Measuring Coating Mechanical Properties

CTT 2019
Rahul Nair
Fischer Technology, Inc. 2018 1
 Coating Mechanical Properties Characterization

Nanoindentation Progressive Load

Scratch

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 Characterizing Surfaces

Treated surfaces

Coatings and Thin Films

Composites

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 Coating Mechanical Properties Characterization

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 Coating Mechanical Properties Characterization
Hardness I Creep I Elasticity I Uniaxial Mechanical Response 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
Modulus I The Poisson Effect I Shearing Stresses and Strains
Stress-Strain Curves Thermodynamics of Mechanical Response I
Enthalpic Response I Entropic Response I Viscoelasticity I
Stiffness I Kinematics: the Strain–Displacement Relations I
Equilibrium: the Stress Relations I Transformation of Stresses
a n d S t r a i n s C o n s t i t u t i v e I Yi 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
Stress States I Effect of Hydrostatic Pressure I Effect of Rate and
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
Yi 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 ys t a l l i n e M a t e r i a l s I
Fracture I Atomistics of Creep Rupture I Fracture Mechanics-the
Energy-Balance Approach I the Stress Intensity Approach I
Fatigue

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 Characterizing Surfaces
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

Hardness – resistance to penetration of a hard indenter

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 Traditional Hardness Testing- Mohs Scale

The ability of one solid to scratch another

or to be scratched by another solid

Austrian mineralogist Friedrich Moh, 1812

Fischer Technology, Inc. 2018 References -1. http://www.hautehorlogerie.org/en/glossary/mohs-scale-187/ 8

 Traditional Hardness Testing- Pencil Hardness

These alternate techniques are inexpensive

Pencil hardness
Handheld Hardness Testers
Scratch Testers for Scratch Hardness

BUT….

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 Traditional Hardness Testing- Pencil Hardness

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

Apply fixed load & Optical measure of the residual

print area

- Swedish engineer Johan August Brinell in 1900

Fischer Technology, Inc. 2018 References -1. http://www.precisiontestingequip.com/p1_02_3.html 2. http://en.wikipedia.org/wiki/Brinell_scale 11

 Traditional Hardness Testing- Rockwell

Apply fixed pre-load, Apply fixed load & Penetration depth measurement
- Patented by Hugh M. Rockwell and Stanley P. Rockwell from CT in 1914

Fischer Technology, Inc. 2018 References -1. http://www.wilson-hardness.com/Products/RockwellTesters.aspx 12

 Traditional Hardness Testing- Vickers & Knoop

Apply fixed load & Optical measure

of the residual print area

- 1921 by Robert L. Smith and

George E. Sandland at Vickers Ltd in
Britain

Optical measurement
Application of a fixed load of the indentation

Fischer Technology, Inc. 2018 References -1. http://www.instron.us/wa/applications/test_types/hardness/vickers.aspx 13

 Traditional Testing- E-Modulus (Young’s modulus)
ideal elastic behaviour of solid states : Hooke‘s law (1676)
ideal spring :  tensile test (e.g. steel)
F = k .x F
stress : 
A
k: spring constant
k
F l (l  l0 ) * 100%
0 strain : 
l0
D
k 2Dl Dl * 100%
l

F l0
x 2
F


E  const. matter constant E [Nmm-2] (Young’s Modulus, 1807)


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 Limitations of Traditional Hardness Testing
• 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

Coating
Large
Stress
Base Material
Field

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 Principles of Nanoindentation

 Apply a load (F) incrementally until a Force Actuator

maximum is reached
 Result: h=f(F,t)
F
 Martens hardness HM is calculated as a Displacement Sensor

function of depth
 The load decrease curve is used for the
calculation of material parameters
Indentation Modulus Eit, Indentation
Hardness Hit Indenter

 ISO14577 and ASTM E2546 Test Specimen

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 Principles of Nanoindentation

 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 h=f(F,t)
Modulus Eit, Indentation Hardness Hit

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 Principles of Nanoindentation
ideal elastic
ideal plastic
(rubber, spring)
(modeling clay)

h h
elastic + plastic

h
F F

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 Indentation hardness : Calculation of Vicker Hardness
Fmax
H IT  ( HV  H IT * 0.0945 ) Indentation Creep
AP (hc ) h2 h1
CIT1 * 100
h2
Indentation modulus
Unloading
h, indentation depth

1 s
2

Martens hardness
hmax E IT  1 i 2
1
Er  Ei
Loading
 S
Er 
Indentation Recovery 2 AP ( hc )
h2 h1
CIT2
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* 100
h2 F, applied force (load) 19
 Dynamic Nanoindentation
Storage and loss moduli, loss tangent

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 Advantages of Nanoindentation
 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 than
classical hardness measurements

 Indentation Hardness HIT  Martens Hardness

 Indentation Modulus EIT  Work Done- Elastic and Plastic
 Creep CIT  Vickers and Knoop Hardness 10%
 Fracture Toughness  Pop-in and Pop-out
 Storage and Loss moduli  Glass Transition

 Mechanical Properties Mapping

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 Nanoindenter Form Factor – Base Instrument
Reliable, cost-effective, user-friendly instrument to measure hardness,
elastic modulus, creep and much more of coatings and bulk material

Automated surface Ample load and depth range;

detection for higher broad range of applications
productivity
Minimal sample
preparation due to open
layout

Solid granite base with

specialized vibration
Compact design makes the isolation silicone feet to
HM2000S an ideal tool for reduce noise
all environments

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 Nanoindenter Form Factor – Fully Equipped
Feature-packed, user-friendly instrument to measure hardness,
elastic modulus, creep and much more of coatings and bulk material

Minimal sample preparation Motorized z-axis and

due to large working area fully-automated surface
and open layout detection for higher
productivity

Enhanced high
resolution optical system
with autofocus and
Same measuring head as multiple objective turret
HM2000 S
Measure on smallest
structures, cross-sections
Custom granite structure with high precision
for enhanced frame programmable xy-table
stiffness and low noise

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 Factors that effect Nanoindentation
Advantage Cone
 Protects Indenters & Speeds up Indentation
 Software algorithms to auto detect surface

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 Factors that effect Nanoindentation
Advantage Cone
 Low Thermal Drift
 Low Frame Compliance

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 Base Instrument
Application: Automotive Paint and Clear Coats
Measurement of two 80 µm thick 2K automotive
repair paints
• Max. indentation depth < 6.5 µm

2K automotive repair HM E IT
paints Samples N/mm² GPa

Mean value Sample A 42.9 1.4

Sample B 143.0 3.1
Standard deviation Sample A 1.2 0.1
Sample B 5.6 0.1

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 Base Instrument
Application: Wood Coating
Measurement of seven 100 µm thick coatings

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 Base Instrument
Application: Wood Coating

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 Base Instrument
Application: Wood Coating
Hardness(HM)

Similar Coating but different

wood substrate

Depth (µm)

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 Fully Equipped Instrument- Motorized XYZ & Microscope
Application: Conformal Coatings- Cross-linking correlation
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] 10 % over cross-linked
5% over cross-linked
Optimally cross-linked
5 % under cross-linked
10 % under cross-linked

Depth [µm] Time [s]

Martens hardness Indentation Creep

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 Fully Equipped Instrument- Motorized XYZ & Microscope
Application: High Polymer Coatings
• 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

• 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

Polyamide PA66

• Thermal properties Increasing

o Glass-transition temperature: 50 – 60 °C Temperature
o Melting point: 260 °C
o Max. operation temperature: 80 – 120 °C

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 Fully Equipped Instrument- Motorized XYZ & Microscope
Application: High Temp Stage – Polymer Coatings
Glass-transition temperature Glass-transition temperature

Creep [%]
Martens hardness[N/mm²]

Elastic part nit[%]

nit
CIT1
150 60 20

100 40

10
50 20

50 100 150 50 100 150

Temperature [°C] Temperature [°C]
• 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

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 Coating Adhesion- Traditional Techniques

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 Progressive Load Scratch Testing
Depth
ASTM C1624 Sensor

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 Progressive Load Scratch Testing

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 Progressive Load Scratch Testing

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 Scratch Test- Actutors and Sensors

Minimal sample preparation Motorized Z-axis and fully-

due to large working area automated surface detection for
and open layout higher productivity

Optical microscope-
Upto 5 objectives with
DIC Mode with Polarized
Measuring with load light filter
system, depth and AE

Custom granite structure Programmable XY-table

for enhanced frame Friction Table built in
stiffness and low noise

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 Key Features
 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

High overload protection protects the instrument from damage

in case of a crash
https://www.youtube.com/watch?v=BflgP7PIzYc

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 Key Features

 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

Faster stages combined with software that quickly acquires and compiles images
results in highest productivity
https://www.youtube.com/watch?v=BflgP7PIzYc

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 Key Features

 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

 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

 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

50µm diamond indenter

LC1 LC2 LC3

S1 3.77 N 5.43 N 7.58 N

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 Application – Paint on Steel

50µm diamond indenter

LC1 LC2 LC3

S1 3.77 N 5.43 N 7.58 N

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 Application – Paint on Steel

50µm diamond indenter

LC1 LC2 LC3

S1 3.77 N 5.43 N 7.58 N

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 Summary

 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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 Thank you!

Visit us at Booth #74

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 Application – DLC on Steel

200µm diamond indenter

LC1 LC2 LC3

S1 5.03 N 27.15 N 58.45 N

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 Application – DLC on Steel

200µm diamond indenter

LC1 LC2 LC3

S1 5.03 N 27.15 N 58.45 N

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 Application – DLC on Steel

200µm diamond indenter

LC1 LC2 LC3

S1 5.03 N 27.15 N 58.45 N

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 Fully Equipped Instrument- Motorized XYZ & Microscope
Application: Cross-sections

Depth
Load
Metallic HM EIT/(1-vs^2) HIT
HV
layer N/mm² GPa N/mm²
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

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