Micro-And Nanoindentation Techniques For Mechanical Characterisation of Materials

Micro- and nanoindentation techniques for
mechanical characterisation of materials

N. K. Mukhopadhyay*1 and P. Paufler2
Indentation techniques have been extensively used for mechanical characterisation of materials.
Development of instrumented indentation techniques at low and ultra low load levels has further
improved their utility for understanding the mechanical responses of solids at micro and nano
scales. The variation of hardness with the load/depth of indentation, known as indentation size
effect, has led to difficulties in using hardness as a fundamental or characteristic mechanical
property of materials. Detailed discussions are focused on the issue of indentation size effect in
brittle and ductile solids. Various theoretical models accounting for the indentation mechanics are
Published by Maney Publishing (c) IOM Communications Ltd
highlighted. The results obtained from these techniques with quasicrystals, bulk metallic glasses
and nanomaterials are reviewed. The issues related to phase transformation during indentation
tests are briefly discussed. The industrial use of the indentation technique has been pointed out.
Some of the current issues and directions for future research in this field are mentioned.
Keywords: Microindentation, Nanoindentation, Indentation mechanics, Hardness, Indentation size effect
Historical development of the concept of study. Apart from Aristotle’s general statement men-
tioned above, at the end of the 17th century, people were
hardness already aware of the varying resistance of minerals and
There have been various approaches to the concept other materials against mechanical loading, in particular
of hardness. It was Aristotle (384–322 BC; Bekker, against scratching. Huygens (1690) noticed the fascinating
1829), who called something ‘hard’ if the surface did fact that the cleavage plane of calcite may be scratched
not move under external pressure. When subdividing when moving the knife forward and may not when
hardness tests into cutting and non-cutting methods moving it in the opposite direction. Réaumur (1722)
of deformation, early attempts belong to the former. differentiated the quality of steel using a bar with
Cutting of the material was mainly the consequence of increasing hardness from one end to the other. The degree
scratching the specimen by needles or corners of certain of hardness was attributed to the specimen according to
reference materials. Non-cutting methods use an inden- the position on the bar which the specimen could scratch
tation perpendicular to the surface of the specimen by an first. Linné (1768, 1793) listed a number of terms relevant
indenter fixed to a load cell or by a bullet of known for an appropriate terminology of the mechanics of solids
momentum. It is not surprising that hardness values which has been adopted by other writers. Werner (1774)
derived from these methods, either relative or absolute, introduced four categories of hardness (hard, semihard,
did not agree satisfactorily, because of the different soft, very soft) defined by the behaviour of the material
physical processes involved in testing. Much work has when scratched by a knife or a file using gauge minerals
been done in the past to understand these processes at for comparison. Then Haüy (1801) classified minerals
a microscopic scale, to make hardness values more according to their ability to scratch each other, assigning
comparable and to find a hardness concept which four grades to the materials scratching quartz, glass or
genuinely reflects a material’s property (Turner, 1886; calcite and those not scratching calcite, respectively. Mohs
Pöschl, 1909; Tertsch, 1949; Tabor, 1951; Mott, 1956; (1812) proposed to use hardness (combined with several
Glazov and Vigdorovič, 1962, 1971; Juškin, 1971; Petty, other properties) as a distinguishing feature of solids.
1971; Grigorovič, 1976; Fischer-Cripps, 2004). Later on, on the basis of the definition of hardness, he
To recognise hardness as a quantity characteristic of a introduced a ten-stage hardness scale (now named after
material and to use it for analysis, several stages had to be him) and instructions for its realisation (Mohs, 1822). The
passed through. Some are just mentioned in the present anisotropy of the depths of scratches along different
directions in a plane as well as on crystallographically
different planes at constant load was measured thor-
1
Centre of Advanced Studies, Department of Metallurgical Engineering, oughly by Frankenheim (1829, 1831). Performing
Institute of Technology, Banaras Hindu University, Varanasi 221 005, India
2
Institute for Structural Physics, Dresden University of Technology,
scratches by hand, he noticed that features of the scratch
D-01062 Dresden, Germany also depend on the topology of the contact and on the
*Corresponding author, email mukho@bhu.ac.in or mukho_nk@rediffmail. speed of scratching. Thus, he recommended using relative
com measures of scratching hardness.
ß 2006 Institute of Materials, Minerals and Mining and ASM International

Published by Maney for the Institute and ASM International
DOI 10.1179/174328006X102475 International Materials Reviews 2006 VOL 51 NO 4 209
Mukhopadhyay and Paufler Micro- and nanoindentation techniques for mechanical characterisation
So far, the force applied was either not determined at on, von Engelhardt and Haussühl (1960) showed that
all or defined only qualitatively. It was Seebeck (1833) resistance against grinding varies rather with the specific
who built an instrument enabling well defined loads to free surface/interface energy.
be applied. Hardness was taken proportional to the Coming back to non-cutting methods, an early attempt
minimum load applied perpendicular to the surface, is mentioned first to find numerical values for the relative
which gave just a noticeable scratch when the surface hardness of metals due to officers of the US Ordnance
was shifted laterally. Franz (1850) introduced a similar Department who in 1856 pressed a pyramid on the metal
method independently of Seebeck, enabling the indenter under test recording the volume of the indent and using
to be moved across the fixed crystal. The methods of bronze as a standard (Turner, 1886). Then Calvert and
scratching were subsequently made on a more quanti- Johnson (1859) applied a steel cone to penetrate the
tative basis by evaluating the scratch geometry. Using material under investigation until a predetermined
essentially Seebeck’s device, Grailich and Pekárek (1854) indentation depth was achieved. The load necessary was
improved the mechanical parts and the optical inspec- used as a measure of hardness relative to the value of pig
tion of the scratches. They called their instrument a iron. The subsequent development of indentation hard-
sclerometer and, in doing so, launched the branch of ness testing methods was mostly stimulated by the rapidly
sclerometry (e.g. Sklerometrija, 1968). With the aid of growing demand of metallurgy.
this instrument, Exner (1873) supplied data on the A milestone towards a quantitative concept of
anisotropy of hardness in great detail. Sometimes hardness was the approach published by Hertz (1882),
alternative definitions were applied, as, for example, who defined the indentation hardness of solids as
hardness being inversely proportional to the lateral force contact pressure in a small circular area at the elasticity
which is needed to move the specimen under a given limit. This definition was applied to brittle as well as to
normal load (Franz, 1850; Grailich and Pekárek, 1854). ductile solids. However, experimental verification latter
In any case, hardness values obtained this way were proved difficult, whereas the elasticity limit of brittle
rather upper limits of this entity, because they were solids could be determined from the pressure at the onset
taken from the minimum load giving rise to a visible of cracking. This was the advent of contact mechanics,
scratch. The visibility, however, strongly depends on the an important tool of present-day hardness testing (cf.,
surface state of the specimen and/or the optical method e.g. Johnson, 1996). In order to take the onset of plastic
of recording the scratch. To reduce this uncertainty, deformation explicitly into account, Prandtl (1920,
Pöschl (1909) proposed to measure the change of the 1921) introduced as decisive criterion, the critical shear
scratch width versus the change of load instead of the stress as the difference of two principal stresses under
width itself. Martens (1898) introduced a scratch the indenter using a proposal made by von Mises (1913).
hardness tester which has been widely used by mechan- On the basis of Hertz’s definition, Auerbach (1890,
ical engineers, to measure the scratch width and the 1891) determined the hardness of brittle solids by
normal load. He took as hardness the normal load optically in situ monitoring the nucleation of cracks
which caused a given scratch width. Recent work on under load in glasses and crystalline quartz. He
nanoscratching shows a proportionality between lateral recognised that the hardness defined by the first
force and (normal force)3/2 for a number of materials appearance of a crack was subject to variation with
(Kaupp and Naimi-Jamal, 2004). Further development the curvature of the indenter. Since cracks opened under
of this idea will not be followed here because it leads to tensile stress, he concluded that the surface condition
the concept of wear, which is not in the focus of the might also have influenced crack nucleation. Extending
present review. the in situ measurements to ductile transparent solids
In addition to scratching, which is still used today to such as rock salt, calcite, fluorite and others, Auerbach
study wear resistance, other approaches to hardness (1892, 1896) proposed that hardness be taken as Hertz’s
assessment in the 19th century should be mentioned pressure at the onset of plastic flow indicated by an
briefly. Examples are planing, drilling, and grinding. almost constant contact pressure. When applying to
Planing was put forward by Pfaff (1883) who improved (opaque) metals, the area of contact was determined
the accuracy of measuring the depth of a scratch by employing a blackened indenter (Auerbach, 1900).
repeating the procedure n times along the same scratch Using loads below 2 N, hardness was termed micro-
and, moreover, employing several diamonds side-by-side hardness, though the distinction between macro- and
at the same time. Knowing the mass density of the microhardness is rather arbitrary. Nevertheless, a micro-
specimen and the area scanned, the scratch depth could hardness tester looked different mainly because of the
be calculated from the weight loss after planing. Relative higher optical resolution required. Various devices have
hardness values of various minerals or various planes been developed. Lips and Sack (1936) and Lips (1937)
and directions of the same mineral were then obtained introduced a small attachment to the light microscope
from the proportion of inverse planing depths, keeping which enabled indentations into small grains of multi-
parameters such as load and speed to be constant. phase alloys to be made by moving the specimen
Drilling with the aid of a cleaved diamond tetrahedron towards a Vickers diamond pyramid coupled to a
has been recommended for hardness measurement by spring. In the Vickers indenter, the angle between
Pfaff (1884) and Jaggar (1898), taking for hardness the opposite faces is 136u. This angle results from the
number of rotations needed to penetrate the surface to a condition that, from the tangents drawn from the points
given depth. When grinding with a standardised powder, of contact of an impression of diameter 0.375D (where D
hardness had been taken proportional to the time is the ball diameter as used in the Brinell test) to the
needed for the removal of a certain layer or inversely circumference of the indent, the included angle be 136u.
proportional to the loss of volume during grinding Smith and Sandland (1925) found that the hardness
(Jannettaz and Goldberg, 1895; Rosiwal, 1896). Later values obtained with the Vickers indenter of that angle
210 International Materials Reviews 2006 VOL 51 NO 4

and with the Brinell ball are nearly equal, when the load Brinell, 1900), other shapes had been found useful
has been adjusted to produce a Brinell impression of the for various purposes, such as cones (Ludwik, 1908;
diameter 0.375D, which is considered the ideal impres- Rockwell, 1922), double cones (Grodzinski, 1951),
sion diameter halfway between 0.25D and 0.5D. Unlike trigonal prisms (Attinger, 1947) or pyramids (tetragonal:
other test methods, Vickers hardness is named after the Smith and Sandland, 1925; orthorhombic: Knoop et al.,
company Vickers Ltd, which designed the first hardness 1939; trigonal: Berkovič, 1951). It was already noticed
testing machine with this indenter. After replacing this by Auerbach (1891), that the exact shape of the indenter
microhardness tester by the objective of the microscope, must have an impact upon the hardness value. The
the diameter of the indents (of the order of 10 mm) could shape of the indents as well as the relation between
be measured (for Russian devices, cf. Glazov and hardness values and indentation geometry is displayed in
Vigdorovič, 1962, 1971). While in a conventional micro- Table 1.
or macrohardness test, penetration depths h of the order This brings us to the evaluation of indentation
of 101–103 mm and forces F in the range 1022–102 N hardness H as it is used today. Let an indenter under
occur, in a nanohardness test, both h and F are load F penetrate the surface of a solid so that the contact
significantly smaller (F,10 mN, h,10 mm) and – in area between indenter and surface is A. Then the
this case compulsory – the dependence F(h) is recorded hardness H of the solid can be defined as the ratio
throughout the loading–deloading cycle. (cf. Fischer-
Cripps, 2004). force F (perpendicular to the surface)
H~ (1)
Indentation methods experienced another diversifica- contact area A
tion. Starting with spherical indenters (Hertz, 1882; If A is taken as the curved area of the indent, H depends
Table 1 Geometrical shape of indenter and projected indentation along with hardness equation and penetration depths
displayed for various indenters
Testing Shape of Shape of impression

method indenter protection Hardness value Penetration depth
Brinell He ~ 2F
1=2
t5D{1–[1–(d/D)2]1/2}<d2/2D
pD 2 1{½1{(d=D)2
Brinell hardness number BHN;
[F]5kg; [D], [d]5mm
Vickers 2F sin 680 1:8544F t<d/7

HV ~ ~
d2 d2
Vickers hardness number VHN;
½F~kg, ½d~mm
Knoop F 14:40F t<d/30.6

HK ~ ~
A d2
Knoop hardness number KHN;
½F~kg, ½d~mm
Ludwik 4F sin450 0:9F t5d/2

HL ~ ~ 2
pd 2 d
Grodzinski 6rF 0:9F t<d/80 for a5154u, r52 mm

HG ~F =At ~ ~
pd 2 tan(a=2)d 3
Double cone number a~1540 r~2 mm
2:77F 6
HGN~ 10
d3
½D~mm, a~1540 , ½F~kg
pffiffiffi
Berkovich HB ~F =A~2F =a 2 3 t<0.19a
International Materials Reviews 2006 VOL 51 NO 4 211

strongly on the shape of the indenter. Hence Brinell, are clearly illustrated. The issues related to phase
Ludwik, Grodzinski, Rockwell, Vickers, or Knoop transformation during indentation tests are discussed.
hardness numbers are differentiated. A more physical Current industrial practices employing indentation
meaning is assigned to H, when A is taken as the techniques are mentioned.
projection of the area of contact, Ap, between indenter
and surface onto the surface. This definition has become
known as Meyer hardness Hmeyer (Meyer, 1908), the
Indentation size effect
physical meaning of which is the mean pressure p over The hardness obtained from the geometrically similar
the surface of the indentation, if the friction between the indenters, i.e. conical or pyramidal (e.g. Knoop, Vickers,
surface of the indenter and the sample can be neglected. Berkovich) at various loads is expected to remain
Then the pressure is normal to the surface of the indent. unchanged as the strain during the indentation is constant
For symmetry reasons, the horizontal component of the unlike the spherical indenter. However, in a practical
resultant force upon the specimen is zero. The vertical situation, the hardness using similar indentations is found
component of that force is equal to the total force F, to vary with the load. The increase in hardness with
which amounts to decreasing load, which is known as indentation size effect
(ISE), is often observed in metallic, ceramic and inter-
ðr metallic materials (Fig. 1a) (see for example, Mott, 1956;
p 2pxdx~ppr2 ~pAp ~F (2) Gane, 1970; Gane and Cox, 1971; Chen and
0 Hendrickson, 1973; Boldt et al., 1992; Poole et al., 1996;
Grau et al., 1998, Murthy et al., 1999; Mukhopadhyay
x being the radius of an annulus of the contact surface.
et al., 2001; Gong and Li, 2000; Ma and Clarke, 1995;
2r is the chordal diameter and pr2 the projected area of
Gao et al., 1999a; Elmustafa and Stone, 2002, 2003;
the indentation. Thus, Hmeyer5p. Knowing the geometry

Swadener et al., 2002; Paufler and Wolf, 2003). There is
of the contact surface of any test method, the
also a report of a decrease in the hardness with the
corresponding hardness values may be readily converted
decrease in the load, known as reverse ISE (RISE)
into values of Hmeyer. Recently, Pohlenz et al. (2001)
(Sargent, 1986; Upit and Varchenya, 1973; Lim and
studied the different hardness definitions usable for
Chaudhuri, 1999; Sangwal, 2000). Earlier, various
micro and nanoindentation in order to describe the
explanations were offered to account for the ISE and
hardness of substrates and layers by relational coeffi-
RISE. All these interpretations to some extent had some
cients. Malzbender (2003) discussed in detail the various
utility, but they failed to account for this effect
definitions of hardness and elastic modulus as obtained
universally. Turley and Samuels (1981) earlier suggested
with conical and spherical indenters and made a
that ISE is due to abraded surface layers and oxides on
comparison in order to obtain a relationship that
the indented surface. Pethica and Taylor (1979) inter-
permits a conversion and assessment of their differences.
preted that the ISE is due to chemical contamination.
Macro-, micro- and nanoindentation hardness testing
However, Samuels (1986) proposed that the ISE is a
continue to be used extensively in materials evaluation, result of inadequate measurement capability of small
and various aspects of this subject have been reviewed areas of indents and elastic recovery of indents. Li et al.
earlier [Westbrook and Conrad, 1973; Blau and Lawn, (1993) suggested that ISE can be attributed to the
1986; Biswas et al., 1996; Fischer-Cripps, 2004; special indenter–specimen friction. These variations of the
issues in Philosophical Magazine A (1996, 2002) and hardness lead to uncertainty in the determination of
Journal of Materials Research (1999, 2004), Materials the characteristic mechanical properties of materials.
Research Society Symposium Proceedings (Baker et al., Therefore, it is important to understand the mechanisms
1995, 2000; Drory et al., 1995; Gerberich et al., 1996; responsible for the variations in the hardness. There are
Cammarata et al., 1997; Moody et al., 1998; Vinci et al., several empirical and micro-mechanism based theories
1999; Ozakan et al., 2001)]. It is interesting to note that based on elastic recovery, energy balance, strain gradient
various techniques have been developed to study the plasticity (SGP), surface roughness and friction, to
materials response during and after the indentation. In account for the ISE. However, it must be emphasised
addition to conventional optical microscopy, these that the origin of the ISE and the RISE are not yet clearly
techniques include cathodoluminescence, scanning elec- understood and it is still a debatable and controversial
tron microscopy, transmission electron microscopy subject. A full hardness characterisation with a hardness
(TEM), focused ion beam techniques (FIB), interface load curve is necessary to attach true significance to
force microscopy (IFM), atomic force microscopy the hardness value as a characteristic property of the
(AFM), acoustic microscopy, acoustic emission techni- material. Various approaches to account for the origin of
que, Raman spectroscopy (see for example Brown et al., the ISE are discussed in the following sections.
1988; Boldt et al., 1992; Muraki et al., 1997; Ray et al.,
1999; Wolf and Paufler, 1999a,b,c; Kiely et al., 1999;
Mukhopadhyay et al., 2001; Tymiak et al., 2004). Meyer’s power law
Recently, Bhushan and Li (2003) have reviewed in detail Plots of hardness versus load/indentation data are
the various aspects of nanoindentation test apparatus, sometimes fitted to Meyer’s law, which was originally
the data analysis and the application of nanoindentation developed to determine the work hardening capacity of
techniques for determination of mechanical properties metals in Brinell hardness tests. The power law equation
with special emphasis on thin films. Here, the origin of generally employed to analyse the load–indentation data
the variation of hardness with the load/depth of (e.g. Mott, 1956; Bückle, 1965) can be expressed as
indentation is discussed in detail. The use of indentation
P~k1 d n (3)
techniques and results on new materials such as
quasicrystals, bulk metallic glasses and nanomaterials where P is the load, k1 and n are materials constants and

irrespective of the type of material. When n is equal to 2,

the above power law equation is also quoted as Kick’s
law in literature (Kick, 1885). Figure 1a shows the
indentation size effect while plotting the Vickers hard-
ness of quasicrystalline material at various loads. These
data were further analysed using Meyer’s power law
(equation (3)) in a log–log plot (Fig. 1b) from which the
power law index, n is obtained as 1.919, the index of
indentation size effect. It has been pointed out earlier by
several workers that Meyer’s constant, k1 has a strange
dimension of force/(length)n, which is dependent on the
value of n (Li and Bradt, 1991; Sargent, 1986; Ghosh
et al., 2003). In order to resolve this problem, Li and
Bradt (1991) introduced the reference indentation size
corresponding to a load independent hardness, whereas
Sargent (1986) suggested the use of 10 mm indentation
size corresponding to the standard hardness as a
reference. Meyer’s power law is unable to determine
the true or load-independent hardness as it is continu-
ously decreasing with load. In fact, in an extended
load range, Meyer’s power law may not be able to
give a good correlation with the experimental data.
Nevertheless, it is convenient to handle the indentation

data. Grau et al. (1998) studied the strain rate
dependence of the hardness of glass and found a good
correlation with Meyer’s law by analysing the depth
sensing Vickers hardness data on glass for various
loading regimes. However, the differences in Meyer’s
parameters under different loading regimes require
further investigation for better understanding of the
implication of Meyer’s law.
Minimum resistance model

Hays and Kendall (1973) were the first to suggest that
there is a minimum resistance on the surface, which
leads to the violation of Meyer’s law and hence the ISE
is observed. This is significant at lower load. Therefore,
the actual force acting during indentation is lower than
that. According to this model, the force–displacement
relation can be expressed as
P~wzkh d 2 (4a)
One can determine w (minimum resistance against
plastic deformation) and constant kh from the intersec-
tion of the linear plot of !P versus d or P versus d2.
1 a Variation of microhardness obtained from Al–Co– Therefore, the load-independent hardness can be
Cu–Si single quasicrystals with load, establishing the expressed as
indentation size effect; error bar in each measurement
P{w
can be seen (after Mukhopadhyay et al., 2001); b HT ~k ~kkh (4b)
variation of microhardness with load from Al–Cu–Co d2
poly-quasicrystals, showing indentation size effect; c where k is the indenter shape factor (e.g. 1.854 for
corresponding logarithmic plot from which the Meyer’s Vickers hardness). This approach has been verified in
index, n is obtained as 1.919 (after Murthy et al., 1999) various metallic materials, such as Al, Cu and mild steel
using the Vickers and Knoop indenter. However, the
d is the indentation (diagonal/diameter) size. This power minimum load obtained by this analysis was higher than
law equation is also referred to in the literature as any practical value. It was also found that for crystals
Meyer’s law (Hays and Kendall, 1973; Li and Bradt, showing a RISE, the plot of experimental data does not
1991; Gong and Li, 2000; Murthy et al., 1999; Liu et al., give a good fit. Furthermore, negative values of w for the
2003). It should be noted that Meyer’s equation was data at low loads do not give rise to any meaningful
originally developed for a spherical indenter, where n is interpretation.
directly related to the strain hardening coefficient of the
material (Meyer, 1908). Onitsch (1947) extended Polynomial series
Meyer’s power law equation for nonspherical indenters Bernhardt (1941), Mitsche (1948), Bückle (1965), and
and observed that in a macrohardness range n is 2.0, other workers (Fröhlich et al., 1977; Babini et al., 1987)
whereas in a microhardness range, n is less than 2, have approached the relation between P and d from a

3 Correlation of power-law index n with hardness-

to-modulus ratio H/E for a range of single-crystal cera-
mics (after Ren et al., 2002)
the effects of the indenter tip radius effect on the elastic

limit during indentation.
Proportional specimen resistance (PSR)

Li and Bradt (1991, 1993) have extended the idea that
the resistance offered by the surface is not constant
throughout the indentation size but rather dependent on
the indentation size. They proposed a model based on a
proportional surface resistance (PSR) model. According
2 a Indentation data for MgO (001) along ,110. plotted to this model, load is expressed as
according to Meyer’s power law in logarithmic form; b
indentation data for MgO (001) along ,110. plotted P~a1 dza2 d 2 (6)
according to the PSR model (after Ren et al., 2002) where a1 is related to the proportional resistance offered
by the surface of the specimen and a2 is related to the
different point of view. They have proposed a poly- volume. Therefore, the hardness can be expressed as ka2.
nomial relation to correlate P and d as The effect of the first term is larger as the load is
X decreased. However, at higher load, the effect of the first
P~ ai d i (5)
term is negligible. The plot of Pd versus d should yield a
i
linear plot from which one can determine a1 and a2 and
where i is a series of integers. By limiting the number of thus the true hardness. This is exactly the same as the
terms and assuming ao is zero for P50 one gets truncated polynomial series indicated above. However,
P~a1 dza2 d 2 . By considering the contracted series as the physical interpretation of the two constants a1 and a2
an energy balance, because Pd is equivalent to the is distinctly different. In the Li and Bradt model (1991),
energy or work so that a1d may be related to the surface a1 describes the Newtonian like specimen resistance
energy (a1d2) and the a2d2 term may be related to volume of the test specimen and a2 is Kick’s law coefficient
energy of deformation (a2d3), some form of physical relating to the true hardness. Ren et al. (2002) have
significance has been attributed to both a1 and a2. Based investigated microhardness indentations on single-
on the consideration of energy–balance, Bernhardt first crystal MgO (001) along ,110. in air for loads between
suggested that the first term of the equation represents 0.125 and 1.001 kg and temperatures between 20 and
the surface energy term and the second term represents 600uC (Fig. 2a), and also the influence of interfacial
the volume energy term. As a result of this series coatings and lubricants. They observed that the ISE
approach, the a1 represents the energy per indentation decreased with increasing test temperature, and it was
surface area and the a2 represents the energy per unaffected by coating or lubrication. The experimental
indentation induced volume deformation. From various data fitted equally well either the Meyer’s power-law and
analyses, it appears that attaching true significance to a1 the proportional specimen resistance (PSR) models
in terms of surface energy was not quite successful. It (Fig. 2a,b). They have proposed qualitatively that the
can be pointed out that the ao term has been neglected ISE is controlled by the extent of elastic recovery
without sufficient justification. However, according to occurring on removal of the load, and shown the
the Hays and Kendall model, ao is w (minimum correlation of n (as in equation (1)), the index of ISE,
resistance), and therefore it should be related to the with the hardness-to-elastic modulus ratio H/E (Fig. 3).
load for initiation of permanent deformation. Because
ao is so small, it can be neglected in microindentation. Energy balance approach
However, to understand the nanoindentation process, Quinn and Quinn (1997) have investigated the varia-
the load for indentation of permanent deformation may tion of Vickers hardness with indentation load for a
need to be included, which necessitates incorporation of variety of ceramic materials. They observed that such

4 Indentation size-dependence of apparent hardness for 5 Load dependence of apparent hardness for sample Ti
annealed mullite sample (after Gong and Li, 2000) (C,N) based cermet; square symbols represent experi-
mentally measured data, solid line represents predic-
hardness–load curves exhibit a distinct transition to a tion of equation (8) and dashed line represents
plateau with constant hardness level and concluded that prediction of equation (8) assuming a050 (after Gong
the transition in such curves corresponds to the intrinsic et al., 2001)
hardness values of the materials. These investigators
suggested an energy balance model for the Vickers of P05Pzr and do5dzd into equation (6), equa-
indentation process. The model considers that the tion (7) may be rearranged in the following form
external work applied by the indenter is consumed in
the deformation and fracture process in the material. The P~ao za1 dza2 d 2 (9a)
load dependence of hardness has been considered by Li
and Bradt (1996) and Dutta et al. (2001). According to where ao ~bHT dzad{r, a1 ~2bHT dza, a2 ~bHT . P
their approach, the measured diagonal of an indentation has now been split into three parts. It is important to note
at a particular load is an apparent value, which remains that all of the parameters are functions of the experi-
associated with an uncertain amount of relaxation. The mental error and the true hardness. However, a2 is only
extent of relaxation in the indentation diagonal occurs dependent on the true hardness. Equation (9a) can be
due to several possibilities such as crack formation, used for estimating the true hardness, i.e. the energy
dislocation activity, elastic recovery at the tip of the needed to produce the permanent deformation of a unit
indentation. The true hardness can be evaluated as volume. Now a reasonable explanation can be offered for
the size effect in low hardness testing. The first parameter

de 2 ao is related to the surface residual stress, depending on
H~Ho 1z (7) the surface preparation, and is not really a materials
d
property. The second parameter is due to the creation of a
where d5dozde is the apparent diagonal, do is the true new surface by indentation and cracking, the third is
diagonal and de the relaxation in the diagonal after dependent on the volume of the indentation. The above
removal of the indenter. equation is easy to appreciate from the energy point of
However, recent works by several researchers have view. The energy applied is related to Pd, and the energies
shown that the linear relationship between P/d versus d related to the surface phenomena and the volume are
may only be valid in a narrow range of applied loads. basically a1d2 and a2d3. The argument is, if the effective
When a relatively wider range of applied loads is energy or the force can be determined, then the true
considered, the above equation was found insufficient. hardness, which is a characteristic property of the
A modification of the above equation has been material, can be easily determined and in that sense, the
suggested (Gong and Li, 2000; Quinn and Quinn, ISE can be tackled. Here a2 is related to the true hardness
1997). The above equation can be written as
k(ao za1 dza2 d 2 ) a a1
o
Po ~ado zbHT do2 (8) HA ~ 2
~k 2 z zHT (9b)
d d d
where Po and do are the load and indentation size In many cases, it is found that the value of ao is so low
without any experimental error. a is constant related to that the above equation without ao will fit the
the surface energy of the material, and b is a constant experimental data very well. The physical significance
related to the indenter. Gong and Li (2000) have argued of the above equation lies in splitting the energy or the
that experimental errors are usually inevitable in force into the surface and volume related terms. This
conventional hardness testing and therefore it should also takes care of the effect of microcracking. The ratio
be considered. In general, the experimental error in the of a2/a1, has been suggested to be related to H/E
test has been divided into two classes (i) measurement of parameter of the materials. It is important to mention
indentation size, and (ii) indentation load. Considering that the above model is able to explain the ISE as well as
the experimental error in both the load and the the RISE, whereas the model by Bradt and Li will not be
indentation size as r and d, respectively, i.e. by insertion able to explain the RISE (Figs. 4 and 5).

Combined approach: Meyer’s power law and in terms of critical load and indentation size should be
energy balance model represented correctly by equation (14) above.
Recently, Mukhopadhyay (2005) combined both the The nature of equation (14) suggests that hardness
Meyer’s law approach and the energy balance model continuously decreases with the increase in load/size.
and analysed the indentation data. The analysis has been Therefore, it cannot predict the transition from ISE
discussed there. The hardness for an indentation using regime to non-ISE regime. In order to determine the
load P, the corresponding indentation area A, and the transition, the true hardness HT based on the energy
indentation size s, can be written using equation (1) in balance model is incorporated. Initially at lower load,
the apparent hardness will give rise to ISE. But after a
terms of indentation size, Meyer’s constant and the
critical load or indentation size, HA will be equal to HT.
indenter shape factor as
The apparent hardness obtained from normalised
P P kk1 sn Meyer’s equation (13b) can be equated with the true
Hs ~ ~k 2 ~ 2 ~kk1 sn{2 (10a) hardness corresponding to the critical indentation size,
A s s
d*. Therefore, from the above argument, Meyer’s
From the above equation, Meyer’s constant k1 can be
equation can be correlated with the energy balance
written in terms of hardness as
model. The condition of equality is as follows
Hs
k1 ~ (10b) HA ~H1 Dn{2 , HT ~kc
ksn{2
Now inserting the expression for constant k1 in therefore
equation (1)
H1 Dn{2 ~kc (15)

Hs n Hs s2 d n
P~ n{2 d ~ (11) Now from the above condition, the critical indentation
ks k s size, d* can be obtained, after which ISE should cease to
2 exist. Using the value of H15kKms2 and the above
or simply as P~Km Dn , where Km ~ Hks s ~Ps is defined
equation has been rearranged as
as the normalised Meyer’s constant and D~ ds is defined
1 2{n1
as the normalised indentation size. By this transfor- Km s2 2{n Km
mation, one can overcome the dimensional problem d~ ~ in mm as s~1 mm (16)
c c
encountered in the classical Meyer’s equation. Now, this
new Meyer’s constant can be related to hardness or load This is an important relation, which correlates the
for the indentation, which can be defined at any length normalised Meyer’s equation and the energy balance
scale. However, as a natural choice, an indentation size model. The implication of this equation suggests the
s51 mm will be assumed so that one can recover Meyer’s existence of a critical length scale related to the upper
equation in the sense of parameters but not in terms of bound of the ISE. Similarly, the corresponding critical
exact units and dimensions of Meyer’s constants. The load can also be determined.
normalised Meyer’s constant will have a force dimen- The indentation data obtained from decagonal
sion. So, equation (9) can be transformed to a hardness quasicrystals AlCoCu (Murthy et al., 1999) and
equation and can be written as (using s51 mm) AlCoNi (Liu et al., 2003) and the intermetallic
compound Mg32(AlZn)49 (Mukhopadhyay et al., 2004)
kKm n{2 have been analysed (Mukhopadhyay, 2005). The true
H~H1m Dn{2 ~ D ~kKm Dn{2 (12)
s2 hardness and critical indentation size have been deter-
Now, one can summarise the relations obtained by mined. Figure 6 shows the plot of the load–indentation
normalising the classical Meyer’s power law equation and hardness–indentation data from Vickers microin-
as dentation experiments. Both the Meyer’s equation and
the energy balance model are fit with the experimental
P~Km Dn ; or P~Ps Dn (13a) data satisfactorily (Fig. 6a) with a regression coefficient
.0.99. The true hardness (HT) was obtained from the
and energy balance model in each case. The details of the
H~H1m Dn{2 (13b) coefficients are summarised as follows
(a) For the decagonal quasicrystalline material
Using the notation of Li and Bradt (1991) for the critical AlCoCu (Murthy et al., 1999)
:
indentation size as do* and critical load Pc, from Meyer’s law: P~0:00631d 1 9409 ; energy model:
equation (6a) P~{0:00358z0:0096dz0:0049d 2
n
d N
P~Pc (14) HT ~1:8544|0:0049 ~9:08 GPa
d0 mm2
While comparing this equation with equation (17) of Li (b) For the decagonal quasicrystal AlCoNi (Liu et al.,
and Bradt (1991), it can be noted that both equations are 2003)
:
identical except for an extra (2/n) factor, which is Meyer’s law: P~0:0061d 1 9059 ; energy model:
associated with the right-hand side of their equa- : : :
P~0 058{0 0011dz0 0044d 2
tion (17). After analysing their approach, it can be seen N

that this factor was erroneously incorporated in the HT ~1:8544|0:0044 ~8:16 GPa
normalised Meyer’s equation proposed by them, though mm2
the actual numerical value may not significantly affect (c) For the intermetallic compound Mg32(AlZn)49
the analysis. However, the normalised Meyer’s equation (Mukhopadhyay et al., 2004)

deformation occurs progressively in a discrete manner to

relieve stresses created by the elastic flexure of the
surface at the edges of the deformation. During
unloading of the indenter, recovery of the elastic
increment of the deformation which proceeds each new
band of plastic deformation, results in an indentation
appearing smaller than expected, particularly as the
indentation size decreases to approach the scale of
plastic deformation band spacing. The model fits
observed experimental data well and the analysis of
hardness/size data in this way is shown to allow both for
a bulk hardness value and a characteristic deformation
band scale to be calculated for a given sample.
It is proposed that this model is applicable to hard
materials where the elastic deformation effects are
significant and the yielding or cracking occurs at
intervals forming visible lines at an average spacing
characteristic of the material, the grain size and the
surface finish. As the contact area extends further under
the increasing load, yielding occurs at the outer edges,
where the tensile stresses of the surrounding elastic field
combine with the stretching imposed by the sloping faces

of the indenter. It seems reasonable to assume the
average elastic recovery to be d and thus
dm ~di {d (17)
6 a Plot of variation of load versus indentation diagonal
obtained from Vickers microindentation experiment The hardness Ho of the ideal plastic material where the
(Mukhopadhyay et al., 2004) of Mg32(AlZn)49 intermetal- deformation is completely continuous is defined as
lic phase; b experimental hardness data, hardness Ho ~kPdi{2 (18)
curve from Meyer’s equation and true hardness line
obtained from energy balance model, are plotted where k is a constant and P is load. For the proposed
against indentation diagonal (after Mukhopadhyay, system of non-continuous deformation, the above
2005) equation may be used to derive Hm from dm
: {2
Meyer’s law: P~0:0021d 1 9243 ; energy model: Hm ~kPdm (19a)
: : :
P~0 0021z0 0011dz0 0016d 2
Also equation (18) can be rewritten as
N
HT ~1:8544|0:0016 ~2:97 GPa Ho ~kPðdm zdÞ{2 (19b)
mm2
Dividing equation (19b) by equation (19a) gives (by
Now using equation (12), d* values are 70, 27 and rearrangement)
36 mm for the AlCoCu and AlCoNi quasicrystals and

for the Mg32(AlZn)49 phase, respectively. This appears d 2
to be reasonable and consistent with the trend of the Hm ~Ho 1z (20)
dm
hardness plot with the indentation size, which can be
seen in Fig. 6b. The intersection between Meyer’s curve At high load dm&d, Hm tends to Ho. At lower load, as d
of hardness and the true hardness line can clearly be is the more significant fraction of dm, the measured
seen. The true hardnesses for the AlCoCu, AlCoNi and hardness will increase. The values of Ho and d may be
Mg32(AlZn)49 phases were found to be 9.01, 8.16 and determined by fitting experimentally determined values
2.97 GPa, respectively, which also seem to be consistent. of Hm and dm. Table 1 shows fitting parameters.
The present analysis lends strong support to the
proposed approach for determining the critical indenta- Indentation-induced cracking
tion diagonal by involving both Meyer’s power law
Li and Bradt (1991) proposed that during loading, the
equation and the energy balance model. Thus, the
test load is balanced by the total specimen resistance
normalised Meyer’s equation proposed here can give rise
composed of four components due to (i) friction at the
to a better understanding of Meyer’s constant (Km) and
indenter/specimen facet interface (frictional component),
its exponent (n). These parameters combined with the
(ii) elastic deformation, (iii) plastic deformation, and (iv)
coefficient of the energy balance model can predict the
critical indentation size after which ISE does not exist. specimen cracking. According to these authors, fric-
tional and elastic effects lead to the normal ISE while
indentation cracking contributes to the apparent hard-
Elastic/plastic deformation (EPD) model ness, HA, measured by a Vickers diamond indenter. It
Bull et al. (1989) proposed a quantitative model to may be written as
explain the ISE often observed in the hardness response 5=3
of hard brittle material which is based on mixed P P
HA ~l1 K1 2 zK2 (21)
elastic and plastic deformation, whereas the plastic d d3

where d is the indentation diagonal, l1, K1 and K2 are

constants. The constant K2 depends on the applied load
P while K1 is a geometrical conversion factor whose
value depends on the indenter geometry. For an ideally
plastic body, HA is equal to the first part, whereas for
brittle solids, the second part is related to HA.
Peng et al. (2004) investigated the nanoindentation
hardness of a commercially available soda-lime glass, a
tetragonal ZrO2 polycrystal and a hot-pressed Si3N4 in
the peak load range from 7.5 to 500 mN and observed
the ISE. This was further analysed using Meyer’s law,
the Hays–Kendall approach, the proportional specimen
resistance (PSR) model, the elastic recovery model and
the modified PSR model. It was established that (i)
Meyer’s law provides a satisfactory description for the
experimental data for each material but cannot account
for the origin of ISE; (ii) the Hays–Kendall approach,
the elastic recovery model, the PSR model and modified
PSR model yield meaningless values of the parameters in
the corresponding equations. For each material, the true 7 Schematic diagram of geometrically necessary disloca-
hardness was also determined based on the PSR model, tions created by rigid conical indenter; dislocation
the elastic recovery model and the modified PSR model,
structure is idealised as circular dislocation loops;

respectively. It was found that the true hardness values angle between surface of conical indenter and surface
obtained from these different models are similar to each plane of indented material is q, and indentation depth
other. This similarity can be attributed to the similarity is denoted by h (after Qui et al., 2001)
between the empirical equations employed in these
models. A similar type of analysis and conclusions was
predominates when the indentation depth is shallow.
also made by Sangwal (2000).
They have found good agreement between theoretical
and experimental results of the size-dependent hardness,
Friction and surface effects indicating that the surface effect plays an important role
Initial elastic resistance, which is characterised by a in size-dependent hardness.
sharp fall in hardness above a very small indentation size Gerberich et al. (2002) proposed that the ISE can be
has been identified in low load indentation tests of non- linked to energy for the newly created surface and
metals. Such behaviour is consistent with a requirement the plastic strain energy dissipation and estimated the
for a critical strain energy to trigger permanent surface work and volume work associated with the
deformation or more probably cracking. Atkinson indentation. Their analysis indicates that the total
(1995a,b) has shown that, in many cases, friction has surface work is given by the product of the contact area
been responsible for a marked indentation size effect in and the surface energy. They observed that the ratio of
low load testing of some metals, and the magnitude of surface work to plastic volume work is nearly constant
the effect has been associated with stain hardening. This for a wide range of shallow depths and decreases rapidly
intrinsic form of a size effect has been related to the with increasing depth of penetration and consequently
special deformation conditions of a plastic hinge at the giving rise to ISE. Zhang and Xu (2002) have studied the
perimeter of the indentation. The principal factor in surface effects on nanoindentation and introduced an
the size effect in low load testing of Fe and Al has been apparent surface stress that represents the energy
identified as due to friction. It is, therefore, reasonable to dissipated per unit area of a solid surface in nanoinden-
suppose that the minimal size effects in these ultra micro tation tests.
indentation tests could be a consequence of a particu-
larly low friction condition. It has been shown by Bobji Strain gradient plasticity: geometrically
and Biswas (1999) that the surface roughness has a necessary dislocations
substantial influence on the nanohardness, irrespective Stelmashenko et al. (1993), De Guzman et al. (1993),
of whether the bulk and surface mechanical properties Fleck et al. (1994), Ma and Clarke (1995), Poole et al.
are the same. Y. Wei et al. (2004) have studied the ISE (1996), Nix and Gao (1998), McElhaney et al. (1998),
and attributed it to dislocation density theory as well as Gao et al. (1999a,b), Acharya and Bassani (2000) and
some environmental effects such as indenter tip curva- Huang et al. (2001) advocated strain gradient theory to
ture and surface roughness. Zhang et al. (2004) discussed account for ISE. This theory assumes that the flow stress
the role of plastic deformation of rough surfaces in the is related to the statistically stored dislocations and
size-dependent hardness. They proposed a bearing ratio geometrically necessary dislocations (Fig. 7). According
for nanoindentation of rough surfaces. During an to the strain gradient plasticity (SGP) model, the strain
indentation, the work done can be separated into bulk gradient plays an important role in plastic deformation.
work and surface work. The surface work causes the In the formulation of plasticity theory, the constitutive
plastic deformation of an indented rough surface and law contains strain gradient as a variable and hence
thus dissipates energy, which is necessary to form the there is an intrinsic length scale. This theory is based on
impression of the solids. The energy dissipation occur- the observation that gradients of plastic shear result in
ring at the indented surface is among the factors that the storage of the so-called geometrically necessary
cause the ISE at the micro/nanoscales. The surface effect dislocations (GND), which affect the yield stress in a

similar manner as the common statistically stored

dislocations. The densities of the geometrically necessary
dislocations being proportional to the strain gradient
become appreciable, when the relevant size of indenta-
tion is small. The indentation at low load means that the
strain gradient is higher as the strain under the indent is
constant (for example 8% in Vickers geometry). The
strain gradient is directly proportional to the geome-
trically necessary dislocation. The shear stress t is
related to dislocation densities as follows
pffiffiffiffiffiffiffiffiffiffiffiffiffiffi
t~CGb rs zrg (22a)
where G is the shear modulus, b is the magnitude of
Burgers vector and C is a constant taken to be 1/3 by
Ashby (1970). rs and rg are the densities of the
statistically stored dislocations and GNDs. Ma and
Clarke (1995) estimated the density of GNDs of the
indentation of diagonal length d as
8 Microindentation hardness data for single-crystal and
4c polycrystalline copper, as well as for single crystal sil-
rg & (22b) ver; h is indentation depth, H is microindentation hard-
bd
ness, and H0 is indentation hardness for large depths
For metals, the hardness is three times the flow stress, so

of indentation; Nix–Gao relation is also shown for
the hardness can be approximately written in terms of
each set of experimental data, and it agrees well with
dislocation as
the microindentation hardness data (after Qui et al.,
1 2001)
4c 2
H&Gbrs 1z (23a)
rs bd
Nix and Gao (1998) expressed the SGP model using
Obviously, when rg&rs, the above equation is dominant the GNDs and Taylor’s dislocation work hardening
to control the hardness and it explains the increase in theory, for a geometrically similar indenter, with the
hardness as the load decreases. However, at higher load or size-dependent hardness in terms of indentation depth as
indentation diameter, the densities of GNDs may be rffiffiffiffiffiffiffiffiffiffiffiffiffi
negligible compared to the statistically stored dislocations. 2 h
H ~Ho 1z (24a)
The above equations can be written in the following form, h
so that it can be tested by fitting the experimental data where h* is a characteristic length that depends on the
a indenter shape, the Burgers vector and statistically
H 2 ~Ho2 1z (23b) stored dislocation. Using this model, Nix and Gao
d
(1998) developed a law for strain gradient plasticity,
where a~ r4cb is constant for a certain material. One can which became the theoretical basis of the mechanism
s
plot H2 versus 1/d and from the intercept, the size based strain gradient (MSG) plasticity to explain the
independent plastic hardness can be obtained and from ISE (Fig. 8). Qui et al. (2001) considered the intrinsic
the slope the dislocation densities can be determined. lattice resistance (Wo) which varies with lattice orienta-
Ma and Clarke (1995) have done this experiment on a tion and modified the above equation as
silver single crystal in order to test the strain gradient
plasticity theory. GNDs are the dislocations which are sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi

necessary to accommodate the geometry of plastic 2 3s0 2 h
deformation. Such dislocations are required to create H ~3so zHo 1{ z (24b)
H0 h
the plastic indent in a microindentation process. These
dislocations act as obstacles to the statistically stored With this modified model, Qui et al. (2001) explained the
dislocations and cause additional work hardening of the dependence of ISE on the crystalline orientation, which
material. It is also important to mention that Ma and was reported by Stelmashenko et al. (1993) in a W
Clarke (1995) developed a geometrical scaling model for crystal. Swadener et al. (2002) have modified the above
ISE. They partitioned the applied indentation force into equation by adding a contact depth-dependent constant
the force on the flat surfaces and the force over the edges H1 as
and finally derived size-dependent hardness for various rffiffiffiffiffiffiffiffiffiffiffiffiffi
2 h
indentation tips. The fitting of the experimental data H ~Ho 1z zH1 (24c)
with this geometric scaling model appears to be as good h
as with the strain gradient plasticity (SGP) model. For where H1 is a work hardening component representing
simplicity, in the case of the SGP model, it can be the increase in hardness from the onset of yielding to an
assumed that the indent is accommodated by the effective strain. The modified equation was employed for
circular loops of GNDs with the Burgers vectors normal studying ISE in NaCl and LiF single crystals. Elmustafa
to the plane of the surface. The presence of these GNDs and Stone (2002, 2003) have added a contact depth-
causes storage of additional defects and increases the dependent term Hf (which is similar to H1) representing
deformation resistance by acting as obstacles to the the hardening mechanism other than dislocations. They
statistically stored dislocations. have observed that for indents shallower than 150 nm,

9 Plot of experimental H versus d (mm) data obtained from microindentation experiment, along with those predicted
based on SGP and modified SGP model including the extra softening term; the modified SGP model shows a better
agreement compared to the SGP model (after Mukhopadhyay et al., 2005)
the slope of the plot decreased abruptly by a factor of expand and propagate into the crystal thereby causing
10 in comparison with the microhardness and deep the ISE. Chen and Hendrickson (1973) studied the
nanoindentation data, resulting a bilinear behaviour. As indentation of Ag single crystals with a wide range of
more and more experimental results were reported, it loads and found both ISE and RISE below a certain
was found that the equation could not satisfactorily fit load. They observed the distinct differences in terms of
all the experimental results (Mukhopadhyay et al., appearances of dislocation rosettes around the indents.
2005). There are attempts to add an extra term to take They concluded that the interaction of the dislocation
care of extra terms due to hardening or softening pattern is different and can be held responsible for ISE
depending on the material (Fig. 9). and RISE. Lim and Chaudhuri (1999) made an
experimental investigation of nanohardness of the
Dislocation mechanics: classical polycrystalline work-hardened and annealed oxygen
In the MSG model, Gao et al. (1999a) extended Taylor’s free copper (OFC) for different indenter loads. The
dislocation model to include the strain gradient plasti- work-hardened sample shows a three-stage behaviour –
city. In Taylor’s dislocation model, the dislocations are once H decreases (I) and increases (II) and then
considered as statistically stored. As the size of the decreases again (III). This phenomenon cannot be
indent becomes smaller, the gradient becomes steeper. obviously explained by the strain gradient plasticity
Taylor’s dislocation hardening model is modified to model. A three-stage qualitative model has been
accommodate GNDs. Gao et al. (1999a,b) indicated that proposed. In stage I – at low penetration depth
the strain gradient plasticity is applicable between 0.1 (150 nm) – dislocation loops are nucleated at a relatively
and 10 mm. When the indent is less than 0.1 mm, high shear stress value of about (G/75). According to this
dislocation mechanics dominates. Several workers have model, at relatively low penetration depths, the nano-
extended the classical theory of dislocations without hardness reflects the shear stress value required for
invoking the strain gradient plasticity theory to explain nucleation and expansion of dislocation loops. Also in
the ISE and the RISE (Mott, 1956; Gane, 1970; Chen this stage, the earlier dislocation densities have little
and Hendrickson, 1973; Upit and Varchenya, 1973; effect on nanohardness values. The indenter penetration
Sargent, 1986; Vitovec, 1986; Sangwal, 1989; Lim and increases and consequently the numbers and diameters
Chaudhuri, 1999; Sangwal, 2000). In the case of an of dislocation loops become significant. This is the
indentation experiment with sharp indenter, stresses beginning of the second stage, when the nanohardness of
always build up under an indenter with a pointed tip the work-hardened material may even increase with
sufficient for homogeneous nucleation of dislocation in a increasing indenter penetration owing to dislocation
perfect crystal. Therefore a change in the length of interactions. For still larger indentations, the third stage
dislocation sources and in the concentration of defects in begins when a sufficiently large number of dislocations is
stressed volumes of different size cannot play the created around the indentation. After the nucleation of
determining role compared to the conditions of disloca- initial dislocation loops under the indenter tip, as the
tion movement under the indenter. Upit and Varchenya load is increased, more and more dislocation loops will
(1973) suggested that the peculiarity in the dislocation be created, the diameter of which correspond to the
movement in the case of indentation is that dislocation current size of the indentation contact. Then to increase
loops nucleated under the indenter near the surface the indentation size further, sufficiently high shear stress

10 Stress–strain diagram for a perfectly plastic, b elastic–plastic, c real elastic–plastic solids
values will be required to cause the dislocation loops to increase in H with h steadily becomes weaker until H
grow in size and to glide. It was suggested that the shear attains a steady value after some particular value of
stress required to propagate a dislocation loop in copper load. The RISE phenomena essentially take place, which
is related to its radius L by readily undergo plastic deformation. It appears that the
RISE can be caused by (i) the relative predominance of
Gb
t~ (25) nucleation and multiplication of dislocations and (ii) the
L relative predominance of the activity of either two sets of
where G544 GPa is the shear modulus of copper and slip planes of particular slip systems or two slip systems
b50.225 nm is the Burgers vector of dislocations. below and above a particular load.
Therefore with increasing radii of the dislocation loops

and with increasing indenter depth, the shear stress Mechanics of indentation
required to glide them will decrease and consequently,
hardness will decrease with load and then finally will be Among the several theoretical models, the three most
independent of load at larger load. extensively discussed models will be highlighted here.
It can be indicated that it is difficult to explain These are (i) the elastic indentation model, (ii) the rigid
maxima due to the RISE using the PSR, elastic/plastic perfectly plastic model and (iii) the spherical cavity
deformation (EPD) and SGP models. It is understood expansion model. The behaviour of these three solids
that the average hardness increases with the dislocation can be realised from the stress–strain diagram in Fig. 10.
density. The appearance of maxima suggests that the
indentation process is intimately connected with nuclea- Elastic model
tion and motion of dislocations. The inherent defect The elastic indentation model was originally developed
structures would obviously act as obstacles for the by Hertz (1882), Boussinesq (1885) and Sneddon (1965)
motion of the defects produced by nucleation. It is clear independently. In this model, it is assumed that the
from the literature that the RISE occurs only in the indenter is rigid and the material of the specimen
single crystals undergoing plastic deformation. satisfies the linear elasticity theories (Fig. 11). The
Therefore, it may be concluded that the RISE occurs pressure distribution, p(r) for the cone can be expressed
only in materials where plastic deformation is dominant. as
It is well known that in the initial stage (i.e. at low loads
or strain), plastic deformation of crystals mainly E cot h
p(r)~ cosh{1 (a=r) (26a)
involves the nucleation of dislocations in a particular 2(1{n2 )
slip system, but with increasing strain, dislocation where E is the elastic modulus, v is Poisson’s ratio, h is
multiplication (by processes like cross slip and activity the semiapical angle of the cone, and a is indentation
of Frank read source) takes place. The latter process is diameter. The mean contact pressure can be written as
accompanied by work hardening. The RISE is also
explained based on the effects of vibration and indenter E cot h
pm ~H~ (26b)
bluntness at low load (Westbrook, 1967; Hanneman and 2(1{n2 )
Westbrook, 1986), the applied energy loss as a result of The solution for other wedge, sphere and flat-end
specimen chipping around the indentation (Banerjee and solutions can be found in the work of Sneddon (1965)
Feltham, 1974; Feltham and Banerjee, 1992) and the
generation of radial or median cracks (Li and Bradt,
1996).
Sangwal (2000) suggested that at low loads, when only
one slip system is active, active parallel glide planes are
few. Therefore, the nucleation of dislocations rapidly
propagates into the material without substantially
experiencing mutual interaction stress between them.
However, with increase in load, when the number of
parallel glide planes is increased, the motion of
dislocations gliding along them slows down due to the
mutual interaction stresses between dislocations. This
leads to a slow increase in indentation depth with
increasing indentation pressure. Consequently, the 11 Indentation of ideally elastic solids by conical indenter

12 Slip-line field solution for indentation of rigid plastic solid by frictionless wedge of semiapical angle h
and Timoshenko and Goodier (1951). With the elastic (Fig. 13). This is perhaps because the metals are not
rubber, the indentation pressure is a direct measure of the rigid but elastic–plastic materials.
elastic properties of the material. One can see that the
hardness is independent of indentation size. However, for Spherical cavity expansion model
a spherical indenter, H will be a function of the load and The spherical cavity model (Fig. 13) was first advocated
the radius of the curvature R of the sphere by Bishop et al. (1945) and later developed by Marsh
2=3 (1964), Hirst and Howse (1969) and Johnson (1970).

P1=3 4E Among all these, Johnson’s analysis has been the most
H~ (26c)
p 3R(1{n2 recognised analysis for indentation of elastic–plastic
It has been assumed that friction and the elastic solids. The results are reasonably close to the experi-
deformation of the indenter are negligible. For elastic mental observations for materials with either very high or
material, the indentation disappears after unloading. very low values of E/Y. An improved analysis comes from
Therefore, the depth can be measured from the Johnson (1970). The radial expansion model is the
instrumented hardness testing equipment so that the bottom half of the spherical cavity and therefore does
area can be found from the depth measurement. not provide for any piling up of any displaced material
outside the indentation. Evidently, the volume of the
indentation is ultimately taken up in the elastic hinter-
Rigid perfectly plastic model (slip-line field
land, so that the shape of the indenter must be involved.
approach) For a cone of semiapical angle h, the critical parameter
This model is based on the slip-line field theory now becomes (E/Y)cot h, while for a spherical indenter,
advocated by Prandtl (1920) and later generalised by the corresponding quantity is (E/Y)(a/R). The final
Hill et al. (1947). In this model, the material is relation for cones or pyramids is then
considered as rigid perfectly plastic, i.e. no plastic
deformation occurs until a stress Y is reached. The H 2 E cot h
~ 1z ln (28)
hardness obtained by this theory is the upper bound of Y 3 3Y
the hardness. These solutions successfully predict the
while, for spherical indenters, cot h is replaced by a/R. This
hardness for materials with high values of E/Y, using
treatment assumes that the material has a constant yield
sharp indenters, but not so successfully for materials
stress, Y, and that there is no work hardening produced by
with low values of E/Y or for blunt indenters. The
pressure p across the punch is uniform and has the value the indentation process itself. According to Hill’s original
solution, the pressure in the cavity when the plastic–elastic
p boundary is at a distance c from the centre is
p~H~cY ~2k 1z (27)
2
P 2 c
Thus H52.6Y (Tresca criterion) and H53Y (von Mises ~ z2 ln (29)
Y 3 a
criterion). In general, one can write H5cY, where c is
the appropriate constraint factor which will depend on This implies that the elastic–plastic boundary coincides
the geometry of the indenter and the interfacial friction. with the boundary of the cavity itself (c5a) at P52/3Y,
The slip-line field for a two-dimensional wedge of and below this contact pressure, the analysis fails and no
semiapical angle h is shown in Fig. 12 and the pressure plastic flow can occur. However, there is no case of plastic
across the face of the indenter for frictionless indenta- indentation occurring in any system for an indentation
tions is p5H52k(1za) where cos(2h–a)5cos a/ pressure less than Y. On the other hand, in the region
(1zsin a). The slip-line field approach to plastic where p53Y, equation (27) shows that c53.2 and it must
deformation has been widely applied to metal forming, be assumed that the elastic yielding of the hinterland no
metal working and indentation hardness. It was pointed longer influences the plastic flow of the material. The
out by Tabor (1986) that deformation patterns predicted contact pressure now corresponds to the classic theory for
by slip-line theory were not observed in indentation a rigid plastic solid. However, there is nothing in the
experiments in metals. However, it was later recognised expanding cavity model to indicate that the indentation
that the mode of deformation observed by Tabor (1986) pressure has an upper limit of 3Y. As noted by Tabor,
closely agrees with that proposed by Mulhearn (1959) the expanding cavity model is a helpful and fairly
and Samuels and Mulhearn (1957) as compression mode realistic description of the indentation process in the

13 Compression mechanism of indentation proposed by Mulhearn (1959) showing elastic–plastic boundary and defor-
mation resembling expansion of spherical cavity into elastic–plastic solid by internal hydrostatic pressure
‘compression’ or radial flow mode. Attempts have been extensively discussed by Bhushan and Li (2003) and
made to improve it to give better numerical agreement Oliver and Pharr (2004) and therefore it will not be
with experiment. A more satisfactory approach involves discussed here further. Some other approaches to
finite element analysis and the newer technique of analysing the load–indentation data will be discussed.
boundary element analysis, but even these techniques It is important to mention that still the problem of
have limitations imposed by the theoretical assumptions actual contact area in case pile-up and sinking-in has not
involved. yet been sorted out. In order to obtain a more accurate
value of hardness and Young’s modulus, there are
Elastic and perfectly plastic model suggestions to use the actual contact area by imaging the
Recently, Yu and Blanchard (1996) developed an indents using scanning probe microscopy (Lim and
analytical model of hardness for four major indentation Chaudhuri, 1999). The total work (Wtot) of indentation
tests. They have determined the analytical relationship and the reversible work Wp of indentation, defined,
for calculating hardness from the uniaxial material respectively, as the area under the loading curve and that
properties and indenter geometry for a wide variety of between the loading and unloading curves (Fig. 14),
elastic and plastic materials. The models are presented have also been used for materials characterisation
here in order to understand the mechanics of the (Sakai, 1993; Hainsworth et al., 1996; Rother, 1995;
indentation process. These models provide a simple Rother and Dietrich, 1994; Cheng and Cheng, 1998e,
but powerful method for relating hardness from one 1999; Faulkner et al., 1998; Giannakopoulos and
type of hardness test with that of a different test, or Suresh, 1999). It is therefore relevant to review the
evaluating uniaxial properties from hardness measure- work investigating the relationships between these
ments. For example, the hardness of a conical indenta- different materials properties and the parameters obtained
tion can be directly calculated by the following from the indentation experiments. Giannakopoulos and
procedure if the uniaxial properties of the material and Suresh (1999) discussed three-dimensional finite element
the angle b of the indenter are known simulations of elastoplastic indentation along with
Vickers and Berkovich indentation experiments and
E tan b 2(1{n2 )YCb
H~ tanh (30a) provided the following results (assuming the load–depth
2(1{n2 ) E tan b
relation as P5Ch2, where C is the indentation curvature)
where Cb ~ p2ffiffi3 (2:845{2:3757|10{2 b), and 0u,b(
37.5u. To evaluate the uniaxial properties of a material
P sy E
from the hardness measurements, the yield stress can be C~ ~M 1 s0 :29 1z M2 z ln ( ) ,
h2 s0:29 sy
evaluated from the following relation
pav
E tan b 2(1{n2 )H for 0:5¢ ¡3:0 (31)
Y~ tanh{1 (30b) sy
2
2(1{n )Cb E tan b
In the above equation, sy and s0.29 are the yield strength
and stress corresponding to the characteristic plastic
Determination of elastoplastic properties: strain of 0.29 for the indented material in uniaxial
relationship between hardness and elastic compression. The constants M157.143 and M2521 for
modulus the Vickers pyramid indenter with an included tip angle
The analysis of load–indentation data following of 136u. The corresponding values for the Berkovich
the technique of Oliver and Pharr (1992) has been indenter are M56.618 and M2520.875 with an included

where d*55 for a Vickers pyramid indenter and

d*54.678 for the Berkovich indenter; the conical
indenter results are similar to the Vickers or Berkovich
indenters depending on the included apex angle. The
step-by-step method has been suggested extracting
the materials properties. Following this approach,
Mukhopadhyay et al. (2001) determined the Young’s
modulus of quasicrystalline materials which matches
well the data obtained by the ultrasonic technique.
Energy-based approaches to the indentation of brittle
materials are proposed by Sakai (1993), analysing the
instrumented load indentation data. The hysteresis loop
energy, Ur which is dissipated during the indentation
loading–unloading cycle is related to the true hardness H,
apparent hardness HA and the work of indentation c1.
The true hardness has its energy-derived meaning of the
irreversible energy consumption to create a unit volume
of indentation of ideally plastic materials. The relation-
ship between Ur and the three half powers of indentation
load P3/2 and between Ur and the volume of the
indentation impression VI are used to separate the plastic
contribution from the complicated plastic/elastic surface

14 Illustration of a conical indentation and b loading and deformation processes in the indentation tests. The linear
unloading curves, where Wtot is total work, Wp is irre- relationship of Ur versus P3/2 provides an important
versible work and We is reversible work: Wtot5 experimental technique for determination of true hard-
WpzWe (after Cheng et al., 2002) ness H of the brittle materials. The linear relationship of
Ur versus V1 is available to the experimental determina-
tip angle of 130.6u. The circular conical indenter also tion of c1. The relationship has been developed as follows
follows the same results as the Vickers or Berkovich sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi!
depending on the apex angle of the cone. If Pav/Wy falls 1 1 1
Ur ~ pffiffiffiffiffi P3=2 (36)
outside the bounds of the equation, the indenter response 3 a0 tan y 2
H
is either elastic or elastic–perfectly plastic. By accounting
for the effects of strain hardening on pile-up and sinking- which enables one to evaluate the true hardness of the
in and on the true contact area through three-dimensional brittle materials from an experimental relationship.
simulations, the following relationship between the Amax Theoretical predictions obtained through this formalism
and hmax has been derived for elastoplastic materials were experimentally confirmed. The energy-based
approach and its application to brittle materials can
Amax
~9:96{12:64(1{S)z105:42(1{S)2 { (32) provide significant and potential directions for studies of
h2 the load–indentation size effect, machining-induced
Pav damage, brittle/ductile transition behaviour at elevated
229:57(1{S)3 z157:67(1{S)4 , with S~
E temperatures of ceramic materials, as well as of the
This equation is a polynomial fit to the computationally dislocation process and plasticity of ceramic single
determined values of Amax/h2. The effective Young’s crystals. Hv Vickers hardness with Meyer definition
modulus of the indenter–specimen system is defined as (indentation load divided by the projected area of
indentation impression), j ratio of residual indentation
{1 depth and the depth at maximum load, finite element
1{n2 1{n2in 1 dP
E ~ z ~ pffiffiffiffiffiffiffiffiffiffi (33) analysis for elastoplastic Vickers indentation are con-
E Ein c Amax dh
ducted in which the effect of strain hardening on
The subscripts ‘in’ (equation (33)) represent properties indentation behaviour is intensively examined. A novel
of the indenter and dP/dh is the slope of the P–h curve of procedure of graphical superposition is proposed to
the initial stages of unloading from Pmax. The constant determine the representative yield stress, YR. It is
c*51.142 for the Vickers pyramid indenter, 1.167 for the confirmed that the concept of YR applied to elastic–
Berkovich indenter and 1.128 for the circular indenter of fully plastic solids is sufficient to describe the indenta-
any included apex angle. The ratio of the penetration hr tion behaviour of elastoplastic solids with strain hard-
upon complete unloading to the maximum penetration ening. However, Tabor’s representative strain (8%) at
depth, hmax, before unloading, is indicative of the extent which YR is described is only applicable to elastoplastic
of plastic deformation and strain hardening such that solids with their ratio of Young’s modulus E to yield
2 ratio Y (E/Y) ranging from about 400 to 1000. The true
s0:29 {sy :142 hr {0:957 hr hardness H as a measure of plasticity is estimated from
~1{0 (34)
0:29E hmax hmax the Meyer hardness HM and then successfully related to
Elastoplastic finite element analysis of the sharp yield stress Y and the strain-hardening modulus Ep, as
indenter, also reveals that well as YR. True hardnesses obtained from this
formalism have been displayed for materials in
hr pav Table 3. The true hardness is always found to be much
~1{d (35)
hmax E higher than the conventional hardness, especially in the

Table 2 Fitting parameters for observed scale dependence of hardness for various ceramic materials
Material Ho, kg mm22 d, mm q, kg mm22 n
Sapphire (1012) 2129 1.34 4265 1.81

Deranox (alumina pc) 1642 2.05 3839 1.79
MgO (001) (sc) 791 2.58 2374 1.73
Silicon (001) (pc) 699 3.97 3004 1.65
SiC (001) (sc) 2513 1.92 6972 1.72
REFEL SiC (pc) 2461 1.10 3764 1.90
ZrO2 1216 1.58 2374 1.83
Parameters q and n refer to the usual ISE model of eqn. (Meyer’s law) while Ho and d are derived from the new model described by
equation (18). It should be noted that while q in the ISE model is hardness value standardised at unit indentation size, Ho in the new
model is large-scale macroscopic hardness (sc5single crystal, pc5polycrystal) (Bull et al., 1989).
case of brittle materials. However, this approach has yet respective loading and unloading curves are given by
to be adopted in real practice. F ~ahm and F ~b(h{hf )l , where a and b are functions
Using a scaling approach to the indentation problems, of materials properties and indenter geometry, a
an approximate relationship between the ratio of relationship between Wp/Wtot and hf/hm is then given by
hardness to elastic modulus and the ratio of irreversible
work to total work has been proposed. The work of Wp mz1 hf m{l
~ { (38)
indentation and the geometry of indentation can be Wtot lz1 hm lz1
referred in Fig. 14 (Cheng and Cheng, 1998a–e; Cheng This discussion obviously suggests that a general
et al., 2002). The ratio of hardness and Young’s modulus relationship exists between Wp/Wtot and hf/hm and this
can be obtained from measuring the work of indenta- relationship is explicitly independent of indenter geo-
tion. Together with a well known relationship between metry. This relationship is also explicitly independent of
the elastic modulus, initial unloading slope and contact the details of the material properties and the stress and
area, a new method is then suggested for estimating the distribution with similar indenters.
hardness and the modulus of a solid using instrumented Using dimensional analysis and finite element calcula-
indentation with conical or pyramidal indenters. In the tions, several relationships that relate the features of
following, the relationships are shown indentation loading and unloading curves to the hard-

dF 2 pffiffiffiffi ness, elastic modulus and work of indentation are
~ pffiffiffi E A (37a) proposed for elastic–plastic solids. These relationships
dh h~hm p
provide new insights into indentation measurements
(Cheng et al., 2002). Earlier, Lawn and Howes (1981)
H 4 F
~ (37b) studied the elastic recovery effect in the indentation of
E 2 p (dF =dh)2 several ceramic materials and steels. By assuming that
the respective loading and unloading curves are given by
p Wtot {Wu ðdF =dhÞ2 F ~ah2 and F ~B(h2 {h2f ) where A and B are functions
H~ P2h (37c)
4 Wtot F of materials properties and indenter geometry, a
relationship between Wp/Wtot and hf/hm was obtained

p Wtot {Wu ðdF =dhÞ2
E ~ Ph (37d) F ~B(h2 {h2f ) (39)
4 Wtot F
The results from this equation are plotted in Fig. 15.
where Ph WtotW{W
tot
u
is a dimensionless function. Several The finite element calculations and equation agree well
experimental data points from the literature using with each other. Finite element calculations reveal the
Berkovich diamond indenters on Cu, W, Al, fused silica relationships between final depth, hardness and elastic
and sapphire are also shown to follow this close modulus and they are shown in Fig. 16. It is obvious
relationship. The finite elastic constants of the diamond that an approximately linear function exists between hf/
indenter are taken into account using the reduced hm and H/E* for each indenter angle. The relationships
modulus. It has been further emphasised that further can be summarised as
experiments and modelling efforts will ascertain the hf H
accuracy of this proposed method. ~1{l , where l~1:50 tan (h)z0:327
hm E
Mencik and Swain (1994) have explored the relation-
ship between Wp/Wtot and hf/hm. By assuming that for 600 ¡h¡800 (40)
Table 3 Density, elastic modulus and hardness parameters (Sakai, 1993)
Bulk density, True hardness Work of indentation Apparent hardness

Material g cm–3 E, GPa HV, GPa H, GPa c, GPa HA, GPa
Al 2.71 74.7 0.39 0.40 0.61 0.65

Cu 8.90 139 1.01 1.05 1.40 1.56
MgO 3.52 309 4.91 7.46 4.90 6.81
Si3N4 3.22 331 15.1 19.7 9.30 17.2
SiC 3.22 448 23.7 54.0 9.70 22.1
Glassy carbon 1.50 29.9 – 202 0.25 2.50

15 Relationship between hf5hm and Wp5Wtot (after Cheng et al., 2002)
It is important to point out that Marx and Blake (1997) where cE and cH are parameters that are affected by the
have shown a linear relationship for conical indentation degree of surface sinking-in or piling-up. A reasonable
with a semicone angle of 70.3u, in elastic–plastic solids agreement between the Lawn–Howes model and the
with bilinear uniaxial stress–strain relationships. Cheng finite element results was found when cE/cH is about
and Cheng (1998e, 1999) have shown a similar relation- 1.18. However, the above equation does not predict the
ship for conical indentation in elastic–plastic solids with approximately linear relationship. Future research is
power law work hardening for a particular semicone needed to understand better the relationship between hf/
angle of 68u. Several other workers have proposed hm and H/E*. From the studies of scaling and finite
models that link the two quantities (Lawn and Howes, element analysis, Cheng et al. (2002) have obtained the
1981; Sakai, 1993). In these models, the degrees of following relation, using We5Wtot–Wp
piling-up and sinking-in of surface profiles were treated
H We 1
as adjustable parameters. The relationships between hf/ ~k where k~ for 600 ¡h¡800 (42)
hm and H/E* are influenced by these parameters. Lawn E Wtot l(1zc)
and Howes (1981) proposed the following relationship However, the value for k obtained using this expression
2 cannot be applied to sharp cones (45u) owing to the
hf c H validity range of l. From this relationship, the ratio of
~1{ 2 E tan h (41)
hn cH E H/E* can be obtained readily by measuring the work
of indentation to obtain We/Wtot. Furthermore, since
the ratio of H/E*2 can be obtained from the initial
slopes of the unloading curves (Joslin and Oliver,
1990; Hainsworth et al., 1996; Cheng and Cheng,
1998a,b,c,d,e), the values of H and E* can, in principle,
be obtained from the work of indentation and the initial
unloading slope.
Indentation studies of quasicrystals

Quasicrystalline phases (QC) of either icosahedral or
decagonal symmetry share an homologous brittle-to-
ductile transition temperature (BDT) of T/Tm,0.7 (Tm
melting temperature) (Bresson, 1994) with the majority
of crystalline intermetallic compounds (Fleischer, 1994;
Sauthoff, 1995). This suggests that diffusion processes
are strongly involved in plastic deformation. It also
means that nucleation and movement of cracks should
become a predominant mechanism in most of the QC
phases when subjected to shear stress at room tempera-
ture. However, due to the small ratio of indent-
to-sample diameter, indentation experiments are in
fact performed under confining pressure conditions. It
16 Relationship between hf5hm and H5E* (after Cheng has been known for a long time that confining pres-
et al., 2002) sure techniques, where uniaxial stress states are

superimposed by hydrostatic pressure, may well shift niobium (185.7 GPa or 104.9 GPa, Brandes and Brook,
the BDT of crystalline materials down to even room 1992). Apart from the small effect in d-Al–Cu–Co–Si, no
temperature by suppressing crack growth (e.g. Castaing pronounced elastic anisotropy has been found in any of
et al., 1981; Francois et al., 1988; Androussi et al., the QC investigated in agreement with the conclusions
1989). Indeed, this principle also seems to work of Chernikov et al. (1998), Reynolds et al. (1990) and
with QC. Recently, a permanent macroscopic plastic Spoor and Maynard (2001). Note that Er increases when
strain of almost 20% has been achieved by Fikar the contact depth hc approaches the surface region
et al. (2001) after deformation of poly-quasicrystalline (Fig. 18). It becomes fairly constant for contact depths
i-Al63.5Cu24.0Fe12.5 under isostatic pressure of 5 GPa .200 nm. This obvious surface influence may arise
and at a strain rate of 5?10 s21 at 300 K. Importantly, from intrinsic as well as from extrinsic causes and is still
their TEM investigation of the microstructure did not not understood. Future databases will have to consider
reveal significant differences between room temperature/ that.
high confining pressure and high temperature/low
confining pressure specimens. The microstructure was Hardness: indentation depth
rather found to be characterised by either a tweed
Despite its physical foundation, Meyer hardness H is not
like or a platelet like contrast and isolated dislocations.
a simple material property. Figure 19 displays values for
The platelets could be shown to correspond to two
H(F) over four orders of magnitude of the load F, which
pentagonal approximant phases (Fikar et al., 2001).
show that hardness more than doubles when lowering
Indication for phase transitions as the vehicle of
the load by a factor of 10. Though this phenomenon has
permanent deformation at room temperature were also
principally been known for quite a long time (cf. Mott,
reported by other workers: For example, Wu et al.
1956), hardness numbers are even today taken as
(2000) and Dong et al. (2001) found a transition in

characteristic of the material, at least when specifying
i-Al62Cu25.5Fe12.5 to a bcc structure in the region
the (large) load and the shape of the indenter applied.
below scratches, whereas Kang and Dubois (1992a)
Despite the problems connected with the significance of
observed transitions under uniaxial compression of
hardness values as a material property, the more
i-Al63.5Cu24.5Fe12 and d-Al63Cu17.5Co17.5Si2.
pragmatic view is taken to use hardness as a quantity
Another mechanism of plastic deformation at room
for comparison and as a feature which – at sufficiently
temperature has been proposed by Wollgarten and Saka
low loads – will enable elementary processes of plastic
(1997) and Wollgarten et al. (1999). Examining the area
deformation to be detected. For the sake of comparison
below a Vickers indent in i-AlPdMn by TEM, they
with other data, microhardness results will first be
concluded, contrary to Fikar et al. (2001), that a poly-
presented (load 1 N) along with nanohardness data
grained material with grain sizes starting from 10 nm up
(load 0.1 mN) in Table 5. Al-based QC proved harder
to 500 nm had been formed and deformation occurred
than Zn-based. The nanohardness is considerably higher
via grain boundary sliding. At about 200uC, dislocation
than the microhardness (see below). Anisotropies are
generation was found. However, the mechanism of this
generally small, but reproducible. Unresolved systematic
fragmentation process was not specified.
deviations seem to prevent results of different authors
from coincidence.
Elastic properties The increase in hardness for FR0 or hR0 has become
The reduced modulus Er has been derived for various known as a (positive) indentation size effect (ISE) (cf.
QCs from a number of indentation tests using the Fig. 19). It has been reported to occur in a wide range of
nanoindenter (Table 4). Examples of corresponding F(h) materials (e.g. Si, TiB2 (Brookes, 1983), MgO (Ren et al.,
curves are displayed in Fig. 17. Aluminium-based alloys 2002), Al (Atkinson, 1995a,b) and has been attributed to
exhibit higher moduli than others. The surprisingly several mechanisms such as, e.g. elastic recovery (Mott,
small modulus of dodecagonal Nb–Ta–Te is of the same 1956), indenter–specimen friction (Li et al., 1993) or
order of magnitude as elemental tellurium (47.1 GPa, geometrically necessary dislocations (Fleck et al., 1994).
Brandes and Brook, 1992) rather than of tantalum or ISE and its RISE are discussed in more detail. The latter
Table 4 Reduced modulus Er at 300 K as derived from indentation experiments on surfaces with normal parallel to
rotation axes indicated
QC Er, GPa* E, GPa
d-Al–Co–Cu–Si 164¡15 {10} 87 (poly QC) (Kang and Dubois, 1992b)

175¡15 {2}
d-Al–Co–Ni 195¡15 {2} 195 (Chernikov et al., 1998), 177 {10} (Li et al., 2004)
i-Al–Cu–Fe (poly QC) 180¡20 172 (Vanderwal et al., 1992), 168 (Tanaka et al., 1996),
140.2 (Fleury et al., 2001), 131 (Lee et al., 2001), 61268 (Kang and Dubois, 1992b)
i-Al–Mn–Pd 190¡12 {5} 182 (Tanaka et al., 1996)
200 (Yokoyama et al., 1993)
i-Dy–Mg–Zn 128¡15 {5}
i-Ho–Mg–Zn 136¡15 {5}
i-Mg–Y–Zn 125¡15 {5} 62 (Edagawa et al., 1998)
126 (Sterzel et al., 2000)
dd-Nb–Ta–Te 35¡10
*Paufler and Wolf (2003).
{2}, {5} {10}, surface normal || to two-, five- or 10-fold symmetry axis.

17 F(h) curves obtained with Berkovich indenter for QC based on Mg–Zn with Y or rare-earths as third component; sur-
face normal fivefold; reduced Young’s moduli were derived from the unloading parts (after Paufler and Wolf, 2003)
model leads to the following form of the depth the testing conditions. Equation (43) may be rewritten
dependence of hardness H as
sffiffiffiffiffiffiffiffiffiffiffiffiffi
h H~½H02 z(40:5ba2 tan2 qG 2 =hc )1=2 (44)
H~H0 1z (43)
hc From measurements of H(hc), parameters of equa-
1/2 tion (44) may be obtained. Fitting contact depths in the
where hc is the contact depth, H05H(hcR‘)527 Gba
range 100 nm,hc,250 nm to equation (44), Paufler and
(rs)1/2 and h*5(81/2)b a2 tan2 q (G/H0)2, G is the shear
Wolf (2003) found H0511.3 GPa and h*540.8 nm for
modulus, b the Burgers vector modulus, rs density of
unimplanted d-AlCoNi (Fig. 20). If b5b||50.377 nm
statistically stored dislocations, q the angle between the
(Yan et al., 1994; Kupsch et al., 2001), then a shear
surface of the indenter and the surface of the specimen, a
modulus G547.8 GPa results (with a50.5 and q537.7u).
constant <0.5, and h* the length that characterises the
These values are consistent with those known from other
depth dependence of the hardness (Nix and Gao, 1998).
authors. The model of geometrically necessary disloca-
There is certainly a lower boundary of validity of
tions fits well for contact depths hc.h*. At smaller hc
equation (43) due to the atomic structure, i.e. hc.1 nm.
values (i.e. higher dislocation densities), H increases more
An upper limit for hc will be due to the formation of
slowly than predicted, contrary to metals (Lorenz, 2001).
cracks, etc., hence dependent on both the material and
Here, the validity of the Taylor model may become
questionable apart from probable surface influences.
19 Meyer hardness versus load (indentation size effect ISE)

18 Reduced Young’s modulus of dodecagonal for i-Al70 Pd21Mn9 and i-Y10Mg30Zn60 at room tempera-
(Nb0.15Ta0.85)181Te112 at room temperature as a func- ture as derived from Vickers (F.10 mN) and Berkovich
tion of contact depth hc; different point sets corre- (F,10 mN) indentation tests; sample surface perpendi-
spond to different sites (after Paufler and Wolf, 2003) cular to fivefold symmetry axis (Wolf et al., 2001)

20 Hardness H versus contact depth hc for d-AlCoNi at

room temperature; squares: experimental data (after 21 Hardness H versus contact depth hc for unimplanted and
Paufler and Wolf, 2003);solid line: model according to for implanted i-HoMgZn (after Paufler and Wolf, 2003)
Fleck et al. (1994)
According to Fig. 23, the change of almost four orders
Hardness H versus contact depth hc for unimplanted and of magnitude in t leads to a decrease of only 10% in H.
for implanted i-HoMgZn (Fig. 21) and dodecagonal (dd) Hence the contact area approaches its equilibrium value
NbTaTe (Fig. 22) showed similar behaviour. pretty rapidly, i.e. the dominating deformation does not
Time dependence require much time.
To assess the influence of loading time t upon the
hardness H, measurements were performed with i- Effect of implantation
YMgZn varying t in the range 261022–102 s by a pulse Specimens of i-Al–Pd–Mn, i-HoMgZn and d-Al–Co–Ni
indentation method (see Golovin et al., 2002). have been implanted using Bz ions (ion dose 1016 cm22,
Table 5 Hardness at room temperature
QC HMeyer, GPa* HV, GPa{ HMeyer, GPa{
d-AlCoCu 10.17¡0.30 (Murthy et al., 1999)

d-AlCoCuSi 9.7¡0.3 {2} (Paufler and Wolf, 2003) 8.1¡0.4 (polyQC) (Kang and Dubois, 16.8¡1.2 {2} (Wolf and
1992b) Paufler, 1999b)
10.2¡0.4 {10} (Paufler and Wolf, 2003) 7.82¡0.10 {10} (Mukhopadhyay et al., 14.6¡1.5 {10} (Wolf and
2001) Paufler, 1999b)
9.6 (Wittmann et al., 1991)
d-AlCoNi 10.9¡0.3 (Paufler and Wolf, 2003) 8.7 {10}, 9.4 {2} (Takeuchi et al., 1991) 11.4 {10} (Li et al., 2004)
8.64¡0.28 {10} (Liu et al., 2003)
d-AlCrCuFe 8.3¡0.7 (Michel, 1992)
i-AlCuFe 7.85¡0.60 (Giacometti et al., 1999)
9.8¡1.0 (Köster et al., 1993)
7.0¡0.4 (Kang and Dubois, 1992b)
i-AlCuLi 5.1 (Takeuchi et al., 1991)
3.82¡0.16 (Bhaduri Sekhar, 1987)
4.10¡0.15 (Sainfort and Dubost, 1988)
R-AlCuLi 4.8 (Takeuchi et al., 1991)
i-AlCuRu (poly-QC) 10.5 (Takeuchi et al., 1991)
i-AlPdMn 9.3¡0.3 (Paufler and Wolf, 2003) 8.4¡0.4 {5} (Deus et al., 1997) 21.6¡2.0 (Wolf and Paufler,
1999b)
8.2¡0.3 {2} (Deus et al., 1997)
6.9 {2}, 7.1 {5} (Yokoyama et al., 1993)
8.0 {3} (Yokoyama et al., 1993)
(poly-QC) 9.3 (Takeuchi et al., 1991)
5.94¡0.02 (Wollgarten and Saka, 1997)
i-YMgZn 5.7¡0.2 (Paufler and Wolf, 2003) 4.3 (Edagawa et al., 1998) 12.3¡1.2 {2} (Wolf and Paufler,
1999b)
i-DyMgZn 6.6¡0.2 (Paufler and Wolf, 2003)
i-HoMgZn 5.4¡0.2 (Paufler and Wolf, 2003)
Al73Co27 10.5¡0.3 (Paufler and Wolf, 2003)
Al3Co 9.0¡0.3 (Paufler and Wolf, 2003)
*Meyer hardness from microhardness. Load 1 N.
{
Microhardness, various loads of the order of 1 N.
{
Meyer hardness deduced from nanohardness data using a corner-of-a-cube indenter. Load 0.1 mN.
{2},{3], {5},{10}5surface of two-, three-, five- or 10-fold symmetry.

22 Hardness H versus contact depth hc for dd-NbTaTe;

24 Comparison of multi-indentation force–displacement
different point sets correspond to different sites
curves (Berkovich indenter) for unimplanted and B
along the surface (after Paufler and Wolf, 2003)
implanted i-HoMgZn (fivefold surface); six unloading/
reloading cycles have been performed for the same
ion energy 180 keV). This treatment is known to give indent before final unloading was done; staircase like
rise to atomic disorder. Measurements by these authors
multiple pop-ins were often found in QC (after Paufler

showed that the hardness of all QC investigated at room and Wolf, 2003)
temperature decreased due to irradiation. This is similar
to the observations of Burnett and Page (1984) with Si.
Pop-in
According to Monte-Carlo simulation, the maximum
penetration depth of Bz ions is 500 nm for i-Al–Pd–Mn Looking more closely at Fig. 17, sudden displacement
and 600 nm for i-HoMgZn (Paufler and Wolf, 2003). discontinuities during loading can be observed. One in i-
Thus the indentation depth was well below the range of HoMgZn is more pronounced at about 2200 N, others
implantation. Figure 24 shows the impact of implanta- are less well developed. This phenomenon, now known
tion upon the F(h) curve of i-HoMgZn. The indenter as a ‘pop-in’ event, has been found in various crystalline
penetrated deeper into the implanted QC, i.e. the materials and was attributed to the nucleation of
dislocation loops or cracks or to phase transitions under
hardness decreased. For hardness values, see Fig. 21.
the indentation stress (cf., e.g. Page et al., 1992). ‘Pop-
Moreover, the ISE practically vanished. The latter result
ins’ were observed in QC for the first time by Wolf et al.
resembles the absence of ISE due to the free volume
(2001). Unloading/reloading cycles were performed
effect in amorphous materials which facilitates atomic
(Fig. 26) to check the first appearance of inelastic
transport. Also, the crack formation probability near
deformation.
indents was found to be reduced and pile-ups were
Hardness decreased due to ion implantation, however,
found to be less pronounced (Fig. 25), i.e. decreasing
pop-ins continued to occur. Having undertaken pure
hardness seems to be accompanied by increasing
elastic cycles, a further increase in load initiated the first
toughness.
pop-in indicating the transition to an inelastic deforma-
tion mode (cf. Fig. 27). As the penetration depth was
increasing discontinuously, the contact pressure pm
(hardness) decreased in the same way (for quantitative
details cf. Fig. 27). The sharper the indenter, the deeper
was the pop-in. Figure 28 illustrates a typical series of
25 Comparison of Berkovich indents at room tempera-

23 Dependence of hardness H of i-YMgZn on the loading ture in i-AlPdMn implanted (left) and unimplanted
time t using a Berkovich indenter (load 40 mN); H is (right); surface normal of fivefold symmetry; lateral
the ‘universal hardness’, which includes elastic defor- scan width 4 mm; height scale 200 nm; no cracks
mation; thus, H values are about 20% smaller than could be observed near the left indent and pile-ups
the Meyer nanohardness used elsewhere in this work were found to be less pronounced (after Paufler and
(after Paufler and Wolf, 2003) Wolf, 2003)

26 Load–displacement curve of a multi-indentation test 28 Load–displacement curve for i-Y–Mg–Zn, when a

on a fivefold surface of i-Y–Mg–Zn using a sphero- cube-corner indenter is used; a series of pop-in
cone indenter; loading/unloading/reloading cycles events has developed with increasing load (after
with increasing maximum force lead to the occur- Paufler and Wolf, 2003)
rence of pop-ins and, simultaneously, inelastic hys-
teresis (after Paufler and Wolf, 2003) Influence of temperature
Measurements of microhardness of d-AlCoNi, d-

pop-ins, when a cube corner was used. Figure 29
AlCuCoSi and i-AlPdMn as a function of temperature
indicates the corresponding pressure drops versus
have been performed up to <800 K (Fig. 30). Hardness
contact depth. While the force was increasing, the
H decreased with increasing temperature T in two stages
contact pressure decreased (i.e. the contact area
similar to the hardness and yield stress of many
increased) during loading. Drops per pop-in amounted
crystalline intermetallic compounds (Kirsten et al.,
typically to 1 GPa.
1964; Schulze and Paufler, 1972). Obviously, two
Adopting the model of dislocation nucleation and/or distinct mechanisms predominate at lower (l) and higher
motion facilitated by hydrostatic stress, it is concluded (h) temperatures. The transition in H(T) occurs at
that the first pop-in corresponds to the maximum shear homologous temperatures (T/Tm)0<0.6 (Wolf and
stress to activate slip. It is approximately given by the Paufler, 1999a,b, 2001). Assuming thermally activated
Tresca stress (Johnson, 1996) tTresca50.46pm, which is processes below and above (T/Tm)0, the ratio of slopes
<5.8 GPa for i-YMgZn at room temperature. As a [dH/dT]l/[dH/dT]h gives an indication of the ratio of
result of the absence of strain hardening (at elevated activation volumes v. For i-AlPdMn, it was found that
temperature) (cf. Brunner et al., 2000; Urban et al., [dH/dT]l/[dH/dT]h5vh/vl<0.12. If the low temperature
1999, 2002), subsequent bunches of dislocations can be process was governed by a cluster friction mechanism
activated at lower shear stress. One of the consequences and the high temperature process by recovery-controlled
of dislocation movement could be deformation by deformation (Messerschmidt et al., 2000), then a factor
twinning, martensitic or related phase transitions to of 10 in the activation volumes seems reasonable.
meet the demands of volume change, as observed by Uniaxial macroscopic deformation experiments on d-
Fikar et al. (2001). AlCoNi (Feuerbacher et al., 1997) and i-AlPdMn (Geyer
et al., 2000) without hydrostatic pressure, however, have
not yet been done at T/Tm(0.7.
27 Contact pressure pm5F/Ac versus contact depth hc

derived from Fig. 26 near first pop-in; note that
hc,total displacement; as a result of the pop-in, pres-
sure drops from 13 to 8 GPa (after Paufler and Wolf, 29 Contact pressure versus contact depth calculated
2003) from Fig. 28 (after Paufler and Wolf, 2003)

et al. (1997, 2000) and Wolf and Paufler (1999b,c).

Moreover, while the surface near an indent on an
icosahedral QC showed typical pie chart like pile-ups, it
was found rather smooth on decagonal QC. In the case
of microhardness indents, the apparent volume of the
piled-up elevations was about 30–40% larger than the
volume of the impression. This is obviously due to
lateral cracking and subsurface defect formation.
Contrary to that, the volume balance for spherical
indentation under the same conditions proved negative,
i.e. about 70% of the displaced material was ‘missing’
(Wolf et al., 2000). There is evidence for long-range
transport of matter from the indent towards the outer
regions thus elevating the overall surface level of the
impression environment and making precise AFM
topology difficult. A proof of the conservation of
30 Meyer hardness versus temperature of d-Al73Co13Ni14 volume after plastic deformation, however, could not
and i-Al70Pd21Mn9 between room temperature and yet be given. Violations, if any, might be due to phase
600uC (load F51 N) as derived from Vickers tests transitions. It is interesting to point out that Reibold
(surface orientation in parentheses) (after Paufler and et al. (2005) have demonstrated the existence of
Wolf, 2003) nanocrystals near the nanoindent through high resolu-
tion electron microscopy. Mukhopadhyay et al. (2006a)
Crack formation have discussed that in the absence of active dislocations

When indented by a microhardness tester at room in quasicrystals, the plasticity during nanoindentation
temperature, most quasicrystals, like other brittle can be related to the nucleation and growth of shear
materials, develop cracks starting at the corners of the bands (i.e. localised deformation) which is observed in
impression pyramid. A statistical analysis of crack AFM images as well as reflected in a load–displacement
directions near indents on surfaces of both two- and diagram in the form of discontinuities (i.e. pop-in effect).
fivefold rotational symmetry of Al70Pd23Mn7 revealed Thus it is reasonable to argue that deformation during
that cracks exhibit a shear like habit and prefer an room temperature nanoindentation proceeds via shear
overall propagation along planes of two-, three- and band formation and subsequent phase transformation.
fivefold symmetry rather than following the plane of However, more detailed studies in this direction are
maximum stress (Deus et al., 1997). However, looking required to understand this aspect from the stability and
more closely at the crack paths, meandering phenomena crystallography of this complex structure.
appeared (Wolf and Paufler, 1999a). They are particu-
larly frequent in the case of cracks with cleavage planes Bulk metallic glasses
of twofold symmetry perpendicular to the surface. Their Indentation techniques have been employed to deter-
propagation direction suddenly changed after typical mine the mechanical properties of thin ribbons of
lengths of 50–100 nm. The angular alteration proved to metallic glasses (Sargent and Donovan, 1982). Now a
be a multiple of 72u thus permitting to continue new generation of metallic glasses unlike thin ribbons
propagation along a plane of the same symmetry can be fabricated in bulk form by conventional foundry
(Wolf et al., 1997; Wolf and Paufler, 1999b). Smaller practices (Inoue, 2000; Johnson, 2002). Extensive
lateral changes in the order of 1 nm could not be indentation studies on various types of bulk metallic
excluded due to the limited resolving power of the glasses (BMG) have been pursued in order to explore
method. The rough appearance of cleavage planes has their structural applications. Like crystalline materials,
been predicted in principle by Trebin (1999) from two- the constraint factor for correlating hardness with yield
dimensional numerical simulations. They showed that stress also seems to be interesting in the case of BMG.
cracks can propagate by emitting dislocations which The applicability of the Mohr–Coulomb versus the von
leave a phason wall of reduced surface energy in their Mises criteria for plastic deformation during indenta-
trail. This trail avoids structural clusters. tion is discussed by several workers. In the load–
The occurrence of Palmquist type microcracks at the displacement indentation curve, many interesting
corners of microindents has been used to evaluate the features in the form of serrations, ripples, displacement
mode I critical stress intensity factor (fracture tough- bursts, discontinuities, pop-ins (all these features are
ness) of i-AlPdMn. The value KIc51.26 MPa m1/2 (Deus identical but differ in terms of scaling) have been
et al., 1997) is an order of magnitude smaller than that of reported. The importance of shear bands for plastic
conventional aluminium alloys (e.g. KIc517 MPa m1/2 deformation are emphasised. Several studies also indi-
for Al–Li–Cu–Mg–Zr (Brandes and Brook, 1992), but cate the possibility of phase transformation during
comparable to other crystalline intermetallic and indentation.
quasicrystalline phases such as, e.g. KIc51 MPa m1/2 Recently, Schuh and Nieh (2004) have surveyed the
(Wittmann et al., 1991) and 1.4¡0.1 (Mukhopadhyay indentation tests on bulk metallic glasses and reported
et al., 2001) for d-AlCuCoSi; KIc51.01¡0.09 MPa m1/2 on the hardness measurements as well as the onset of
(Liu et al., 2003), 0.80¡0.08 MPa m1/2 (Murthy et al., plasticity, the role of shear banding, structural changes
1999) and 0.81 MPa m1/2 (Li et al., 2004) for d-AlCoNi. beneath the indenter and the rate dependent effects
A strong influence of surface symmetry upon the measured by nanoindentation. It has been reported that
morphology of impressions has been reported by Wolf yield strength Wy can be approximated following Tabor’s

32 Comparison of theoretical and experimental data from

the work of Vaidyanathan et al. (2001) for Berkovich

indentation on Zr-based bulk metallic glass; experi-
31 Plot of hardness and yield stress for various types of mental data are found to agree well with those calcu-
metallic glasses; most of the data can be seen to lie lated by the Mohr–Coulomb yield criterion (after
closely near the slope K53, though some theoretical Schuh and Nieh, 2004)
values of K are somewhat lower than the trend; data
from various metallic glasses are compiled and
where B, N1, N2 are numerical constants, and Er is the
plotted by Schuh and Nieh (2004)
reduced modulus. It appears that, for metallic glasses,
Er/Wy can be approximated to 45. Setting N1 and N2
relation (Tabor, 1986) equal to 9.4509 and 21.2433, respectively, B can be
H~Ksy (45) obtained as 24.5. Considering all constants of equa-
tion (47) and comparing with equation (45), the value of
where K is dependent on the indenter shape as well as on K is obtained as 2.1, which is a lower bound of the
the mechanical properties of the material being experimental data. It is observed from experimental and
indented, especially on the strain hardening character- various theoretical work that the constraint factor is
istics. The value of K is found to be close to 3 in most of lower than the value for crystalline material. Therefore
the amorphous materials including glassy materials and the material is harder than the crystalline material with
bulk metallic glasses (Fig. 31). From Fig. 31, a simple the same yield strength. The reason has been argued on
linear relationship can be justified, though there is a the basis that the glassy material is pressure-sensitive
scatter which needs to be understood from the and the normal stress on a shear plane plays an
mechanics of plastic deformation of glassy materials. It important role, and it delays the yielding which causes
can be mentioned that metallic glasses are non-strain the shallower indentation compared to that predicted by
hardenable materials and therefore they can be regarded the von Mises criterion. Therefore the Mohr–Coulomb
as rigid perfectly plastic material. The slip-line field criterion appears to be more applicable for the glassy
theory applicable for perfectly rigid plastic material material. This can be expressed as
suggests a simple relation between hardness and yield
ty ~k{asn (48)
strength. The experimental results shown in Fig. 31 are
based on the Vickers or Berkovich indenters, and the where ty is the shear stress on the slip plane at yield, sn is
relevant numerical slip-line field analysis for various the normal stress acting on the shear plane and k and a
conical indenter can be expressed as (Lockett, 1963). are system-specific constants that define the shear
sy strength and the atomistic ‘friction coefficient’ of the
H~ pffiffiffi ð1:41z2:72hÞ (46) glass, respectively. Vaidyanathan et al. (2001) performed
3
the simulations run for the von Mises and Mohr–
where h is the half angle of the cone-shaped indenter in Coulomb criteria and showed the comparison with the
radians. Introducing the value of 2570u for Vickers or experimental data (Fig. 32). It is clear from this work
Berkovich indenters in equation (2) and comparing with that the von Mises criterion predicts greater depth at a
equation (45), the value K52.7 is obtained which is particular load whereas the Mohr–Coulomb criterion
close to the empirical value 3. Dao et al. (2001) have predicts a lower depth which agrees well with the
considered this problem in much more detail using experimental data with a50.13. Though these results are
finite element simulations and obtained the following supporting the Mohr–Coulomb criterion, still more
relationship studies are required in this direction. Recently,
Ramamurty and co-workers (Patnaik et al., 2004; Jana
2N1 Er et al., 2004a,b; Ramamurty et al., 2005) have studied the
H~ sy N2 z ln (47)
B sy deformation characteristics and recognised with the help

33 Example of indentation loading (P–h) curves for a

variety of metallic glasses illustrating that discrete

pop-ins or flow serrations are common to many
amorphous alloys; origin of each curve has been off-
set for clarity, and several pop-in events have been
denoted by arrowheads (after Schuh and Nieh, 2004) a As-cast alloy subjected to indentation load of 2500 g;
b As cast alloy subjected to indentation load of 2000 g,
of their experimental evidence that the von Mises exhibiting semi-circular shear band morphology
criterion is inappropriate for metallic glasses even 34 Morphology of subsurface deformation zones under-
though some earlier reports supported this model neath Vickers indenter (after Jana et al., 2004a)
(Kimura and Masumoto, 1983; Bruck et al., 1994). It
has been suggested that a Mohr–Coulomb type criterion followed by rapid propagation of these bands and
which takes into account the normal stress across the catastrophic fracture. It is known that in compression
slip plane in addition to the local shear stress is better tests, the BMGs exhibit essentially no strain hardening,
suited. They have attributed this aspect to the high and plastic flow is serrated, with many small load drops.
constraint factor of metallic glasses such as Zr-based Figure 34 shows the formation of shear bands which are
glass. They have also extended the expansion cavity commonly observed on the surface and beneath the
model and found that this model agrees well with their surface while indenting bulk metallic glasses (Jana et al.,
FEM results. It is shown that the high plastic constraint 2004a). The nature of shear bands also depends on the
factor exhibited by metallic glasses at large indentation indentation rate, which can be clearly seen in Fig. 35
strains is an outcome of their pressure-sensitive plastic (Jiang and Atzmon, 2003). Wright et al. (2001) and
deformation. Golovin et al. (2001) used nanoindentation for the study
In metallic glasses, a few very small and isolated pop- of serrated flow in BMGs and observed discrete
in events were observed by Wang et al. (2000) in a Zr- displacement burst (‘pop-ins’) which they attributed to
based glass, after which the phenomenon was reported the emission of shear bands. It is also observed that a
in many other alloys (Golovin et al., 2001; Schuh et al., lower strain rate promotes more prominent serrations or
2002; Schuh and Nieh, 2003; Nieh et al., 2002; Greer displacement bursts. Chinh et al. (2004) observed the
et al., 2004; Greer and Walker, 2002; Wright et al., plastic instability as serrated flow in bulk metallic
2001). In all these alloys, the displacement bursts are glasses. They noted that the phenomenon is similar to
very small in the range of 1–25 nm and appear to occur that in crystalline alloys and manifested itself as discrete
with higher frequencies at a low indentation rate steps in the load–depth indentation curve (Schuh and
(Fig. 33). However, Vaidyanathan et al. (2001) did not Nieh, 2003; Dao et al., 2001; Vaidyanathan et al., 2001;
observe the displacement burst which could be due to Kim et al., 2002; Wright et al., 2001; Jiang and Atzmon,
the high loading rate during indentation. Various BMGs 2003; Benameur et al., 2002; Nieh et al., 2002; Golovin
such as Cu-based (Cu60Zr20Hf10Ti10), Zr-based et al., 2001). In crystalline solids, the physical basis for
(Zr65Al10Ni10Cu15), Pd-based (Pd40Ni10Cu30P20), the appearance of plastic instabilities is the negative
and La-based (La55Al25Cu10Ni5Co5) were studied strain rate sensitivity originating mainly from the
(Schuh and Nieh, 2003). interaction with the precipitates.
It is now understood that the plastic deformation of As loading rate is increased by several orders of
BMG is dependent upon structural dynamics. Homo- magnitude, the nature of serrated flow changes sub-
geneous and heterogeneous deformation have been stantially from step like P–h curves at the lowest rates, to
discussed in Zr and La based BMG in terms of the a very smooth parabolic curve at the highest rates
kinetic aspects of plastic deformation. Heterogeneous (Fig. 36). At rates in between these extremes, P–h curves
deformation (localised deformation) occurs at room exhibit serrations that appear more as fluctuations or
temperature by the formation of localised shear bands, ripples than as discrete, horizontal displacement bursts.

36 Indentation–depth load curve of a Pd–40Ni–20P

BMG measured at different loading rates (after Schuh
et al., 2002)
contrast, which may be due to the lower strain rate or to

hydrostatic pressure. Recently, Mukhopadhyay et al.
(2006b) showed the evolution of nanocrystals during
indentation of Cu-based metallic glasses. It was also
reported that the propensity of nanocrystallisation is
much more prominent near the indent region compared
to that of regions far from the indent. However, this
35 AFM illumination image of indents produced at pene- aspect of phase transformation from the kinetic point of
tration rates of a 100 nm s–1 and b 1 nm s–1 on amor- view for nucleation and growth of nanocrystals during
phous Al90Fe5Gd5 (after Jiang and Atzmon, 2003) the indentation period requires further theoretical and
experimental investigation.
During nanoindentation with a constant loading rate,
the displacement rate is a non-linear function of time t, Nanomaterials
as is the indentation strain rate defined by 1/h(dh/dt). At
Some interesting work on nanomaterials employing
the outset of each experiment, the strain rate is very high micro/nanoindentation techniques is discussed.
but decreases with depth as 1/h approaches an approxi- Attempts are not made to discuss nanostructured thin
mately constant value at very large depths. The trends in film studies, except to cite a few examples. Recently,
strain rate are not smooth and monotonic but exhibit Mirshams and Parakala (2004) reported nanoindenta-
many short peaks that appear to increase in size as the tion experiments on electrodeposited nanocrystalline
indentation proceeds. These short bursts of rapid (size ,19 nm) and commercially produced microcrystal-
displacement correspond to the pop-in events exhibited line (,21 mm) Ni with three geometrically different
in the P–h curve. Furthermore, the magnitude of the indenters. The highest value was obtained from the
peaks is strongly affected by the indentation strain rate. conical indenter and the lowest from the Berkovich
These effects are shown for other types of BMGs such as indenter. The hardness measurements obtained from
Zr-based and Pd-based systems. Berkovich and cube-corner indenters showed a good
Golovin et al. (2001) have earlier observed that correlation with the strain gradient plasticity model. The
localised (inhomogeneous) plastic flow of metallic ISE was found to be strongly dependent on the indenter
glasses can be accompanied by noticeable serrations in geometry and less on indentation depth. There was
the stress–strain curves. They have reported the results negligible strain rate dependence (within the range of
of nanoindentation tests of bulky glassy PdCuNiP. The 0.05–0.15 s21) of hardness to deeper depths and a
strain serrations of the indenter can occur both towards significant increase in the hardness due to the decrease
and against the applied force. It is known that in grain size. The hardness obtained by Berkovich and
nanocrystallisation can form in shear bands produced cube-corner indenters has been shown to justify the
during severe bending or high energy ball milling of thin mechanism based strain gradient plasticity approach.
ribbons of a metallic glass. Kim et al. (2002) have Their results also indicated that the microstructural
demonstrated experimentally that highly confined and length scale parameter is small in nanocrystalline
controlled local contact at the ultrafine scale in the form material and therefore the strain gradient length is
of quasi-static nanoindentation of a bulk glassy metal higher in nanocrystalline nickel to produce the same
alloy at room temperature can cause nanocrystallisation. stress in microcrystalline material. The present study
However, other studies did not show any phase suggested that a more detailed study is needed for the
transformation except for a subtle change in the TEM analysis of deformation mechanism for conical indenter.

38 Plot showing microhardness varying with load in

Mg32(AlZn)49 for a RSP foil; b as cast; variation of
hardness with load (indentation size effect) is greater
in RSP foils containing nanophase materials (after
Mukhopadhyay et al., 2004)
ductility has increased. The microhardness of nanoqua-

sicrystalline alloy shows several interesting features. The
average hardness of the alloy was found to be around
3.6 GPa. The absence of cracks around the indented
area suggests a superior toughness of the material. This
is further supported by the evolution of shear bands, a
signature of localised deformation. The hardness was
found to increase with load initially and then to
37 a Microindentation at 200 g; absence of cracks shows decrease. This may be due to the easy flow of materials
better toughness of material; b magnified image of in nanocrystalline/nanoquasicrystalline material by
shear bands developed during indentation; c SEM of grain boundary sliding or to phase transformation.
microindentation of microcrystalline version of Ti–Zr– Localised flow indicates the evolution of shear bands
Ni alloy, showing no shear bands (after Shaz et al., during indentation loading, analogous to deformation
2002) of metallic glasses (Sargent and Donovan, 1982).
However, this is an interesting feature and may require
Schwaiger et al. (2003) examined strain rate sensitivity in further study. Mukhopadhyay et al. (2004) have
a nanocrystalline Ni sample (grain size ,40 nm) using synthesised nanoquasicrystalline phases in the
the nanoindentation technique with different loading Mg32(AlZn)49 intermetallic alloy and compared the
rates and observed that nanocrystalline (nc) pure nickel microhardness data obtained from the nanoquasi-
was found to exhibit a positive strain-rate sensitivity in crystalline and microcrystalline phases of the same
flow stress, an effect that was not observed in ultrafine composition. The microhardness values of the nano-
crystalline (ufc) and microcrystalline (mc) nickel. This quasicrystalline phases are reported to be more than
rate sensitivity was confirmed by the depth sensing those of the microcrystalline phases. They found that the
nanoindentation and tensile testing. The strain rate indentation size effect is more prominent in nanophase
sensitivity was observed to be related to the grain size. material compared to that of microphase material
The indentation hardness at 1 mm depth increased from (Fig. 38). The propensity of cracking is also less in
5.7 GPa at a strain rate of 0.01 s–1 to 6.4 GPa at a strain nanomaterials.
rate of 0.1 s–1. A similar trend was observed at higher The applicability of the Hall–Petch equation to
loads: the hardness increased by almost 10% when the materials with grain sizes smaller than 1 mm is a
loading rate was increased from 3.8 to 186.1 mN s–1. question of significant technological importance in view
Shaz et al. (2002) have investigated the microhardness of the recent advances in materials processing techniques
measurement of Ti–Zr–Ni nanoquasicrystalline (40 nm) such as rapid solidification, vapour deposition and
materials. The indentation experiments were carried out sputtering, producing ultrafine grain sizes. Experi-
at 25, 50, 100 and 200 g load, which show the reverse mental studies have indicated that the refining of grain
indentation size unlike the micrometre size material. sizes to the nanometre scale can improve mechanical
SEM observation clearly brings out the presence of properties. For example, an increase from 0.9 GPa in
shear bands but no cracking was found (Fig. 37). As has the hardness of nickel was observed when the grain size
been shown earlier, microquasicrystalline and single was decreased from 12.5 mm to 12 nm (Hughes et al.,
quasicrystalline samples always show microcracking 1986). Similarly, an increase from 0.5 to 2.5 GPa was
(Murty et al., 1999; Mukhopadhyay et al., 2001). In achieved in nanocrystalline copper by reducing the grain
the present system, because of the formation of size from 50 mm to 6 nm (Nieman et al., 1989). The
nanoquasicrystalline phases, the hardness as well as observed increase in hardness with grain size which can

. .
39 Hardness versus grain size, d–0 5 for nanocrystalline 40 Hardness versus grain size, d–0 5 for nanocrystalline
Cu and Pd (after Chokshi et al., 1989) (Fe,Co)33Zr67 alloys (after Alves et al., 1996)
be explained by the Hall–Petch equation has also been and nanocrystalline TiSi2, nc-TiN/a-SiNx/a- and nc-
reported by other workers (Valiev et al., 1992; Jang and TiSi2 on steel substrate by the chemical vapour
Koch, 1999). An important aspect of strengthening by deposition (CVD) technique. The load independent
microstructural refinement is that the strength increase Vickers microhardness from 80 to .105 GPa was
need not be at the expense of ductility. However, it is measured by the load–depth sensing techniques for
also well documented in the literature that below a applied loads between 30 and 200 mN and verified by
certain grain size, the Hall–Petch slope may decrease measuring the size of the remaining plastic indentation
and even become negative (Fig. 39) (Chokshi et al., using SEM. It has been observed that the ultrahardness
1989; Lu et al., 1990; Fougere et al., 1992). The type of of 80–100 GPa depends on the amount of a- and nc-
processing method used for varying the grain size, such TiSi2 phases. Veprek (1999) has reported that when the
as heat treatment as well as the presence of imperfec- grain size decreases below 10 nm, the inverse Hall–Petch
tions such as triple junctions or porosity (Palumbo et al., relation is observed. It has been concluded that a high
1990; Wang et al., 1995) have been cited among the hardness with a high fracture toughness and elastic
possible causes for observed inverse Hall–Petch beha- recovery is a simple consequence of such nanostructure.
viour. Recently, Farhat et al. (1996) investigated hard- As pointed out by Koch and Narayan (2001), there
ness of nanocrystalline aluminium of various sizes are many problems associated with measurement of
ranging from 15 to 100 nm, using the ultra-microhard- hardness as a function of grain size for nanocrystalline
ness indenter and observed that the experimental data materials. If the grain size is varied by annealing the
are well represented by the Hall–Petch relationship. finest grain samples for grain growth, it is possible that
From the present study, it can be concluded that the other structural and/or compositional effects may occur
grain boundaries may be providing strengthening down on annealing. Most of the experiments that report the
to grain sizes as small as 15 nm. inverse Hall–Petch effect have samples which exhibit
clear artefacts or are at least questionable. However,
Nanophase TiAl, with grain sizes in the range of 10–
there are reports where no obvious artefacts or other
20 nm, was synthesised by magnetron sputtering in an
problems exist. They have identified at least three such
inert gas atmosphere and consolidated, in situ, under
apparently artefact free examples of the inverse Hall–
vacuum, and Vickers microindentation tests were
Petch effect in hardness tests (Figs. 40 and 41).
carried out by Chang et al. (1993). The Vickers micro-
Computer simulations also predict softening at grain
hardness of these samples at room temperature and at
sizes below some critical value. Both the simulations
230uC revealed an inverse Hall–Petch relationship at
show this critical grain size to be of the order of 10 nm
small grain sizes, 10–30 nm, and the usual Hall–Petch or smaller. While it has been difficult to assess the
behaviour at larger grain sizes. A small component of hardness of the smallest nanocrystalline samples unam-
indentation creep was also observed. The maximum biguously, it appears that the inverse Hall–Petch effect is
hardness is four times larger than that of a cast TiAl real. Models which describe the deformation of nanos-
specimen of the same composition. The Vickers hard- cale materials should use only the few experimental sets
ness was also observed to decrease rapidly with of data that are clearly artefact free to test their
temperature above 200uC. Schuh and Nieh (2003) have predictions (Fig. 42) (Koch and Narayan, 2001).
investigated the Hall–Petch breakdown regime by Obviously, many more investigations are required to
conducting hardness testing in nanocrystalline pure Ni establish the inverse Hall–Petch behaviour in nanocrys-
and Ni–W alloys. They observed the breakdown of the talline materials and its mechanism.
Hall–Petch relationship near d514 nm and d57 nm in
the case of nanocrystalline Ni and Ni–W alloy and
suggested a diffusional creep mechanism is responsible Phase transitions during hardness tests
for this inverse relationship. Early observations of morphologic features of scratches
Recently, Veprek et al. (2000) developed multiphase on glass by Klemm and Smekal (1941) led Madelung
nanocomposite coatings (3–20 mm thick) consisting of (1942) to conclude that local melting could arise due to
nanocrystalline TiN, amorphous Si3Ni4 and amorphous the highly localised introduction of mechanical energy

.
42 Hardness versus grain size, d–0 5 for nanocrystalline
Zn made by laser ablation or mechanical attrition
(after Koch and Narayan, 2001)
16.67 N s21, maximum loads 0.1–0.5 N) has been

detected by Clarke et al. (1988) using electron diffraction
.
and electrical conductivity measurements. The authors
41 Hardness versus grain size, d–0 5 for electrodeposited argued that remanent stresses inside the indented
Ni (after Erb, 1995) material give rise to this amorphous phase. After
scratching, a small amorphous region was developed

into the solid surface. Although first-order phase surrounded by a region of high dislocation density
transitions of this type will probably not occur during (Minowa and Sumino, 1992). Using a spherical indenter,
indentation at conventional speed, pressure-induced Williams et al. (1999) observed the transition of Si to a
structural phase transitions, which have become known ß-tin structure at about 13.3 GPa which compares
for numerous materials, should nevertheless play a role favourably with 12.5 GPa found under hydrostatic
in hardness tests, in particular when load–displacement pressure (Hu et al., 1986). It seems worth mentioning
curves are considered. In order to initiate a certain phase that transition pressures observed with indentation
transition, the (hydrostatic or deviatoric) pressure experiments are not to be equated with equilibrium
beneath the indenter should exceed the critical value pressures because of kinetic effects. They may be
for the phase transition but should not do so for the overestimated on increase in Si, for example, by a
spontaneous nucleation of dislocations in the parent minimum of 2 GPa (Hu et al., 1986).
phase. If the latter condition is violated, plastic strain Phase transformations alter the shape of the load–
will diminish the stress quickly below the critical value, penetration depth curve. They may show up in a ‘pop-in’
which in turn may be lowered under deviatoric stresses along the loading curve (Williams et al., 1999; Bradby
(Gilman, 1993). This implies that the presence of et al., 2000, 2001, 2003) and/or a ‘pop-out’ and/or an
dislocations and their ability to move under the stress ‘elbow’ (Page et al., 1992; Novikov et al., 1996; Williams
field of the indent will have an impact upon the et al., 1999; Domnich et al., 2000; Bradby et al., 2001,
occurrence of phase transitions, too. Since the hardness 2003; Zarudi et al., 2003; Ho et al., 2004) on the
is of the order of the average contact pressure beneath unloading branch. Whereas ‘pop-ins’ often also indicate
the indent, materials that undergo a phase transition the nucleation of dislocations (e.g. Lorenz, 2001; Lorenz
during indentation might be anticipated knowing their et al., 2003), ‘pop-outs’ and ‘elbows’ seem to be more
phase transition pressures. specific of a phase transition. They occur due to a
It is, therefore, not surprising that semiconductors sudden expansion of the volume, which has no counter-
were the materials where genuine phase transitions had part in plastic slip. Figure 43 gives an example indicat-
been directly observed for the first time. These solids ing that loading/unloading rates and maximum loads
exhibit both a very low initial dislocation density and a determine which of these features will appear.
high Peierls stress for moving dislocations. Indeed, Because of the small volumes involved with indentation,
Gridneva et al. (1972) concluded from an athermal various techniques have been applied to prove that a phase
region of the temperature dependence of hardness of Si transformation is correlated with those mechanical fea-
and Ge that a phase transformation had occurred, and tures. These are mainly transmission electron microscopy/
Eremenko and Nikitenko (1972) reported on the electron diffraction studies (Eremenko and Nikitenko,
formation of the high pressure phase VII in silicon 1972; Clarke et al., 1988; Wu et al., 1999; Bradby et al.,
when indented at temperatures of 400–700uC. According 2000, 2001; Mann et al., 2000, 2002; Ge et al., 2003; Zarudi
to Hu et al. (1986), this phase appeared under et al., 2003; Haberl et al., 2004), Raman microspectro-
hydrostatic pressures of 40 GPa. Comparing average metry (Kailer et al., 1997; Lucazeau and Abello, 1997;
pressures achieved during hardness measurements with Domnich et al., 2000; Bradby et al., 2001; Mann et al.,
phase transition pressures, Gerk and Tabor (1978) drew 2002; Ge et al., 2003; Zarudi et al., 2003), differential
the conclusion that a metallic phase of Ge, Si and scanning calorimetry (Riontino and Massazza, 2004),
diamond must have been formed beneath the indenter. acoustic emission (Mann et al., 2000) or electrical
A phase transition of single-crystalline Si and Ge resistance measurements (Clarke et al., 1988; Mann et al.,
through an electrically conducting state to a metastable 2000, 2002; Bradby et al., 2003; Ho et al., 2004).
amorphous phase after unloading Vickers and While silicon is by far the dominant goal of phase
Knoop indentations (loading-unloading rate transformation studies connected with indentation,

other authors reported on ‘pop-ins’ with quasicrystals

(Al–Cu–Fe: Dub et al., 2001, 2002; Ti–Zr–Ni: Azhazha
et al., 2004). Although the deformation behaviour of
quasicrystals is generally less well understood than that
of crystalline materials, there are direct and indirect
indications of phase transformations occurring in this
type of solid under localised load. The former refer to i-
Al–Cu–Fe, where a scratch-induced phase transition
from the quasicrystalline to a bcc phase was detected
using electron diffraction (Wu et al., 2000; Dong et al.,
2001). Nanocrystallisation in quasicrystals has been
reported by Reibold et al. (2005) while indenting the
Al–Ni–Co decagonal single quasicrystals. They found
that the phase transformation is quite likely due to the
volume reduction during this indentation. Phase trans-
formations of the martensitic type, giving rise to the
shape-memory effect, have been examined using both
spherical and pyramidal indenters. The deformation of
spherical indents (tip radius 213 mm, indents (8 mm) on
NiTi was almost completely reversed by heating (Ni
et al., 2002). At indentation depth less than 100 nm,
recovery was found to be almost complete (Shaw et al.,
2003).
Automated ball indentation (ABI) and

field indentation microprobe (FIM)
technique
The industrial applications of nanohardness measure-
ments were reviewed by Michler and Dommann (2001).
Here, in situ indentation techniques are discussed for
evaluating mechanical properties in order to assess the
degradation and hence the remaining life of high
temperature components in a thermal power plant, the
oil/gas industry, nuclear industry, aerospace and chemi-
cal industries. Monitoring the progressive changes in
mechanical properties has been mandatory from the
point of view of ensuring the structural integrity of the
components and safety of the operation. Therefore,
nondestructive methods for mechanical characterisation
are required for any materials aging and life manage-
ment programme.
A field indentation microprobe (FIM) apparatus was
developed and patented by Haggag and Nanstad (1989)
and Haggag et al. (1989, 1990) to evaluate nondestruc-
tively the mechanical properties. The FIM consists of
two main units: an automated ball indentation (ABI)
unit for measuring the mechanical properties and a
nondestructive evaluation (NDE) unit (consisting of
ultrasonic transducers and a video camera) for deter-
mining the physical properties such as crack size,
a ‘Pop-out’ appears in unloading curve at slower load- material pile-up around indentation, residual stress
ing/unloading rates (,1 mN s–1) and higher maximum presence and orientation. The main components of the
loads (50 mN); b ‘Elbow’ is formed at faster rates FIM apparatus are shown schematically in Fig. 44. The
(3 mN s–1) and lower loads (30 mN); c Mixed behaviour tripod arrangement adjusts the ball indenter to be
is also possible perpendicular to the surface of the structure or test
43 Impact of phase transitions upon shape of load– specimen. The load can be applied by hydraulic,
displacement curves as obtained by nanoindentation pneumatic, mechanical, or any other means. The ABI
of Si (after Domnich et al., 2000) test is based on multiple indentations (at the same
penetration location) of a polished metallic surface by a
other materials have been studied. ‘Pop-in’ and ‘elbow’ spherical indenter (in the order of 1 mm diameter). The
shaped parts of the load–penetration curve along with data are collected during the test and these are analysed
hysteresis have been observed with quasicrystalline automatically by the computer attached to the equip-
i-Y10Mg30Zn60 by Wolf and Paufler (2001), Wolf et al. ment. The applied loads and associated displacements
(2001) and Paufler and Wolf (2003) (Fig. 26). Also, (depth of penetration of the indenter into the test

45 Samples of ABI test results (load versus depth using

a 0.76 mm diameter ball indenter) on 316L stainless
steel (SS) base metal (after Haggag et al., 1989)
Zarzour et al. (1996) carried out microindentation

hardness tests on HY-100 weldments by automated ball
indentation on the weldments and obtained information
from the ABI tests in various regions of the heat affected

zone (HAZ). The results provide a relationship between
grain size and corresponding stress–strain data across
the HAZ. Byum et al. (1997) investigated the through-
the-thickness variations of mechanical properties in
SA508 Gr.3 pressure vessel steels using the automated
ball indentation (ABI) test technique and evaluated
mechanical properties, such as the yield strength,
ultimate strength, flow curve and hardness from
44 Schematic diagram showing basic components of indentation load–depth curves. Malow et al. (1998)
field indentation microprobe (FIM) apparatus (after conducted ABI tests on nanocrystalline (nc) iron which
Haggag et al., 1989) was produced by mechanical attrition and compacted
into near fully dense samples followed by isothermal
specimen) are measured using a load cell and a linear
annealing at 800 K resulting in grain sizes between 15
variable differential transducer (LVDT). The load
and 24 nm. The ABI method proved useful in examining
displacement data (Fig. 45) from each unloading
the mechanical properties of nc iron compared to that of
sequence are fitted with a first-degree polynomial and
conventional hardness testing methods. Stress–strain
the fit extrapolated to obtain the displacement corre-
curves were obtained which indicated a low strain
sponding to zero load. These displacements and the
hardening at high flow stresses around 3 GPa and a
maximum cycle load and displacement values from each
indentation sequence are used to determine the hardness room temperature strain-rate sensitivity. The deforma-
and yield strength, to produce the true-stress/true- tion pile-up around the indentations exhibited intense
plastic-strain curve, and to estimate fracture toughness. plastic deformation in localised shear bands.
The ABI analyses are based primarily on elasticity and Murty et al. (1998) investigated the tensile and
plasticity theories and some empirical correlations as fracture properties of ASTM grade A36 steel using a
described by Haggag and Nanstad (1989) and Haggag nondestructive Stress–Strain Microprobe system (SSM),
et al. (1989, 1990). The agreement between ABI-derived developed on the basis of automated ball indentation
data and those from standard ASTM uniaxial tensile (ABI) technique on as-received, and cold worked
and fracture toughness tests was demonstrated to be materials at several temperatures in the range and at a
satisfactory. The authors have suggested that this constant strain rate. From their study, they observed a
technique could also be extended for high temperature close agreement with the expected tensile and fracture
studies as well as indentation fatigue, fracture and creep. properties, and concluded that ABI is a reliable
The mechanical properties determined by the FIM nondestructive technique for determining tensile and
apparatus include elastic modulus, yield strength, fracture properties of materials. Murty et al. (1999) have
Lüders strain, strain-hardening exponent, Brinell hard- studied the gradients in mechanical and fracture proper-
ness, true-stress/true-plastic strain curve up to 20% ties of SA-533B steel welds using the ball indentation
strain, and presence of residual stress. The fracture technique. The local stress–strain behaviours of different
toughness is also estimated using the ABI measured flow microstructural zones of the weld were determined.
properties and a modified critical fracture strain model. Gradients in the strength of the base metal, weld metal
Furthermore, the shift in the ductile-to-brittle transition and the different positions in the heat affected zone were
temperature for steel plates and welds, for example, due observed to be consistent with the changes in the
to neutron irradiation embrittlement, can be estimated microstructure. Mathew et al. (1999) have carried out
from the ABI measured changes in the material’s yield ABI tests on service aged cast stainless steel components
strength and flow properties. and identified the embrittlement as well as increase in

strength and decrease in toughness due to aging. They the remaining life of components in service has proved
have further investigated the effect of aging on mechan- to be indispensable compared to other conventional
ical behaviour of Alloy 625 using the non-destructive techniques. However, semiempirical approaches for the
Stress–Strain Microprobe (SSM) system based on an assessment of brittleness need to be established on the
automated ball indentation (ABI) technique, and invol- basis of more fundamental analysis.
ving multiple indentations by a small spherical indenter
at a single penetration location under strain-controlled Acknowledgements
conditions and evaluated mechanical properties such as
yield strength, ultimate tensile strength, strength coeffi- The authors would like to thank Professors
cient and strain hardening exponent. These studies S. Ranganathan, P. Ramachandra Rao, S. Lele,
demonstrate that ABI can be used as a non-destructive K. Chattopadhyay, S.N. Ojha, G.V.S. Sastry,
technique to determine changes in mechanical properties U. Ramamurty, N. Chakraborty, I. Manna, B.S.
of nickel base alloy components due to aging. Seok and Murty, and Dr T. Sudarshan and Dr R.K. Mandal,
Murty (2000) using ABI tests have explained the Dr M. Chandrasekhar and Dr V.S. Sarma for their keen
decrease in fracture resistance (J–R) curves in SA516 interest and useful discussions. The authors would also
steel due to increased strain hardening and generation of like to thank Dr V.C. Srivastava, Mr G. Narayana,
tensile residual stress at the crack tip during cyclic Thakur Prasad, Sunil Pal, G. Subba Rao, André Belger
loading. Murty and Mathew (2004) have studied the for supplying useful references and stimulating discus-
applicability of an automated technique based on ball sions. One of the authors (NKM) thanks the Alexander
indentation for laboratory and field applications for von Humboldt Foundation, Germany, for a research
determining the mechanical and fracture properties of fellowship during which period a part of the work was
materials. Das et al. (2004, 2005a,b) have exploited this completed. Partial financial support from the
ball indentation technique extensively to study the Department of Science and Technology (DST), India
mechanical properties of many engineering and service is also gratefully acknowledged.
aged materials. They have observed that the pile-up
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Micro-And Nanoindentation Techniques For Mechanical Characterisation of Materials

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Micro- and nanoindentation techniques for

mechanical characterisation of materials

ß 2006 Institute of Materials, Minerals and Mining and ASM International

210 International Materials Reviews 2006 VOL 51 NO 4

Testing Shape of Shape of impression

Vickers 2F sin 680 1:8544F t<d/7

Knoop F 14:40F t<d/30.6

Ludwik 4F sin450 0:9F t5d/2

Grodzinski 6rF 0:9F t<d/80 for a5154u, r52 mm

International Materials Reviews 2006 VOL 51 NO 4 211

the indentation. Thus, Hmeyer5p. Knowing the geometry

212 International Materials Reviews 2006 VOL 51 NO 4

irrespective of the type of material. When n is equal to 2,

Nevertheless, it is convenient to handle the indentation

Minimum resistance model

International Materials Reviews 2006 VOL 51 NO 4 213

3 Correlation of power-law index n with hardness-

the effects of the indenter tip radius effect on the elastic

Proportional specimen resistance (PSR)

214 International Materials Reviews 2006 VOL 51 NO 4

International Materials Reviews 2006 VOL 51 NO 4 215

tion (17). After analysing their approach, it can be seen N

216 International Materials Reviews 2006 VOL 51 NO 4

deformation occurs progressively in a discrete manner to

combine with the stretching imposed by the sloping faces

International Materials Reviews 2006 VOL 51 NO 4 217

where d is the indentation diagonal, l1, K1 and K2 are

structure is idealised as circular dislocation loops;

218 International Materials Reviews 2006 VOL 51 NO 4

similar manner as the common statistically stored

For metals, the hardness is three times the flow stress, so

International Materials Reviews 2006 VOL 51 NO 4 219

220 International Materials Reviews 2006 VOL 51 NO 4

10 Stress–strain diagram for a perfectly plastic, b elastic–plastic, c real elastic–plastic solids

Therefore with increasing radii of the dislocation loops

International Materials Reviews 2006 VOL 51 NO 4 221

2=3 (1964), Hirst and Howse (1969) and Johnson (1970).

222 International Materials Reviews 2006 VOL 51 NO 4

International Materials Reviews 2006 VOL 51 NO 4 223

where d*55 for a Vickers pyramid indenter and

contribution from the complicated plastic/elastic surface

224 International Materials Reviews 2006 VOL 51 NO 4

Material Ho, kg mm22 d, mm q, kg mm22 n

Sapphire (1012) 2129 1.34 4265 1.81

Table 3 Density, elastic modulus and hardness parameters (Sakai, 1993)

Bulk density, True hardness Work of indentation Apparent hardness

Al 2.71 74.7 0.39 0.40 0.61 0.65

International Materials Reviews 2006 VOL 51 NO 4 225

15 Relationship between hf5hm and Wp5Wtot (after Cheng et al., 2002)

Indentation studies of quasicrystals

226 International Materials Reviews 2006 VOL 51 NO 4

(2000) and Dong et al. (2001) found a transition in

QC Er, GPa* E, GPa

d-Al–Co–Cu–Si 164¡15 {10} 87 (poly QC) (Kang and Dubois, 1992b)

International Materials Reviews 2006 VOL 51 NO 4 227

19 Meyer hardness versus load (indentation size effect ISE)

228 International Materials Reviews 2006 VOL 51 NO 4

20 Hardness H versus contact depth hc for d-AlCoNi at

QC HMeyer, GPa* HV, GPa{ HMeyer, GPa{

d-AlCoCu 10.17¡0.30 (Murthy et al., 1999)

International Materials Reviews 2006 VOL 51 NO 4 229

22 Hardness H versus contact depth hc for dd-NbTaTe;

2=3 (1964), Hirst and Howse (1969) and Johnson (1970).