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Micro-And Nanoindentation Techniques For Mechanical Characterisation of Materials
Micro-And Nanoindentation Techniques For Mechanical Characterisation of Materials
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.
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
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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
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
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Table 1 Geometrical shape of indenter and projected indentation along with hardness equation and penetration depths
displayed for various indenters
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
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;
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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
Published by Maney Publishing (c) IOM Communications Ltd
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
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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
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
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.
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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
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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
Table 2 Fitting parameters for observed scale dependence of hardness for various ceramic materials
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
Published by Maney Publishing (c) IOM Communications Ltd
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)
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.
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
Published by Maney Publishing (c) IOM Communications Ltd
Table 4 Reduced modulus Er at 300 K as derived from indentation experiments on surfaces with normal parallel to
rotation axes indicated
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.
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
et al., 2002)
. .
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
Published by Maney Publishing (c) IOM Communications Ltd
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)
2003).
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
Published by Maney Publishing (c) IOM Communications Ltd
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
around the indent is an important parameter. Based on References
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