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Probing Linear viscoelasticity with micro-indentation
C.G.N. Pelletier, L.E. Govaert, J.M.J. den Toonder, H.E.H. Meijer
Eindhoven University of Technology, Department of Mechanical Engineering

Introduction where h(t) is the monitored displacement, R the tip radius, P 0
This study gives a quantitative comparison of the creep com- is the maximum applied load.
pliance and relaxation modulus obtained by indentation with
those obtained by conventional tests. For that, DMTA tests Indentation relaxation
were performed, and creep compliance and relaxation mod- A stepwise indentation depth is applied and the load is mon-
ulus were predicted from the master curves obtained using itored in function of time. From the experimental data we can
a generalized Maxwell approach. The samples investigated, calculate the relaxation modulus for ν =const [2]:
were two acrylate films with a glass transition temperature of
50◦ C and 80◦ C respectively. 2P (t)(1 − ν 2 )
E(t) = √ 3 (2)
8
3 Rh0
2
Soft Film Hard Film
1.0E+10 1 1.0E+10 1

1.0E+9 where P (t) is the load, h0 is the maximum applied displace-
tan(delta) [-]
1.0E+9
tan(delta) [-]

E', E" [Pa]
E', E" [Pa]

1.0E+8 0.1
ment, R the tip radius.
1.0E+8 0.1

E'
1.0E+7
E' 1.0E+7
E"

1.0E+6
E"
tan(delta)
0.01 1.0E+6
tan(delta)
0.01
Results
1.0E-9 1.0E-6 1.0E-3 1.0E+0 1.0E+3 1.0E+6 1.0E-10 1.0E-7 1.0E-4 1.0E-1 1.0E+2 1.0E+5 −8
Indentation Creep
10

Omega [rad/s] Omega [rad/s]

Figure 1a and b: DMTA master curves at 25 C for both films. ◦

D(t) [1/Pa]

Theoretical Background
−9
10

Creep compliance and relaxation modulus were calculated
°
from the experimental data using the correspondence prin- Soft film (Tg=50 C)
Hard film (T =80°C)
g
ciple [1]:
−10
10
Laplace Transform:
¥
10
1
10
2
10
3

Time [s]
L[ f (t )] = F ( s ) = ò f (t )e dt - st
Figure 2: Creep compliance obtained from indentation (open sym-
0
bols) compared with the prediction of creep compliance obtained
from modelling the DMTA master curve (solid line).
Linear Viscoelastic 10
Indentation relaxation
Elastic Regime 10
Regime
°
Soft film (Tg=50 C)
Hard film (T =80°C)
g

Inverse Laplace Transform:
s + j¥
1
E(t) [Pa]

2p j s -òj¥
L-1[ F ( s )] = f (t ) = F ( s )e ts ds 9
10

Experiments
Indentation tests were performed on the micro-indenter de-
signed by Philips, with a 300µm diameter spherical tip. 10
8

10
1 2
10 10
3

Load (P) Time [s]
Figure 3: Relaxation modulus obtained from indentation (open sym-
bols) compared with the prediction of relaxation modulus obtained
from modelling the DMTA master curve (solid line).
Displacement
(h)

Conclusions
Indentation creep For both creep and stress relaxation, the experimental data
A stepwise load is applied on the indenter and indentation obtained by micro-indentation compare well to the prediction
depth is monitored in function of time. From the experimen- based on the (macroscopic) DMTA master curves.
tal data we can calculate the creep compliance for ν =const
References:
[2]: [1] N.W. T SCHOEGL ,T HE PHENOMENOLOGICAL T HEORY OF LINEAR VISCOELASTIC
BEHAVIOR AN INTRODUCTION : Springer, Berlin, 1989
√ 3
8
Rh02 (t) 3 [2] J.M.J. DEN T OONDER , Y. R AMONE , A.R. VAN D IJKEN , J.G.J B EIJER , G.Q.
D(t) = (1) Z HANG .: proc. ESIME 2002, IEEE,2002,pp270-280
2P0 (1 − ν 2 )

/department of mechanical engineering PO Box 513, 5600 MB Eindhoven, the Netherlands