CSM Users Meeting 2012, 23-24 October, Gruyres, Switzerland

Hae-Jin Kim and Dae-Eun Kim

Center for Nano-Wear
School of Mechanical Engineering,
Yonsei University, Seoul, Korea
Considerations in Nanoindentation
Technique for Tribological
Applications
Contents
Introduction to Center for Nano-Wear (CNW)
Background
Issues in the field of tribology (Friction and wear)
Hardness measurement considerations
Proximity effect on mechanical properties of materials
Comparison of Continuous Multi-Cycle (CMC) and
individual indentation methods
Effect of penetration depth on thin film hardness
Modification of wear model
Conclusions
Key Issues in Tribology
Mechanisms of friction and wear
Surface coatings
Surface texturing/structuring
.
Friction and wear control
Precise measurement of
material properties
Tribological Interaction
Frictional
force
Asperity
Interlocking/
Abrasion
Capillary junction Delamination
crack propagation
Contamination
Oxide layer
Adhesion
Applied
force
L
F
=
0.001~1
10
3
x L
H V
k

=
10
-2
~10
-8
10
6
Wear Quantification of Si Bushing
Stiction reduction in micro-components (MEMS)
Fabrication of bushing by photolithography
Specimen dimension : 30.5 mm triangular shape
Dimple diameter : ~ 14 m, Weight : ~ 100 N
Bare Si wafer (100)
Chung et al., J. of Micromechanics and Micro-engineering, 2007
Wear of Si(100) Bushing on Bear Si(100)
Wear rate: ~ 0.0001 nm per cycle
Wear coefficient: 10
-7
~ 10
-8
Hardness is significant
in determining the
wear coefficient

Chung et al., J. of Micromechanics and Micro-engineering (2007)
VH
k
xL
=
V : Wear volume
H : Hardness
x : Total distance
L : Load
Archards wear model
0 10 20 30 40 50
0.0
0.1
0.2
0.3
0.4
Before test
After test


H
e
i
g
h
t

(

m
)
Scan length(m)
Plowing Friction Model
Lee et al., JMST, 2010
Horizontal force in
plowing model
f h
F H A =
A
h
: Horizontal
projected area
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4
-1.5
-1.0
-0.5
0.0
0.5
1.0


H
e
i
g
h
t

(

m
)
X axis (m)
6
0
.
0

n
m

4
2
m
m
4
2
5
3
1
1
3
6
5
6

L
n
Substrate
F
f
AFM diamond tip
scratch test
Is Hardness Constant? If not..
How does hardness vary between adjacent
points?
How does hardness vary with respect to depth?
How do we get hardness for thin films?
L
n
Substrate
F
f
Measurement Conventions
d

> 3 x D
d
h
h

< 0.1 x t
What happens if we dont ?
Device Specification
Ultra Nanoindentation Tester (UNHT)
Nano Scratch Tester (NST)






Follow ISO regarding surface roughness, substrate effect
Environmental conditions: ~20 C, 45% RH
Clean room (Class 100)
Maximum load 100 mN
Load resolution 0.001 N
Maximum depth 100 m
Depth resolution 0.001 nm
Proximity Effect
The distance between centers of adjacent
indentations should be at least three times the
diameter of indentation for error of 1% or less
Hardness Testing,
ASM International 1978
Appropriate distance between indents
~ diameter x 3 ~ (depth x 7) x 3
~ depth x 30 (30 times rule)
L
Berkovich
diamond tip
Scope of Proximity Effect
Assessment of proximity effect
Hard bulk material : Fused silica
Soft bulk material : Copper
Thin metallic film : Copper film (~600 nm)
Quantification of discrepancies between results

Simulation analysis
Investigate the stress distribution with finite
element method (FEM) simulation
H. J. Kim and D. E. Kim, Tribology Letters, 2012, in press
Properties of Fused Silica





R
a
: ~ 2 0.2 nm
Recommended P
d,max
: > 40 nm
Diameter of the indent : 1.5 m
(under 10 mN of normal load)
Recommended distance : > 4.5 m
Top surface
1 cm
0 50 100 150 200 250 300 350
0
2
4
6
8
10
N
o
r
m
a
l

f
o
r
c
e

(
m
N
)
Penetration depth (nm)
AFM image
Indents
P
max
> 40 nm
L

> 4.5 m
D
Proximity Effect of Fused Silica
0 100 200 300
0
2
4
6
8
10
N
o
r
m
a
l

f
o
r
c
e

(
m
N
)
Penetration depth (nm)
0 100 200 300
0
2
4
6
8
10
N
o
r
m
a
l

f
o
r
c
e

(
m
N
)
Penetration depth (nm)
Hardness
9.9 0.12 GPa
Hardness
10.1 0.14 GPa
2 %
4.5 m
1.5 m
1. Reference set 2. Test set
Properties of Bulk Copper






R
a
: ~ 6.5 1.5 nm
Recommended P
d,max
: > 130 nm
Diameter of the indent : 4 m
(under 10 mN of normal load)
Recommended distance : > 12 m
Top surface
1 cm
Indent
AFM image
0 100 200 300 400 500
0
2
4
6
8
10
N
o
r
m
a
l

F
o
r
c
e

(
m
N
)
Penetration depth (nm)
P
max
> 130 nm
L

> 12 m
Proximity Effect of Bulk Copper
Hardness
1.883 0.1 GPa
Hardness
1.879 0.08 GPa
15 m
4 m
0 100 200 300 400 500 600
0
2
4
6
8
10
N
o
r
m
a
l

F
o
r
c
e

(
m
N
)
Penetration depth (nm)
0 100 200 300 400 500 600
0
2
4
6
8
10
N
o
r
m
a
l

f
o
r
c
e

(
m
N
)
Penetration depth (nm)
1. Reference set 2. Test set
0.2 %
Properties of Thin Copper Film




R
a
: ~ 3.5 0.5 nm
Recommended P
d
, max : > 70 nm
Film thickness : 595 13 nm
Recommended P
d
, max : < 60 nm
Diameter of the indent : 600 nm
Recommended distance : ~ 2 m
Thickness Roughness
AFM image
0 20 40 60 80
0
50
100
150
200
250
N
o
r
m
a
l

L
o
a
d

(

N
)
Penetration depth (nm)
P
max
~ 60 nm
L

> 2 m
Proximity Effect of Thin Copper Film
Hardness
1.91 0.05 GPa
Hardness
1.92 0.07 GPa
2 m
0.6 m
0 20 40 60 80
0
50
100
150
200
250
N
o
r
m
a
l

L
o
a
d

(

N
)
Penetration depth (nm)
0 20 40 60 80
0
50
100
150
200
250
N
o
r
m
a
l

L
o
a
d

(

N
)
Penetration depth (nm)
1. Reference set 2. Test set
0.7 %
Substrate Effect
Substrate effect can be found when
measuring material properties of thin films
Al
2
O
3
Al
Si
Size effect
Substrate effect
Constant value
International Journal of Modern Physics B Vol. 24. (2010)
0 50 100 150 200 250 300 350 400
2.8
3.2
3.6
4.0
4.4
4.8
H
I
T

(
G
P
a
)
Indentation depth (nm)
Substrate
Material Property Variation wrt depth
Hardness
Consideration of hardness variation with
penetration depth
Substrate
Film
F
N F
N
Substrate
F
N
VH
k
xL
=
V : Wear volume
H : Hardness
x : Total distance
L : Load
Wear coefficient from
Archards wear equation
Horizontal force in plowing model
f h
F H A =
A
h
: Horizontal
projected area
Wear Volume Calculation
Total volume = Area x sliding distance
Assumptions
Shape of the wear track was assumed to be a
segment of a circle Only penetration depth
and width of the wear track are required
Idealized cross-section
of the wear track
P
d
Width

R

2
( )
2
d
w
A R R P t u =
where
2 2
4
4
d
d
w P
R
P
+
=
1
tan
d
w
R P
u

| |
=
|

\ .
,

Result of Scratch Test (1)
Penetration depth of the wear track









0.0 0.1 0.2 0.3 0.4 0.5
0
2
4
6
8
10
N
o
r
m
a
l

l
o
a
d

(
m
N
)
Sliding Distance (mm)
0.0 0.1 0.2 0.3 0.4 0.5
-300
-200
-100
0
100
P
e
n
e
t
r
a
t
i
o
n

d
e
p
t
h

(
n
m
)
Sliding distance (mm)
Ramp
loading

Result of Scratch Test (2)
Width of the wear track







Widths were directly measured from SEM
images
W : 0.8 m W : 1.5 m W : 1.2 m
A

B

C

Area of the Wear Track
0.0 0.1 0.2 0.3 0.4 0.5
-300
-200
-100
0
100
P
e
n
e
t
r
a
t
i
o
n

d
e
p
t
h

(
n
m
)
Sliding distance (mm)
0.0 0.1 0.2 0.3 0.4 0.5
0.75
0.90
1.05
1.20
1.35
1.50
W
i
d
t
h

(

m
)
Sliding distance (mm)
2
( )
2
d
w
A R R P t u =
0.0 0.1 0.2 0.3 0.4 0.5
0.00
0.05
0.10
0.15
0.20
A
r
e
a

(

m
2
)
Sliding Distance (mm)
Overall Conclusions

Proximity effect of SiO
2
, bulk Cu and Cu thin film,
showed no significant dependence on distance
between neighboring indents.
Composite hardness was measured to investigate
the intrinsic material properties of a few nm thick
film.
Modified wear (Archards) and friction (Plowing)
models were proposed to improve the accuracy of
wear prediction.