship. [18] In order to generate cracks, a high load Berkovich
indenter (10 N) was employed. In this context, it is worthwhile to
mention, that all crack tests were carried out in a displacement con-
trolled manner rather than a load controlled one. This choice was made
due to the fact that fracture is often accompanied by a sudden change in
displacement, thus load controlled manner potentially might add extra
work to the system and consequently affect the crack length. For sta-
tistical reasons, about 30 crack tests were performed at various max-
imum load for each sample of interest. Subsequently, the crack lengths
(c, l and a) were examined and measured using a scanning electron
microscope (SEM, Zeiss Ultra 55). The actual position of the crack tips is
determined at high magnification to ensure an accurate measurement
of the crack length. Most importantly, to exclude the potential com-
plexity of multiple cracks, only indentations solely featuring radial
cracks (judging by the top-view SEM images) and not showing any R-
curve behavior were used to calculate fracture toughness. All other ones
that show lateral cracks, delamination, chipping or spalling at enhanced
indentation loads were discarded in this work.
In order to investigate the details of crack morphology below the
materials surfaces, the focus ion beam (FIB, Helios NanoLab 600) cross-
sectioning was utilized to create a series of cross-section images along
the crack as shown in Fig. 2. Sequentially, the crack morphology can be
reconstructed from the crack lengths observed on the various cross-
sections. In general, 5 or more cross-sections are created for the re-
construction depending on the total crack length.
Finally, a diamond/SiC composite film deposited by microwave
plasma chemical vapor deposition (MPCVD) was investigated. The de-
tails of the growth parameters as well as the strategy to access its
hardness and elastic modulus are given elsewhere. [19] Lastly, the
fracture toughness of this diamond/SiC composite film was evaluated
using the criterion developed within this work.
3. Result and discussion
3.1. The examination of Anstis’s and Laugier’s equations
Anstis’s and Laugier’s equations are the first that are examined with
respect to the six reference materials as they are likely the most widely
used equations for fracture toughness determination based on radial
cracks. The top-views of the indented surface region post testing are
Fig. 2. A schematic diagram illustrating the procedure utilized to obtain in-
formation about the crack morphology: The reconstruction is realized by cri-
tically analyzing a series of cross-sections along the indentation crack.
shown in Fig. 3. The triangular imprints caused by the three-sided
Berkovich indenter can be readily observed. Additionally, radial cracks
emanating from the corners of the indentation impressions can be
noted, while no signs of lateral cracks, delamination, chipping or
spalling is observed. In this context, fused quartz represents an excep-
tion as it exhibits frame-like cracks/cone cracks, which are presumably
caused by a different crack mechanism. This finding agrees well with
Cook et al.’s report. [20] They observed the appearance of cone cracks
in fused quartz at a very early stage in the loading cycle prior to the
formation of radial cracks.
Based on the mechanical properties of the reference materials along
with their corresponding crack dimensions (c, a and l), the empirical
constants in Anstis’s and Laugier’s equations can be calculated. In
Anstis’s equation, KIF (H/E)1/2 c3/2 is plotted against P and the slope of
this relationship is taken as the empirical constant χ. Likewise, in
Laugier’s equation, KIF (H/E)2/3 (l/a)1/2 c3/2 is plotted against P and the
corresponding slope is taken as the empirical constant χv. The fracture
toughness values used in these equations stem from well-accepted
conventional methods in literatures (values are given in Table 3)
[16,21–23]. The KIF (H/E)1/2 c3/2 – P and KIF (H/E)2/3 (l/a)1/2 c3/2 – P
relationships mentioned above are displayed in Fig. 4.
Overall, the data points of Si (100), Si (111), soda-lime glass, SiC
(0001) and sapphire exhibit an almost linear relationship with respect
to both equations. However, the data points of fused quartz do not fall
on this relationship. The reason for this, as mentioned before, pre-
sumably lies in fused quartz’s tendency to show cone cracks prior to
radial cracks, see Fig. 3. In Anstis’s research [4], a variety of materials
featuring a wide range of fracture toughness values were fitted together
to obtain a global constant. Therefore, using the same strategy and
fitting the reference materials used here as a whole dataset (except for
fused quartz), results in a global constant of ˜0.025. In comparison,
Cook got a value of 0.022 for a variety of ceramics and glasses exposed
to ambient air with a Vickers indenter [24,25] and Cuadrado obtained
0.026 ± 0.001 for Si (100), SiC (0001) and soda-lime glass with a
Berkovich indenter [16]; both findings are in good agreement with our
results. Similarly, fitting with Laugier’s equation will give a global
constant of ˜0.022, which is identical to the one presented by Cua-
drado’s [16]. Consequently, the results we’ve obtained so far for the
reference materials used here are in excellent agreement with existing
literatures.
Nevertheless, a closer look at the lower load regime reveals that, the
linear relationships actually differ for the various reference materials.
The latter implies that their crack behavior is best described by dif-
ferent empirical constants. The details of the KIF (H/E)1/2 c3/2 – P and
Y. Guo, et al.

Fig. 3. SEM images of the indent imprints on reference materials (a) Si (100), (b) Si (111), (c) soda-lime glass, (d) SiC (0001), (e) sapphire and (f) fused quartz.

Table 3
Calibration of the constants χ and χv in Anstis’s equation and Laugier’s equation for Berkovich indenter.
Material χ in Anstis’s equation KIF (H/E)1/2 c3/2 = χP χv in Laugier’s equation KIF (H/E)2/3 (l/a)1/2 c3/2 = χvP Fracture toughness used for equation fitting (GPa m1/
2
)

Si (100) 0.024 ± 0.001 0.015 ± 0.001 0.95

Si (111) 0.024 ± 0.001 0.016 ± 0.001 0.95
Soda-lime glass 0.025 ± 0.001 0.023 ± 0.001 0.7
SiC (0001) 0.037 ± 0.001 0.024 ± 0.001 3.4
Sapphire 0.032 ± 0.001 0.027 ± 0.001 2.4
Fused quartz 0.012 ± 0.001 0.006 ± 0.001 0.7
Y. Guo, et al.
Fig. 4. A Berkovich indenter is employed to induce cracks in six reference
materials at various maximum indentation load. (a) shows the KIF (H/E)1/2 c3/2
– P relationship for the calculation of χ in Anstis’s equation; (b) displays the
relationship of KIF (H/E)2/3 (l/a)1/2 c3/2 – P for the calculation of χv in Laugier’s
equation. Details of the data points at low load (highlighted in red) are pre-
sented in Fig. 5 and will be discussed in the text. (For interpretation of the
references to colour in this figure legend, the reader is referred to the web
version of this article.)
KIF (H/E)2/3 (l/a)1/2 c3/2 – P relationships at the lower load regime are
shown in Fig. 5. The large number of experimental data points allows
for a detailed insight into this phenomenon. At lower loading regime,
the linear relationships for Si (100) and Si (111) clearly differ from that
of SiC (0001); the latter shows a significantly steeper slope, i.e. em-
pirical constant. In order to get an overview of the differences in con-
stants received for the various reference materials, the numerical results
of the linear fitting of the individual materials are listed in Table 3.
Of all calculated constants of the reference materials, the constants of
fused quartz are significantly lower than the constants of the other mate-
rials in both fitting scenarios, which is in accordance with the experimental
results shown in Fig. 4. Hence, in later discussions, fused quartz will mostly
be excluded. Moreover, it is noticeable that Si (100) and Si (111) behave
almost identically in both scenarios. Although crystal anisotropy may result
in slight change in fracture toughness, it is confirmed that the discrepancy
is less significant when indenting (100) and (111) planes. [16,26] With
Anstis’s equation, a constant of 0.024 has been achieved for Si (100) and Si
(111), which is very close to the one reported by Pharr, 0.0237, in the
context of a study dedicated to the effect of the indenter angle on the
cracking of Si [27]. In the case of Laugier’s equation, Si (100) and Si (111)
result in constants of ˜0.015. The constant of soda-lime glass in Anstis’s case
Fig. 5. (a) KIF (H/E)1/2 c3/2 – P relationship for the calculation of χ in Anstis’s
equation; (b) KIF (H/E)2/3 (l/a)1/2 c3/2 – P relationship for the calculation of χv
in Laugier’s equation at lower loads corresponding to Fig. 4 (a) and (b), re-
spectively.
is 0.025 and barely varies when changing to Laugier’s equation. The reason
behind this lies in the l to a ratio range and will be discussed in detail in
Section 3.2. The constant of SiC (0001) is calculated to be 0.037 in Anstis’s
equation and 0.024 in Laugier’s equation. Finally, sapphire shows similar
numerical results to SiC (0001). Considering the non-ideal crack mor-
phology in real measurements and the different loading regimes applied to
initiate cracks for different reference materials, it is speculated that to some
extend sapphire’s crack behavior resembles the one shown by SiC (0001)
rather than that of Si or soda-lime glass.
At this point, we can summarize the findings presented so far as fol-
lows: In the first part of this section, the global empirical constants of
Anstis’s and Laugier’s equations have been calculated with a dataset
consisting of all reference materials (except for fused quartz). In the second
part, the individual constants are calculated for each reference material,
respectively. Subsequently, now the relationship between the global and
the individual constants needs to be examined from a pure mathematical
point of view. Mathematically, the global linear fitting (of the first part)
will try to match the data points of soda-lime glass in order to reduce the
associated R square (R2) because of the large maximum load it requires to
crack the glass. Thus, in the case of a linear fitting with Anstis’s equation,
the data points of SiC (0001) and sapphire play a minor role since their
indentation load range sufficient for cracking is significantly smaller
compared to the one necessary to crack the soda-lime glass. Consequently,
the global constant will always be close to the individual one of soda-lime
glass, Si (100) and Si (111). Furthermore, the fracture toughness of these
materials agrees well with the corresponding information gained by
Y. Guo, et al.

conventional methods. Moreover, there is no doubt that the fracture indenting low fracture toughness materials with a Vickers indenter
toughness of SiC and sapphire will be underestimated when calculated generally leads to the formation of a Half-penny crack whereas high
using this global constant. In the case of a linear fitting with Laugier’s fracture toughness materials show Palmqvist cracks [28]. Following
equation, the global constant will be close to the individual one of soda- this argument, the crack morphology might be the reason for the
lime glass, SiC (0001) and sapphire. Thus, the fracture toughness of these classification of reference materials and will be discussed in Section 3.3.
three reference materials agrees well with conventional results while the Based on the discussions above, the six reference materials studied
fracture toughness of Si (100) and Si (111) will be overestimated. Findings here can be classified into three groups: Group I: Si (100), Si (111),
like these of an underestimated fracture toughness for SiC or sapphire or soda-lime glass; Group II: SiC (0001), sapphire; Group III: fused quartz.
an overestimated fracture toughness for Si are often reported in literature
[4,16]. Therefore, the discussion presented above is helpful in order to
3.2. The investigation of other equations
resolve some of the irritations caused by under- or overestimated fracture
toughness values obtained for some reference materials under certain
In this section, the equations summarized in Ponton’s work [7] have
boundary conditions. Furthermore, it became obvious that the reference
been reexamined with respect to their empirical constants in order to
materials most widely used for fracture toughness evaluation based on
further test the validity of the classification idea. In all considerations,
radial cracks actually show quite a diverse behaviors. Hence, a possible
the value of the constants is calculated for the six reference materials
solution to solve the issues mentioned above could be to classify the re-
using the same procedure and strategy as described in Section 3.1. It is
ference materials into groups. In that case, a group would be composed of
noteworthy that, once the equations are investigated from the per-
materials featuring similar constants in the corresponding fracture
spective of the empirical constant, a substitution of Hv (load/real con-
toughness equation. For example, Si (100) and Si (111) belong to one
tact area) by H (load/projected contact area) does not result in any
group while SiC (0001) and sapphire are part of another group.
differences for some of the equations.
The exponential relationship between the maximum load P and total
In Ponton’s work, 19 equations based on different physical models
crack length c for reference materials is depicted in Fig. 6. It can be seen
are given. However, some equations actually feature the same expres-
that the general relationship P ∝ cn holds true for all reference mate-
sion and only differ in the value of the empirical constant. In such a
rials. The corresponding exponents are about 1.5, which represents the
case, we treat them as one equation here. The remaining 15 equations,
value typically taken for Half-penny cracks in most references. More-
which have been examined in this work, are listed in Table 4. Generally,
over, the data points of Si (100), Si (111) and soda-lime glass all fall on
Eq. B1 to Eq. B12 were originally derived for a Half-penny crack mode
one linear relationship, while the data points of SiC (0001), sapphire
and Eq. B13 to Eq. B15 were tailored for a Palmqvist crack mode. It is
and fused quartz exhibit another linear relationship, which is shifted
noteworthy that, unlike the equations in Ponton’s work, which are
slightly upwards. The reason behind this two linear relationship phe-
summarized in chronological order, the equations in our work are re-
nomenon can be the different fracture toughness regimes the reference
arranged reflecting on their complexity. Moreover, formal similarities
materials feature, since Si (100), Si (111) and soda-lime glass feature a
are considered and the corresponding equations are bundled to facil-
relatively low fracture toughness compared to SiC (0001) and sapphire.
itate further comparison. Eq. B4 and Eq. B15 represent Anstis’s and
Notably, fused quartz’s showing up as a high fracture material is ac-
Laugier’s equations, respectively.
tually an artifact when its fracture toughness is calculated from radial
The resulting constants (for each reference material) of the 15 dif-
cracks. In fused quartz, cone-cracks are produced prior to radial cracks.
ferent equations are listed in Table 5. The errors stated in this table
Here, subsequent to the occurrence of the first cone-crack, the forma-
arise from the accuracy of the measurements of elastic modulus,
tion of new cone-cracks and the propagation of radial cracks are sup-
hardness and crack lengths c, l and a.
posed to take place simultaneously while a major part of energy is
In summary, the constants of Si (100) and Si (111) are almost
dissipated through cone-cracks. Hence, any fracture toughness value of
identical for all equations. Moreover, considering any specific equation,
fused quartz solely based on radial crack length will be dramatically
the constants of Si (100) and Si (111) are always ˜1.5 times smaller than
overestimate its fracture toughness. Consequently, the exponential re-
those of SiC (0001), indicating that the fracture behavior of Si and SiC is
lationship between P and c provides another evidence of the necessity
different, regardless of the equation used. Consequently, it is advisable
to classify the existing reference materials. Dukino argued that
to never utilize Si and SiC as reference materials for constant calibration

Table 4
Fifteen equations arranged according to their formal similarities taken from
reference [7].
Equation expression Equation number

KIF = k1 P/c3/2 Eq. B1

KIF = k2 (E/H)1/4 P/c3/2 Eq. B2
KIF = k3 (E/H)2/5 P/c3/2 (c ≥ 2.5a) Eq. B3
KIF = k4 (E/H)1/2 P/c3/2 Eq. B4
KIF = k5 (E/H)2/3 P/c3/2 Eq. B5
KIF = k6 P/ac1/2 (c ≥ 2a) Eq. B6
KIF = k7 P/a3/2 log(4.5a/c) (0.6 ≤c/a＜4.5) Eq. B7
KIF = k8 P/a3/2 (E/H)2/5 log(8.4a/c) Eq. B8
KIF = k9 P/a3/2 (E/H)2/5 (a/c)1.56 Eq. B9
KIF = k10 P/a3/2 (E/H)2/5 10F Eq. B10*
KIF = k11 [f(E/H)] P/ac1/2 (c/a ≤ ≈ 2.8) Eq. B11#
KIF = k12 [f(E/H)] P/(a0.42c1.08) (c/a ≥ ≈ 2.8) Eq. B12#
KIF = k13 (E/H)2/5 P/ al1/2 (0.25 ≤ l/a ≤ 2.5 or 1 ≤ l/a ≤ Eq. B13
2.5)
KIF = k14 P/ al1/2 Eq. B14
Fig. 6. Exponential relationship between the maximum load P and total crack
KIF = k15 (E/H)2/3 (a/l)1/2 P/c3/2 Eq. B15
length c for the reference materials. Si (100): black dots; Si (111): green dots;
soda-lime glass: blue dots; SiC (0001): yellow dots; sapphire: purple dots; and * F = -1.59-0.34B-2.02B2+11.23B3-24.97B4+16.32B5, B = log(c/a).
fused quartz: orange dots. (For interpretation of the references to colour in this #
f(E/H) = 0.75*(βEXP2/δ – 1.5), δ = 2(1 + 3lnβEXP)/3, βEXP = 0.768(E/
figure legend, the reader is referred to the web version of this article.) H)0.408.
Y. Guo, et al.

Table 5
Resulting constants for a Berkovich indenter using the 15 different equations listed in Table 4.
Material Eq. B1 Eq. B2 Eq. B3 Eq. B4 Eq. B5 Eq. B6 Eq. B7 Eq. B8

Si (100) 0.092 ± 0.001 0.047 ± 0.001 0.031 ± 0.001 0.024 ± 0.001 0.015 ± 0.001 0.046 ± 0.001 0.092 ± 0.001 0.017 ± 0.001
Si (111) 0.093 ± 0.001 0.048 ± 0.001 0.032 ± 0.001 0.024 ± 0.001 0.016 ± 0.001 0.046 ± 0.001 0.092 ± 0.001 0.018 ± 0.001
Soda-lime glass 0.085 ± 0.002 0.046 ± 0.001 0.031 ± 0.001 0.025 ± 0.001 0.016 ± 0.001 0.028 ± 0.001 0.088 ± 0.005 0.013 ± 0.001
SiC (0001) 0.14 ± 0.01 0.071 ± 0.001 0.048 ± 0.001 0.037 ± 0.001 0.024 ± 0.001 0.067 ± 0.001 0.13 ± 0.01 0.027 ± 0.001
Sapphire 0.13 ± 0.01 0.064 ± 0.001 0.043 ± 0.001 0.032 ± 0.001 0.021 ± 0.001 0.047 ± 0.001 0.12 ± 0.01 0.020 ± 0.001
Fused quartz 0.035 ± 0.001 0.021 ± 0.001 0.015 ± 0.001 0.012 ± 0.001 0.009 ± 0.001 0.022 ± 0.001 0.038 ± 0.001 0.011 ± 0.001
Eq. B9 Eq. B10 Eq. B11 Eq. B12 Eq. B13 Eq. B14 Eq. B15
Si (100) 0.032 ± 0.001 0.59 ± 0.02 0.077 ± 0.003 0.12 ± 0.01 0.011 ± 0.001 0.034 ± 0.001 0.015 ± 0.001
Si (111) 0.033 ± 0.001 0.60 ± 0.03 0.080 ± 0.003 0.12 ± 0.01 0.012 ± 0.001 0.034 ± 0.001 0.016 ± 0.001
Soda-lime glass 0.034 ± 0.001 0.45 ± 0.02 0.068 ± 0.003 0.13 ± 0.01 0.008 ± 0.001 0.023 ± 0.001 0.023 ± 0.001
SiC (0001) 0.050 ± 0.001 0.90 ± 0.04 0.13 ± 0.01 0.20 ± 0.02 0.017 ± 0.001 0.048 ± 0.001 0.024 ± 0.001
Sapphire 0.045 ± 0.001 0.64 ± 0.07 0.081 ± 0.002 0.14 ± 0.01 0.013 ± 0.001 0.038 ± 0.001 0.027 ± 0.001
Fused quartz 0.016 ± 0.001 0.37 ± 0.03 0.12 ± 0.01 0.15 ± 0.01 0.006 ± 0.001 0.013 ± 0.001 0.006 ± 0.001

at the same time. This is also true for the case of soda-lime glass and
sapphire (the constants of soda-lime glass, in most cases, except for Eq.
B12 and Eq. B15, are ˜1.5 times smaller than those of sapphire).
A closer look at the individual expressions of the equations reveals
that Eq. B1 to Eq. B5 only contain the total crack length c, whereas, P/
c3/2 is a fixed term and the exponent in (E/H)n varies from 0 to 2/3.
Moreover, based on the values of the calculated constants presented in
Table 5, the classification proposed here still remains reasonable. For
Eq. B6 to Eq. B15, the crack length a or l is introduced, adding a higher
degree of complexity:
I) For some equations (Eq. B7, B9 and B12), Si (100), Si (111) and
soda-lime glass belong to the same group; while for other equations
(Eq. B6, B8, B10, B11, B13, B14 and B15), the constants indicate
that they should not be categorized into one group.
II) For some equations (Eq. B7, B9 and B15), SiC and sapphire belong to
the same group; while for others (Eq. B6, B8, B10, B11, B12, B13
and B14), the constants show that they probably should not be
considered as members of the same group.
To shed some light on this phenomenon, subsequently, Eq. B6 to Eq.
B15 will be rewritten into a new form. Since c = a + l, assuming
c/a = m,
then a and l are,
a = c/m
and
l = (m-1)/m·c,
respectively.
Inserting Eqs. 4 and 5 into Eq. B6 to Eq. B15 (replacing a and l with c
and m) results in a new form of Eq. B6 to Eq. B15, which is composed of
two parts. One part is identical to Eq. B1 to Eq. B5, which, as has al-
ready been shown, follows our idea of classification. The second part is
a function of m as can be seen in Table 6, which, as will be shown later
on, is the actual reason behind some of the irritations stated above
concerning classification.
All equations that have been proposed earlier based on various
physical theories or models can be written into a universal form as
shown in Eq. 6, where k is the empirical constant. E, H, Pmax and c are
elastic modulus, hardness, maximum indentation load and total crack
length at the maximum indentation load, respectively. f(m) is a function
of m, or c to a ratio.
Kifr = k (E/H)n Pmax/c3/2 f(m) (6)
If f(m) is taken as unity in Eq. 6, Kifr = k (E/H) P/c n 3/2
can be
regarded as a universal form representing Eq. B1 to Eq. B5.
Accordingly, the calculated constants should meet the classification
Group I: Si (100), Si (111), soda-lime glass; Group II: SiC, sapphire and
Group III: fused quartz, which can also be confirmed by observing
Table 5. However, when f(m) is considered in the formulation, it seems
that the classification changes according to the values of the calculated
constants. Regardless of any physical implications behind these equa-
tions, mathematically, this change is mainly due to the different re-
gimes of f(m) associated with the different reference materials. To
(3)
clarify the effect of different regimes, Fig. 7 displays a plot of f(m) for
the various equations. In our case, the m value (c/a ratio) of Si (100), Si
(111) and SiC (0001) is in the same range ranging from 1.4 to 2.0
(4)
(grey), since the total crack length c increases more rapidly than a with
increasing maximum load. For sapphire, m falls in the range from 2.0 to
2.5 (orange), while m shows values ranging from 2.4 to 2.8 (light blue)
(5) for soda-lime glass. Moreover, at different m regimes, f(m) is also a
constant that will have an effect on the value of the empirical constant
k.
Generally, an increase in f(m) in Kifr = k (E/H)n P/c3/2 f(m) will

Table 6
The new form of Eq. B6 to Eq. B15, rewritten with c and m.
Equation number Equation expression

Eq. B6 KIF = k6 P/ac1/2 = k6 P/c3/2 m = (Eq. B1)·m

Eq. B7 KIF = k7 P/a3/2 log (4.5a/c) = k7 P/c3/2 m3/2 log(4.5/m) = (Eq. B1)·m3/2 log(4.5/m)
Eq. B8 KIF = k8 P/a3/2 (E/H)2/5 log(8.4a/c) = k8 P/c3/2 (E/H)2/5 m3/2 log(8.4/m) = (Eq. B3)·m3/2 log(8.4/m)
Eq. B9 KIF = k9 P/a3/2 (E/H)2/5 (a/c)1.56 = k9 P/c3/2 (E/H)2/5 m−0.06 = (Eq. B3)·m−0.06
Eq. B10* KIF = k10 P/a3/2 (E/H)2/5 10F = k10 P/c3/2 (E/H)2/5 m3/2 10F = (Eq. B3)·m3/2 10F
Eq. B11# KIF = k11 [f(E/H)] P/ac1/2 = k11 P/c3/2 [f(E/H)] m = (Eq. B1)·[f(E/H)] m
Eq. B12# KIF = k12 [f(E/H)] P/(a0.42c1.08) = k12 P/c3/2 [f(E/H)] m0.42 = (Eq. B1)·[f(E/H)] m0.42
Eq. B13 KIF = k13 (E/H)2/5 P/ al1/2 = k13 (E/H)2/5 P/c3/2 m3/2/(m-1)1/2 = (Eq. B3)·m3/2/(m-1)1/2
Eq. B14 KIF = k14 P/ al1/2 = k14 P/c3/2 m3/2/(m-1)1/2 = (Eq. B1)·m3/2/(m-1)1/2
Eq. B15 KIF = k15 (E/H)2/3 (a/l)1/2 P/c3/2 = k15 (E/H)2/3 P/c3/2 (m-1)−1/2 = (Eq. B5)·(m-1)−1/2

* F = -1.59-0.34B-2.02B2+11.23B3-24.97B4+16.32B5, B = log(c/a).
#
f(E/H) = 0.75*(βEXP2/δ – 1.5), δ = 2(1 + 3lnβEXP)/3, βEXP = 0.768(E/H)0.408.
Y. Guo, et al.

Fig. 7. Graphical representation of the second part (the function of m) in Eq. B6 to Eq. B15 after replacing a and l with c and m. m ranges from 1.4 to 2.0 for Si (100),
Si (111) and SiC (0001) (grey); from 2.0 to 2.5 for sapphire (orange) and from 2.4 to 2.8 for soda-lime glass (light blue). (For interpretation of the references to colour
in this figure legend, the reader is referred to the web version of this article.)
Y. Guo, et al.
lead to a decrease in k and vice versa. Furthermore, the following ex-
planations can be derived when taking the addition of f(m) in Eq. B6 to
Eq. B15 into consideration.
I) The m regimes for Si (100), Si (111) and SiC (0001) are identical
(from 1.4 to 2.0), thus the finding that the constants for SiC (0001)
are always 1.5 times larger than the ones for Si (100) and Si (111) is
unaffected by f(m).
II) In Eq. B7 and Eq. B9, despite the fact that the m regime varies for
the different reference materials, f(m) remains almost unchanged.
Thus, for these equations, the calculated constants are or rather the
classification of reference materials is hardly affected by the term f
(m). The classification of the reference materials according to the
constants values using Eq. B7 and Eq. B9 is very close to the clas-
sification, which results from using Eq. B1 to Eq. B5.
III) In other equations (Eq. B6, B8, B10, B11, B12, B13, B14 and B15), f
(m)soda-lime glass is approximately 1.5 times larger than f(m)Si (100)
and f(m)Si (111). Therefore, in such cases, the empirical constant
calculated for soda-lime glass will be ˜1.5 times smaller than the
one of Si (100) and Si (111). This statement is also applicable to the
case of sapphire and SiC.
IV) It should be noted that the term [f(E/H)] in Eq. B11 and Eq. B12 is a
material dependent constant, which further adds to the complexity
in the calculation of the empirical constants k in those equations.
However, the change of the calculated constants due to term [f(E/
H)] still obeys a similar interrelationship as described above for f
(m) and k, that an increase in [f(E/H)] will lead to the decrease of k,
and vice versa.
Consequently, the classification of the six reference materials in-
vestigated in this work has again been recognized/verified: Group I: Si
(100), Si (111), soda-lime glass; Group II: SiC, sapphire; Group III: fused
quartz. If the materials within one group are chosen as reference ma-
terials, all equations should give similar results. Moreover, according to
our discussion, the underestimation/overestimation of fracture tough-
ness values and the non-universal applicability property of the fracture
toughness equations are both owing to the inappropriate choice of re-
ference materials.
Although the classification of the reference materials can explain
many unanswered questions, the scientific reason behind such a clas-
sification remains unclear. It is strongly believed that the morphology
of the indentation induced cracks can always be identified as Half-
penny or Palmqvist type. [12] Furthermore, Dukino reports, that in-
denting materials featuring a low fracture toughness with a Vickers
indenter generally leads to the formation of a Half-penny crack whereas
materials with a high fracture toughness typically show Palmqvist
cracks [28]. Therefore, the actual crack morphology of the reference
materials might be the reason behind the classification. Consequently, it
is necessary to take a closer look at the crack morphology formed
within the individual reference materials.
3.3. The investigation of crack morphology
Within this chapter, the crack morphology of the reference materials
is investigated to further work on a scientifically meaningful basis of the
classification concept. However, the difference in crack morphology
(Half-penny or Palmqvist crack) within the six reference materials
cannot be distinguished by top-view SEM images. Thereby, for the
purpose of crack morphology investigation, FIB-cutting has been em-
ployed to obtain several cross-sections along the cracks. It is also no-
teworthy that the core discussion of this chapter is about Half-penny
and Palmqvist cracks, whereas cone cracks, as in the case of fused
quartz, cannot be handled with existing fracture toughness equations.
Therefore, for the sake of simplification, in this chapter we only focus
on the first two groups and discard the third group (fused quartz). One
reference material from each group was chosen to perform the FIB
experiments. In the first group, Si (100) was chosen, while in the second
group, SiC (0001) was selected. Fig. 8 illustrates the experimental and
analytical procedure, including examples of images taken from the top
view and cross-sectional view of some cracks.
In this context, Fig. 8(a) gives a schematic, introducing the para-
meters that are measured after one cross-section is created. Fig. 8(b)
and (e) are SEM images of the untreated cracks of Si (100) and SiC
(0001), respectively. The crack in Si (100) was created at an indenta-
tion displacement of 680 nm and features a total crack length of 4.3 μm.
The one on SiC (0001) was created at an indentation depth of 650 nm
and its total crack length is about 4.4 μm. Fig. 8(c) and (f) show the
cross-sections of Si (100) and SiC (0001) after a clean cut, while
Fig. 8(d) and (g) display the corresponding surface views after the cut,
respectively. The length measured from the center of the indentation
impression to the cross-sections ds as well as the crack length on the
corresponding cross-section dcs are evaluated by SEM observation and
recorded. It should be noted that there can be a so called curtaining
effect [29] on the cross-sections as marked by the red arrows in Fig. 8(c)
and (d). In the case of Si (100), the crack is easily distinguishable from
the curtaining effect. However, when the curtaining effect is in line
with the crack, as in SiC (0001), it will add some difficulties with re-
spect to the accurate estimation of the crack length. To tackle with this
situation, images taken at higher magnification and higher contrast are
required. Subsequently, several cross-sections are created along a crack
– i.e. along the direction towards the center of the indentation induced
imprint. The lengths of ds and dcs are recorded for each cross-section,
respectively. Finally, based on the obtained information, the crack
morphology within Si (100) and SiC (0001) can be reconstructed as
shown in Fig. 9.
The colored regions in Fig. 9(a) and (b) correspond to the crack
morphology in Si (100) and SiC (0001), respectively. The plots them-
selves are based on the measured crack lengths on several cross-sections
and the positions of the corresponding cross-sections. In general, the
crack morphology in Si (100) and SiC (0001) are significantly different
with respect to each other and, in particular, are neither ideal Half-
penny nor Palmqvist type in shape. The crack in Si (100) features an
almost Half-penny shaped morphology and the deepest part of the crack
is situated at the center of the crack itself. Moreover, the ratio of crack
length on the surface to crack depth is ˜1.5 for Si (100). The crack
morphology in SiC (0001) approximately resembles a rectangle with
the deepest part of the crack situated directly at the center of the indent
induced impression. Besides, there is quite a large, non-negligible re-
gion around the indenter free of any cracks in SiC (0001) as seen in
Fig. 9(b), which implies that the cracks start somewhere below the
indent impression. Such a median crack starts possibly at the stress
concentration sites featured by shear fault intersections [30], definitely
relying on a completely different mechanism compared to the one ob-
served for Si (100).
In summary, the crack morphology in Si (100) and SiC (0001) dif-
fers in shape. This finding could account for the necessary classification
of the reference materials. Based on these results, we propose an im-
proved procedure to determine fracture toughness from radial cracks
induced by nanoindentation, which will be introduced in the next
chapter.
3.4. An improved procedure to determine fracture toughness from radial
cracks by nanoindentation
The previous chapters highlighted the role of the choice of reference
materials in the context of fracture toughness evaluation by means of
Y. Guo, et al.

Fig. 8. (a) Schematic of a cross-section along the indent-induced crack; SEM images of the untreated crack of (b) Si (100) and (e) SiC (0001); the cross-sections of (c)
Si (100) and (f) SiC (0001); top view SEM images of (d) Si (100) and (g) SiC (0001) corresponding to (c) and (f).
Y. Guo, et al.

Fig. 9. Crack morphology in (a) Si (100) and (b) SiC (0001) reconstructed ac-
cording to the measured crack lengths on the cross-sections and the positions of
the corresponding cross-sections.

the analysis of radial cracks induced by nanoindentation. Therefore, in

order to achieve a more reliable fracture toughness determination of
unknown materials, the following procedure is proposed:

1 Create indentation induced cracks into the preferably polished sur-

face of the unknown materials utilizing sharp indenters such as
Vickers, Berkovich, Cube corner, etc. Subsequently, identify the
crack morphology with the help of FIB tomography.
2 Create cracks in some candidate materials whose hardness, elastic
modulus and fracture toughness are already known, check the cor-
responding crack morphology and calculate the associated constants
of one or more preferred equations. It is noteworthy that the crack
morphology is generally believed to be related to the mechanical
properties of the material being indented as well as the geometry of
the indenter utilized to create the crack. Sometimes the degree of tip
rounding of the indenter might also affect the final crack mor-
phology, thus leading to slightly different constants. Even though
this step might be time consuming, it is recommended in order to
have a general view of the status of the experimental setup. In some
specific cases it might even be inevitable.
Fig. 10. (a) SEM image of the untreated crack of a nanostructured diamond/SiC
composite film; (b) SEM micrographs showing the cross-section and (c) surface
of the corresponding film after one cross-section is created by FIB.
3 Candidate materials with similar crack morphology and corre-
sponding calculated constants can serve as reference materials to
derive constants using one or more equations.
4 Calculate the fracture toughness of the unknown material using a
specific equation and the calculated constant (step 3) for this spe-
cific equation.
Y. Guo, et al.
Fig. 11. Crack morphology of the nanostructured diamond/SiC composite film.
In summary, the examination of crack morphology and an appro-
priate choice of reference materials are essential in order to achieve a
scientifically meaningful and reproducible fracture toughness evalua-
tion of any unknown material.
3.5. The fracture toughness of diamond/SiC composite films
After we established the procedure to determine fracture toughness
based on nanoindentation-induced radial cracks, the fracture toughness
of a 13 μm thick diamond/SiC composite film is investigated. Fig. 10
provides top view as well as cross sectional images of the cracked re-
gion of this film. In this case, the bright regions are associated with the
diamond phase while the dark regions represent SiC. Please find the
details about sample preparation elsewhere. [19]
Initially, the cracks are generated with a high load Berkovich in-
denter. Subsequently the crack morphology is examined. An example
for the latter is shown in Fig. 10. In Fig. 10(a), an untreated crack,
produced at an indentation depth of 1600 nm, is imaged on the sample
surface. It features a crack length of ˜8.1 μm. Consequently, several
cross-sections are created along this crack. It should be pointed out that,
the columnar structures, which can be observed on the cross-sections,
are a typical phenomenon observed for a composite material featuring
components with different properties that is etched by an ion beam. To
reconstruct the crack morphology, dcs and ds are measured in the na-
nostructured diamond/SiC composite film. The latter is visualized in
Fig. 11. The crack morphology of the nanostructured diamond/SiC
composite film is analogous to that of Si (100). Moreover, its ratio of
crack length on the surface to crack depth is very close to the Si (100)
ratio calculated before. Consequently, according to our strategy in-
troduced above, Si (100), Si (111) and soda-lime glass should be used as
reference materials to derive the constants in the context of the de-
termination of the fracture toughness of this film material rather than
SiC or sapphire.
All discussions so far are applicable to bulk materials. However, for
film systems, the problem of residual stresses needs to be taken into
consideration when calculating their fracture toughness. In order to
account for any pre-existing or residual stress in the film (the influence
of substrate), an additional part has been added to Anstis’s equation as
in Eq. 7. [31–33]
Kifr = χ (E/H)1/2 Pmax c−3/2 + 2mσ (c/π)1/2 (7)
where m is a dimensionless modification factor and σ is the residual
stress in the film. Therefore, we will use Eq. 7 to calculate the fracture
toughness of our composite film. Eq. 7 can be rewritten as
Fig. 12. The Pmax c−3/2 – c1/2 relationships for the nanostructured diamond/SiC
composite film analyzed within this study.
Pmax c−3/2 = (1/χ) (H/E)1/2 Kifr – 2mσ (1/χ) (H/E)1/2 π-1/2 c1/2 (8)
Kifr = B·χ (E/H) 1/2
(9)
−3/2 1/2
where B is the intercept of the linear fitting of Pmax c – c re-
lationship. The fracture toughness of the composite film can now be
calculated as suggested by Eq. 9. Nevertheless, one important issue still
remains open: Whether the constant derived using Anstis’s equation can
directly be transferred to Eq. 7 or not. This issue needs to be addressed
prior to any fracture toughness calculation of the film system.
In order to do so, the materials of group one, Si (100), Si (111) and
soda-lime glass, are used as reference materials to derive the corre-
sponding constant of Eq. 7 anew. The relationship of Pmax c−3/2 – c1/2 is
plotted for all three materials. In this context, the slope of the fitting
curve is forced to be zero under the assumption that the residual stress
in the reference materials is almost zero (σ ≈ 0). Consequently, the
empirical constant χ obtained from the three reference materials is
˜0.024, identical with the value gained from Anstis’s equation (Eq. 1).
Therefore, any constant derived from Anstis’s equation is valid for Eq. 7
too and a constant of 0.024 is used for the calculation of fracture
toughness of the structured diamond/SiC composite film. The corre-
sponding relationship of Pmax c−3/2 – c1/2 for the nanostructured dia-
mond/SiC composite film is shown in Fig. 12.
In this figure, it is possible to observe that the data points actually
fall into two linear regimes. Here, the absolute value of the slope of the
second regime is smaller compared to the first one. The reason for this
phenomenon can be explained by crack propagation within the com-
posite film. Initially, one crack is produced at a specific load and the
crack morphology is close to the one shown in Fig. 10. Subsequently,
the crack starts to propagate within the composite film and its mor-
phology remains unchanged until the crack approaches the film/sub-
strate interface. Once the crack is close to/in touch with the substrate,
the crack behavior (crack morphology and radial crack length on the
surface) is influence by the Si substrate. Moreover, fracture toughness
determined based on the second regime is smaller compared to the one
obtained in the first one as the second one already is affected by the Si
substrate, who features a relative low fracture toughness.
Therefore, in order to avoid any substrate effect, only the data
points whose corresponding crack depth lies within the thickness of the
film, are used for and the calculation of fracture toughness. In this
context, it is possible to estimate the depth of the cracks dividing the
crack length observed on the surface by 1.5. The intercept received for a
linear fit of the Pmax c−3/2 – c1/2 relationship (data points in regime 1 is
(1.34 ± 0.09) x 108 and the corresponding fracture toughness of the
diamond/SiC composite film is calculated to be 11.1 ± 1.1 MPa·m1/2.
Y. Guo, et al.
The hardness and elastic modulus of the composite film used are
49.8 ± 2.1 GPa and 598 ± 7 GPa, respectively. For details, please
refer to our previous work [19]. The error in the result stems from
uncertainties in the linear fitting procedure as well as in the experi-
mental hardness and modulus data.
In literatures, the fracture toughness of diamond/SiC composite
material – synthesized by reactive sintering under high pressure and
high temperature conditions or sintered by a high pressure infiltration
technique are comparable to our results [34,35]. However, in those
references, fracture toughness is calculated based on the length of radial
cracks utilizing certain equations to obtain fracture toughness. How-
ever, since all potential drawbacks of the classical approach we dis-
cussed above have not been considered in the process of achieving the
values, a direct comparison of the values reported there and the ones
obtained in our study has to be handled with care. Nevertheless, we are
able to support the finding of an enhanced fracture toughness of the
diamond/SiC composite film, as has already been reported for bulk
diamond/SiC composites [34,35].
4. Conclusion
In this work, a thorough examination of the existing fracture
toughness equations has been carried out utilizing six common re-
ference materials (Si (100), Si (111), soda-lime glass, SiC (0001), sap-
phire and fused quartz). The choice of appropriate reference materials
was identified as crucial key to obtain scientifically meaningful and
reproducible results. Furthermore, the classification of the reference
materials into three groups is proposed: Group I: Si (100), Si (111) and
soda-lime glass; Group II: SiC and sapphire; Group III: fused quartz. A
Focus ion beam study proved that the basis of this classification could
be related to the actual crack morphology – Si (100) in Group I features
an almost Half-penny shaped morphology while the cracks in SiC
(0001) in Group II display nearly a rectangle type of morphology. The
actual crack morphology of the reference materials differs strongly from
the ideal Half-penny or Palmqvist assumptions made by the corre-
sponding models. Moreover, all equations typically utilized in the
context of fracture toughness evaluation have been shown to yield
equally valid results as long as appropriate reference materials are
chosen. Based on these results, an improved procedure to determine
fracture toughness has been proposed. Nevertheless, it should be
pointed out that this improved procedure proposed in this work is for
better accuracy in fracture toughness measurements by nanoindenta-
tion and is valid only under specific background researches (e.g. ex-
tensive study of the crack behavior and crack morphology of a variety
of reference materials). Moreover, none of the existing equations is
recommended for better universality. Finally, with the help of this
improved method, the fracture toughness of a diamond/SiC composite
film has been successfully estimated and an enhanced fracture tough-
ness of 11.1 ± 1.1 MPa·m1/2 was observed for this film material.
Aside from an improved procedure to estimate fracture toughness
with increased accuracy, the importance of this work also lies in its
capability to answer some of today’s open questions in indentation
based fracture toughness analysis. Here it was possible to show that the
reason for the issue of the nonexistence of a universal equation to
calculate fracture toughness as well as issues occurring in context of
under- or overestimated fracture toughness values could be tracked
back to an inappropriate choice of reference materials. Consequently,
this work represents new promising guidelines/criterions to re-
producibly determine fracture toughness based on indentation induced
radial cracks.
Declaration of Competing Interest
The Authors claim non-conflicts of interests.
We declare that we have no financial and personal relationships
with other people or organizations that can inappropriately influence
our work, there is no professional or other personal interest of any
nature or kind in any product, service and/or company that could be
construed as influencing the position presented in, or the review of, the
manuscript entitled “A detailed analysis of the determination of frac-
ture toughness by nanoindentation induced radial cracks”.
Acknowledgements
Yuning Guo gratefully acknowledges the financial support from the
China Scholarship Council (Chinese Government Scholarship, Award
No. 201504910733). Part of this work was performed at the Micro- and
Nanoanalytics Facility (MNaF) of the University of Siegen.
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