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Measuring Coating Mechanical PropertiesCTT 2019
Rahul Nair
Fischer Technology, Inc. 2018 1
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Coating Mechanical Properties Characterization
2Fischer Technology, Inc. 2018
Nanoindentation Progressive Load
Scratch
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Characterizing Surfaces
3Fischer Technology, Inc. 2018
Treated surfaces
Coatings and Thin Films
Composites
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Coating Mechanical Properties Characterization
4Fischer Technology, Inc. 2018
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Coating Mechanical Properties Characterization
5Fischer Technology, Inc. 2018
H a r d n e s s I C r e e p I E l a s t i c i t y I U n i a x i a l M e c h a n i c a l R e s p o n s e I
Te n s i l e S t r e n g t h a n d Te n s i l e S t r e s s I S t i f f n e s s i n Te n s i o n - Yo u n g ’ s
M o d u l u s I T h e P o i s s o n E f f e c t I S h e a r i n g S t r e s s e s a n d S t r a i n s
S t r e s s - S t r a i n C u r v e s T h e r m o d y n a m i c s o f M e c h a n i c a l R e s p o n s e I
E n t h a l p i c R e s p o n s e I E n t r o p i c R e s p o n s e I V i s c o e l a s t i c i t y I
S t i f f n e s s I K i n e m a t i c s : t h e S t r a i n – D i s p l a c e m e n t R e l a t i o n s I
E q u i l i b r i u m : t h e S t r e s s R e l a t i o n s I T r a n s f o r m a t i o n o f S t r e s s e s
a n d S t r a i n s C o n s t i t u t i v e I Y i e l d a n d P l a s t i c F l o w I M u l t i a x i a l
S t r e s s S t a t e s I E f f e c t o f H y d r o s t a t i c P r e s s u r e I E f f e c t o f R a t e a n d
Te m p e r a t u r e I C o n t i n u u m P l a s t i c i t y I T h e D i s l o c a t i o n B a s i s o f
Y i e l d a n d C r e e p K i n e t i c s o f C r e e p i n C r y s t a l l i n e M a t e r i a l s I
F r a c t u r e I A t o m i s t i c s o f C r e e p R u p t u r e I F r a c t u r e M e c h a n i c s - t h e
E n e r g y - B a l a n c e A p p r o a c h I t h e S t r e s s I n t e n s i t y A p p r o a c h I
F a t i g u e
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Characterizing Surfaces
6Fischer Technology, Inc. 2018
Mechanical Properties of these coatings is greatly influenced by several factors
i. Chemistry
ii. Deposition Technique
iii. Curing Procedure
iv. Aging and Weathering- Thermal, Oxidative and UV
v. Environmental Conditions- Temperature and Humidity
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Traditional Hardness Testing
7Fischer Technology, Inc. 2018
Hardness – resistance to penetration of a hard indenter
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Traditional Hardness Testing- Mohs Scale
8Fischer Technology, Inc. 2018
The ability of one solid to scratch another
or to be scratched by another solid
Austrian mineralogist Friedrich Moh, 1812
References -1. http://www.hautehorlogerie.org/en/glossary/mohs-scale-187/
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Traditional Hardness Testing- Pencil Hardness
9Fischer Technology, Inc. 2018
These alternate techniques are inexpensivePencil hardness
Handheld Hardness Testers
Scratch Testers for Scratch Hardness
BUT….
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Traditional Hardness Testing- Pencil Hardness
10Fischer Technology, Inc. 2018
i. Study to check the variability in the standard Pencils used in
Pencil hardness testing
ii. Our nanoindentation tester used to measure Martens
Hardness of standard Pencils
iii. At higher hardness range there is inconsistency of the pencil
hardness of the standard pencils
iv. Even at lower hardness levels pencil hardness of standard
pencils overlaps
v. Additionally, more uncertainty introduced by influence from
user
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Traditional Hardness Testing- Brinell
11Fischer Technology, Inc. 2018
Apply fixed load & Optical measure of the residual
print area
- Swedish engineer Johan August Brinell in 1900
2. http://en.wikipedia.org/wiki/Brinell_scaleReferences -1. http://www.precisiontestingequip.com/p1_02_3.html
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Traditional Hardness Testing- Rockwell
12Fischer Technology, Inc. 2018
Apply fixed pre-load, Apply fixed load & Penetration depth measurement
- Patented by Hugh M. Rockwell and Stanley P. Rockwell from CT in 1914
References -1. http://www.wilson-hardness.com/Products/RockwellTesters.aspx
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Traditional Hardness Testing- Vickers & Knoop
13Fischer Technology, Inc. 2018
Application of a fixed load
References -1. http://www.instron.us/wa/applications/test_types/hardness/vickers.aspx
Optical measurement
of the indentation
Apply fixed load & Optical measure
of the residual print area
- 1921 by Robert L. Smith and
George E. Sandland at Vickers Ltd in
Britain
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Traditional Testing- E-Modulus (Young’s modulus)
14Fischer Technology, Inc. 2018
tensile test (e.g. steel)ideal spring :
F = k.x
k: spring constant
F
x
k
k
matter constant E [Nmm-2] (Young’s Modulus, 1807)
A
F
F2
F
D
l 2Dl
l0
0
0
0
%100*
%100*)(
l
l
l
ll
D
ideal elastic behaviour of solid states : Hooke‘s law (1676)
stress :
strain :
.constE
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Limitations of Traditional Hardness Testing
15Fischer Technology, Inc. 2018
Coating
Base Material
Large Stress Field
• In applications where treated surfaces, coatings, thin films or composites are tested
• shows substrate influence
• indent may be too small to observe with a microscope
• (Soft) imprint on elastic materials may be too small to observe with microscope
• Testing big volumes of material can be time consuming
• Only hardness can be calculated
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Principles of Nanoindentation
16Fischer Technology, Inc. 2018
Force Actuator
F
Displacement Sensor
Indenter
Test Specimen
Apply a load (F) incrementally until amaximum is reached
Result: h=f(F,t)
Martens hardness HM is calculated as afunction of depth
The load decrease curve is used for thecalculation of material parametersIndentation Modulus Eit, IndentationHardness Hit
ISO14577 and ASTM E2546
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Principles of Nanoindentation
17Fischer Technology, Inc. 2018
h=f(F,t)
Apply a load (F) incrementally until a maximum is reached
Result: h=f(F,t)
Martens hardness HM is calculated as a function of depth
The load decrease curve is used for the calculation of material parameters Indentation Modulus Eit, Indentation Hardness Hit
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Principles of Nanoindentation
18Fischer Technology, Inc. 2018
h
F
F
h
F
h
ideal elastic
(rubber, spring)ideal plastic
(modeling clay)
elastic + plastic
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19
Fischer Technology, Inc. 2018
hmax
Loading
UnloadingIndentation modulus
Indentation hardness : Calculation of Vicker Hardness
)0945.0*()(
maxIT
cP
IT HHVhA
FH
Martens hardness
F, applied force (load)
h,
ind
en
tati
on
de
pth
h2IT1C
h1
h2
* 100
h2IT2C
h1
h2
* 100
Indentation Creep
Indentation Recovery )(2
12
11
2
cP
r
EE
sIT
hA
SE
E
i
i
r
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Dynamic Nanoindentation
20Fischer Technology, Inc. 2018
Storage and loss moduli, loss tangent
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Advantages of Nanoindentation
21Fischer Technology, Inc. 2018
Wide variety of Materials: Applies low load - Measure shallow depths
No optical measurement: no influence of the user
The instrumented indentation test yields more information thanclassical hardness measurements
Mechanical Properties Mapping
Indentation Hardness HIT
Indentation Modulus EIT
Creep CIT
Fracture Toughness
Storage and Loss moduli
Martens Hardness
Work Done- Elastic and Plastic
Vickers and Knoop Hardness
Pop-in and Pop-out
Glass Transition
10%
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Nanoindenter Form Factor – Base Instrument
22Fischer Technology, Inc. 2018
Reliable, cost-effective, user-friendly instrument to measure hardness,
elastic modulus, creep and much more of coatings and bulk material
Ample load and depth range;
broad range of applications
Minimal sample
preparation due to open
layout
Solid granite base with
specialized vibration
isolation silicone feet to
reduce noise
Compact design makes the
HM2000S an ideal tool for
all environments
Automated surface
detection for higher
productivity
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Nanoindenter Form Factor – Fully Equipped
23Fischer Technology, Inc. 2018
Measure on smallest
structures, cross-sections
with high precision
programmable xy-table
Enhanced high
resolution optical system
with autofocus and
multiple objective turret
Motorized z-axis and
fully-automated surface
detection for higher
productivity
Custom granite structure
for enhanced frame
stiffness and low noise
Minimal sample preparation
due to large working area
and open layout
Feature-packed, user-friendly instrument to measure hardness,
elastic modulus, creep and much more of coatings and bulk material
Same measuring head as
HM2000 S
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Factors that effect Nanoindentation
24Fischer Technology, Inc. 2018
Advantage Cone
Protects Indenters & Speeds up Indentation
Software algorithms to auto detect surface
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Factors that effect Nanoindentation
25Fischer Technology, Inc. 2018
Advantage Cone
Low Thermal Drift
Low Frame Compliance
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Base Instrument
Application: Automotive Paint and Clear Coats
26Fischer Technology, Inc. 2018
Measurement of two 80 µm thick 2K automotive
repair paints
• Max. indentation depth < 6.5 µm
2K automotive repair
paints Samples
HM
N/mm²
E ITGPa
Mean value Sample A
Sample B
42.9
143.0
1.4
3.1
Standard deviation Sample A
Sample B
1.2
5.6
0.1
0.1
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Base Instrument
Application: Wood Coating
27Fischer Technology, Inc. 2018
Measurement of seven 100 µm thick coatings
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Base Instrument
Application: Wood Coating
28Fischer Technology, Inc. 2018
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Base Instrument
Application: Wood Coating
29Fischer Technology, Inc. 2018
Hard
ness(H
M)
Depth (µm)
Similar Coating but different
wood substrate
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Fully Equipped Instrument- Motorized XYZ & Microscope
Application: Conformal Coatings- Cross-linking correlation
30Fischer Technology, Inc. 2018
Two-component conformal coatings are often used to minimize current leakage on
PCBs and as protection against humidity and other environmental factors
HM[N/mm²]
Depth [µm]
Depth [µm]
Time [s]
10 % over cross-linked
5 % over cross-linked
Optimally cross-linked
5 % under cross-linked
10 % under cross-linked
Martens hardness Indentation Creep
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Fully Equipped Instrument- Motorized XYZ & Microscope
Application: High Polymer Coatings
31Fischer Technology, Inc. 2018
• Indenter – Spheroconical diamond• F =10mN, Loading Time = 10sec, F =80mN, Loading Time = 36sec
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Fully Equipped Instrument- Motorized XYZ & Microscope
Heating Stage
32Fischer Technology, Inc. 2018
• Temperatures up to 200°C
• Two temperature sensors (internal in the table and external to place on the
sample)
• Ceramic indenter and heat shield to eliminate thermal expansion in the head
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Fully Equipped Instrument- Motorized XYZ & Microscope
Application: High Temp Stage – Polymer Coatings
33Fischer Technology, Inc. 2018
Polyamide PA66
• Thermal properties
o Glass-transition temperature: 50 – 60 °C
o Melting point: 260 °C
o Max. operation temperature: 80 – 120 °C
Increasing
Temperature
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Fully Equipped Instrument- Motorized XYZ & Microscope
Application: High Temp Stage – Polymer Coatings
34Fischer Technology, Inc. 2018
150
100
50
Mar
ten
s h
ard
nes
s[N
/mm
²]
15010050
Temperature [°C]
60
40
20
Elas
tic
par
tn
it[%
]
15010050
Temperature [°C]
20
10
Cree
p[%
]
nitCIT1
• Coating thickness 100 µm Max. load 10 mN
• Martens hardness shows decrease with increasing temperature
• Creep and elastic behavior: extreme in the region of the glass transition temperature
Glass-transition temperatureGlass-transition temperature
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Coating Adhesion- Traditional Techniques
35Fischer Technology, Inc. 2018
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Progressive Load Scratch Testing
36Fischer Technology, Inc. 2018
Depth
SensorASTM C1624
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Progressive Load Scratch Testing
37Fischer Technology, Inc. 2018
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Progressive Load Scratch Testing
38Fischer Technology, Inc. 2018
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Scratch Test- Actutors and Sensors
39Fischer Technology, Inc. 2018
Programmable XY-table
Friction Table built in
Optical microscope-
Upto 5 objectives with
DIC Mode with Polarized
light filter
Motorized Z-axis and fully-
automated surface detection for
higher productivity
Custom granite structure
for enhanced frame
stiffness and low noise
Minimal sample preparation
due to large working area
and open layout
Measuring with load
system, depth and AE
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Key Features
40Fischer Technology, Inc. 2018
Load
Industry leading range from 0.01 to 30N with 6uN
resolution
Active Force Feedback- Capacitive Sensor
Excellent linearity of sensor Non-linearity- <= 0.02%
of FSO
Most robust design- Overload protection of 500% of
FSO
https://www.youtube.com/watch?v=BflgP7PIzYc
High overload protection protects the instrument from damage
in case of a crash
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Key Features
41Fischer Technology, Inc. 2018
https://www.youtube.com/watch?v=BflgP7PIzYc
Faster stages combined with software that quickly acquires and compiles images
results in highest productivity
X, Y & Z Stages- BLDC motors
Almost 4 times higher torque than stepper motors
Better repeatability
Scratch Length- 100mm
Stages displacement- 200 x 50 x 100mm
Programmable for multiple scratches and samples
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Key Features
42Fischer Technology, Inc. 2018
Microscope
Microscope with excellent video image as a result
of high quality optics with 5x and 20x objective
Easy to resolve different failure mechanisms with
DIC Mode with Polarized light filter
Optically identifying the failure is the most important for
characterizing scratches- hence we chose the best optics
for any scratch tester
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Key Features
43Fischer Technology, Inc. 2018
Friction Table
Use same capacitive sensor as
normal load
Very high resolution
Negligible compliance
In addition to better quality friction data, the results do not change with or without
friction table.
There is no loss of energy compared to LVDT based friction tables which can
cause 5-15% error in data.
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Key Features
44Fischer Technology, Inc. 2018
Depth sensor-
Pre scan and Post Scan
Range- 1600 um
Resolution- 0.2nm
Higher depth range- Test across smaller curvatures and
difficult geometries without the depth signal saturating
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Application – Paint on Steel
45Fischer Technology, Inc. 2018
LC1 LC2 LC3
S1 3.77 N 5.43 N 7.58 N
50µm diamond indenter
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Application – Paint on Steel
46Fischer Technology, Inc. 2018
LC1 LC2 LC3
S1 3.77 N 5.43 N 7.58 N
50µm diamond indenter
![Page 47: Measuring Coating Mechanical Properties...Rahul Nair Fischer Technology, Inc. 2018 1 Coating Mechanical Properties Characterization Fischer Technology, Inc. 2018 2 Nanoindentation](https://reader031.vdocument.in/reader031/viewer/2022011911/5f93c208904a793a0878a5ae/html5/thumbnails/47.jpg)
Application – Paint on Steel
47Fischer Technology, Inc. 2018
LC1 LC2 LC3
S1 3.77 N 5.43 N 7.58 N
50µm diamond indenter
![Page 48: Measuring Coating Mechanical Properties...Rahul Nair Fischer Technology, Inc. 2018 1 Coating Mechanical Properties Characterization Fischer Technology, Inc. 2018 2 Nanoindentation](https://reader031.vdocument.in/reader031/viewer/2022011911/5f93c208904a793a0878a5ae/html5/thumbnails/48.jpg)
Summary
48Fischer Technology, Inc. 2018
Nanoindentation
Quantitative test for coatings on any substrate
Fundamental properties of only the coating
More than just hardness- elastic modulus, creep, etc.
Progressive Load Scratch
Simulation of real world under controlled lab conditions
Test of the entire coating-substrate system
Measure mar, crack and chip resistance and adhesion
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49Fischer Technology, Inc. 2018
Thank you!
Visit us at Booth #74
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Application – DLC on Steel
50Fischer Technology, Inc. 2018
LC1 LC2 LC3
S1 5.03 N 27.15 N 58.45 N
200µm diamond indenter
![Page 51: Measuring Coating Mechanical Properties...Rahul Nair Fischer Technology, Inc. 2018 1 Coating Mechanical Properties Characterization Fischer Technology, Inc. 2018 2 Nanoindentation](https://reader031.vdocument.in/reader031/viewer/2022011911/5f93c208904a793a0878a5ae/html5/thumbnails/51.jpg)
Application – DLC on Steel
51Fischer Technology, Inc. 2018
LC1 LC2 LC3
S1 5.03 N 27.15 N 58.45 N
200µm diamond indenter
![Page 52: Measuring Coating Mechanical Properties...Rahul Nair Fischer Technology, Inc. 2018 1 Coating Mechanical Properties Characterization Fischer Technology, Inc. 2018 2 Nanoindentation](https://reader031.vdocument.in/reader031/viewer/2022011911/5f93c208904a793a0878a5ae/html5/thumbnails/52.jpg)
Application – DLC on Steel
52Fischer Technology, Inc. 2018
LC1 LC2 LC3
S1 5.03 N 27.15 N 58.45 N
200µm diamond indenter
![Page 53: Measuring Coating Mechanical Properties...Rahul Nair Fischer Technology, Inc. 2018 1 Coating Mechanical Properties Characterization Fischer Technology, Inc. 2018 2 Nanoindentation](https://reader031.vdocument.in/reader031/viewer/2022011911/5f93c208904a793a0878a5ae/html5/thumbnails/53.jpg)
Fully Equipped Instrument- Motorized XYZ & Microscope
Application: Cross-sections
53Fischer Technology, Inc. 2018
Metallic layer
HMN/mm²
EIT/(1-vs^2)GPa
HIT
N/mm²HV
X 4734.2 151.8 6961.9 657.8
s 223.9 8.8 263.6 24.9
V/% 4.7 5.8 6.0 6.0
Load
Depth