Biomedical Engineering Reference
In-Depth Information
from the harmonic average of two tip geometries (conical and spherical)
and in which the only two parameters are the effective tip radius R and
the included cone angle
. Of course, this expression is less useful at
extremely small indentation depths since it gives A c ( h c )
0 at h c = 0, but
it is very effective in estimating a tip effective radius. Any area function
A c ( h c ) can be determined by solving the E R - S relationship ( Eq. 5-12 ) for
A c at each contact depth h c :
= h max − 0.75 P max
S
h c
(5-15)
The calibration is performed by assuming the fixed value of E R for
a material with known (and constant with depth) elastic modulus (and
thus reduced modulus). This calibration standard is typically the glass
fused silica (a.k.a. fused quartz) with an elastic modulus E = 72 GPa
and Poisson's ratio = 0.17 such that, with diamond ( E = 1.02 TPa and
= 0.07) the reduced modulus E R = 69.6 GPa.
In addition to the area function, there is an additional calibration-
derived quantity, the machine (frame) compliance. The measured
stiffness, S , is the series combination of the sample stiffness, S s , and the
frame compliance, S f , as:
1
S =
1
S s +
1
S f
(5-16)
The contact area ( A c ) and the frame compliance ( C f = S f -1 ) are related,
and the calibration protocol used to obtain these values has been
discussed at length in other sources 1 and in the manuals for commercial
nanoindentation instruments.
Once the full calibration (frame compliance and tip area function) is
known, the analysis of elastic-plastic DSI data using the Oliver-Pharr
protocol is straightforward. Three parameters are obtained directly from
raw P - h data, the peak load ( P max ), the peak displacement ( h max ) and the
unloading stiffness ( S = d P /d h ) as shown in Fig. 5-6 . The measured
stiffness S is corrected by Eq. 5-16 to obtain the sample stiffness and the
contact depth ( h c ) is computed from Eq. 5-15 . The corresponding contact
area A c ( h c ) is calculated from the area calibration ( Eq. 5-13 or 5-14 ) and
used to calculate properties of reduced modulus ( Eq. 5-12 ) and the
 
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