You are on page 1of 36

www.bruker-axs.

com

Advanced Scratch Testing for Evaluation of


Coatings
Suresh Kuiry, PhD
Bruker Nano Surfaces Division
Tribology and Mechanical Testing, 1717 Dell Ave, Campbell, CA 95008, U.S.A.
May 8, 2012

Introduction
Scratch Tests Fundamentals

Scratch Failure Regimes and Their Characteristics


Existing Scratch Models
CETR-UMT Scratch Tester

Advanced Scratch Testing with CETR-UMT


Some Scratch Test Results Obtained Using CETR-UMT
Q&A

June 5, 2012

Why Scratch Test ?


Coatings are used for optical, microelectronic, packaging, biomedical, and
decorative applications to improve:

tribological (lower friction),


mechanical (wear/abrasion resistance),
chemical (barrier to aggressive gases),
optical, magnetic, and electrical properties of any substrate.

Functional behaviour of a coating is critical to its adhesion to the substrate.


Scratch test is one of widely used, fast, and effective methods to obtain the
critical loads that are related to adhesion properties of coating.

June 5, 2012

Scratch Tests
1. Scratch Hardness Test: Scratch with constant normal load on a
specimen and on a reference specimen using a stylus. Scratch width
data are utilized to obtain the scratch hardness of the specimen as
follows [1]:
=

(1)

where, subscripts s and ref stand for the test specimen and the
reference specimen, respectively. The terms H, L, and W denote
hardness, normal load, and scratch width, respectively. The test is
used for bulk and coating materials.
2. Scratch Adhesion Test: This test is performed by applying either a
progressive (~linearly increasing) or constant load [2-4].

June 5, 2012

Progressive Load Scratch Test


Load
Stylus
Coating

A stylus is moved over a specimen


surface with a linearly increasing
load until failure occurs at critical
loads (Lci). Normal force (Fz) and
tangential force (Fx) are recorded.
The failure events are examined by
an optical microscope. Acoustic
Emission (AE) is also measured
during the test.

Scratch Direction

Lc is a function of coating-substrate
adhesion, stylus-tip radius, loading
rate, mechanical properties of
substrate and coating, coating
thickness, internal stress in coating,
flaw size distribution at substratecoating interface, and friction
between stylus-tip and coating.
June 5, 2012

Constant Load Scratch Test


Series of scratch tests are performed with constant normal loads on a
coating to obtain a load where the coating exhibits failure. Each scratch is
examined with an optical microscope for failure. The load at which such
failure of the coating occurs is termed as the critical load (Lc). Acoustic
Emission (AE) and Electrical Surface Resistance (ESR) are also measured
simultaneously during the constant load scratch test to supplement/confirm
the failure.

Constant load test requires more time but it provides greater statistical
confidence.
Progressive load test is suitable for rapid assessment and quality
assurance (QA) of coating. Hence, it is more popular for research and
development work on coating processes.

June 5, 2012

Coating Failure during Scratch Test


At sufficient stress, cracks initiate preferentially at defect sites in
the coating and/or coating-substrate interface. Propagation of
such cracks lead to coating failure.
Cohesive Failure: occurs by tensile stress behind the stylus
(Through-Thickness Cracking)
Adhesive Failure: Due to compressive stress, the coating
separates from the substrate either by cracking and lifting
(Buckling) or by full separation (Spallation; Chipping).
Practical scratch adhesion value of coating is defined as the
lowest critical load at which a coating fails. It is an important
parameter related to coating-substrate adhesion that could be
used for comparative evaluation of coatings.

June 5, 2012

Damage Features
Through Thickness Cracking
Brittle Tensile Cracking: Nested microcracks; open to the direction of scratch;
straight and semi-circular; formed behind
the stylus.

Scratch Direction
Chevron Cracks

Arc Tensile

Hertz Cracking: Series of nested microcracks within the scratch groove

Hertz

Conformal Cracking: micro-cracks form


while coating try to conform to the groove;
open away from the direction of scratch.

Conformal

Scratch Direction
Chipping

June 5, 2012

Chipping
Rounded regions of coating removal extending
laterally from the edges of the scratch groove
8

Damage Features
Spallation
Buckling : coating buckles ahead of the stylus
tip; irregularly wide arc-shaped patches
missing; opening away from scratch direction.
Wedging : Caused by a delaminated region
wedging ahead to separate the coating;
regularly spaced annular-circular that extends
beyond the edge of the groove.
Recovery: regions of detached coating along
one or both sides of the grove; produced by
elastic recovery behind the stylus and plastic
deformation in the substrate.
Gross Spallation : Large detached regions;
common in coating with low adhesion strength.
June 5, 2012

Scratch Direction
Buckling

Wedging

Recovery

Gross Spallation

Failure Mechanisms of Coating


Substrate Hardness

Coating Hardness
High
Low

Low

June 5, 2012

High

Plastic deformation of
coating and substrate
produces tensile and
conformal cracking with
buckling failure of
coating

Plastic deformation and


conformal cracking of
coating, followed by
spallation and buckling
failure in coating as
substrate cracks.

Tensile and Hertzian


cracks in coating
progressing to chipping
and spallation of
coating as substrate is
deformed

Tensile crack followed


by chipping and
spallation of coating

10

Scratch Models
Benjamin and Weaver: They proposed two scratch models [5] based on
(a) tangential force (Fx) at the tip and (b) normal force. The 1st model can
be summarized as:
=

12

+ 4 2 +

(2)

where, d is scratch width, R is the tip radius, Hs and Hc are the hardness
of substrate and coating, respectively; t is the shear stress at the coatingsubstrate interface and t is the thickness of the coating.
The 1st, 2nd, and 3rd terms in the RHS of the equation (2) are the ploughing
force required to deform the substrate, the force to remove coating from
the surface, and the ploughing force required to push aside the sheared
film, respectively. This model can be used to obtain critical shear stress (tc)
of the coating-substrate interface. This model was found to work well with
Al-coated glass specimen.
June 5, 2012

11

Scratch Models
The 2nd model of Benjamin and Weaver is based on normal force that
describes scratching in terms of shear stress (ts) at the lip of stylus tip:
=


2 2

(3)

where, a is the contact radius between the tip and the coating (a d/2).
The model gives a measure of adhesion in terms of critical shear stress by
substituting a measured at the critical load.
Ollivier and Matthews: They [6] replaced HS in equation (3) by Fz/pa2,
resulting in a critical shear stress given by:
=

2 2

(4)

where, Lc = critical load and ac = contact radius at the critical load. This
model was able to yield semi-quantitative results for DLC films.
June 5, 2012

12

Scratch Models
Laugier: Total compressive stress (sx) under the leading edge of the
indenter is expressed as [8,9]:

= 2 2

4 +

3
8

1 2

(5)

where, is the Poissons ratio of the substrate and m is friction coefficient


(Fx/Fz) between the indenter and the coating. The first terms originates
from the compressive stress at the leading edge of the indenter induced by
the friction during sliding. The second term describes the radial surface
stress at the edge of the contact circle induced by the force normal to the
surface. Assuming elastic Hertzian contact, the contact radius (a) is
expressed as:
3

3
1 2

4

1 2
+

(6)

is the Poissons ratio of the coating, Es and Ec are the Youngs moduli of
the substrate and the coating, respectively.
June 5, 2012

13

Scratch Models
For a << R, the shear stress (t) acting on the coating-substrate interface at
the lip of the indentation was approximated as :

(7)

The value of the t at the critical load is considered a measure of coating


adhesion.
Laugier later [9] introduced practical work on adhesion (W) as:
W=

(8)

The critical stress (sc) is the sum of external stress and internal stress at
the critical load. This model was purely elastic, and it was assumed that a
>> t. The model predicted results on carbide and nitride coatings
reasonably.
June 5, 2012

14

Scratch Models
Burnett and Rickerby [10]: The driving forces for removal of coating
consists of components of (i) an elastic-plastic indentation stress, (ii) an
internal stress, and (iii) tangential force. The following relation was derived
for critical scratching load:
=

2 2
8

(9)

where, W is the work of adhesion, dc is the scratch width at the critical


load.

June 5, 2012

15

Scratch Models
Bull et al [7] modified Burnett-Rickerby model assuming that the coating
detachment occurs when the tangential compressive stresses in the
coating in front of the stylus induce critical tensile stresses normal to the
coating-substrate interface: The critical load is given by:
=

(10)

where Ac is the cross-sectional area of the scratch track at the critical load:
=

2 1 2

1/2
2
2

(11)

Equation (10) could be used to calculate work of adhesion (W).

June 5, 2012

16

Limitation of Scratch Models


The existing models invariably use assumptions and simplifications to deal
with the inherent complexity of any scratching process, which involves
large number of variables. Hence, the existing scratch models experience
great difficulties to give a complete analytical description of the mechanics
of scratch testing. Predicted scratch adhesion values from such models
differ widely from the actual scratch test results.

Evaluation and fine-tuning of such scratch models certainly requires


continuous developmental effort with an objective to obtain a standard
model that would give comprehensive description of any scratching
process.

June 5, 2012

17

Practical Approach
For all practical application, we perform scratch test to obtain the critical load
as a useful adhesion parameter for evaluation of coatings to ensure their
fitness for use.

June 5, 2012

18

Scratch Tester (CETR-UMT)


CETR-Universal Materials Tester (CETR-UMT) is a unique test and
measurement system that can be used for Scratch Testing:

Constant load scratch Test for hardness and adhesion


Progressive load scratch Test for practical adhesion
Electrical Contact Resistance (ECR)
Electrical Surface Resistance (ESR)
Acoustic Emission (AE)
in-situ scratch depth profiling using capacitance sensor, tipdisplacement (Z-encoder)
Optical microcopy and AFM for imaging
3D-Optical Microscopy (interferometry) for imaging and metrology
June 5, 2012

19

Scratch Tester (CETR-UMT)

June 5, 2012

20

Linear Scratch Test

Specimen: 3.5-mm thick DLC coating on steel substrate.


Tool: Diamond stylus 12.5-mm tip radius
Scratch Parameters: Linear; 1 mm at 0.02 mm/s; Load 20 to 500 mN;
Coating failed at 298 mN
June 5, 2012

21

Linear Scratch Profile with K0

Specimen: 3.5-mm thick DLC coating on steel substrate.


Tool: Diamond stylus 12.5-mm tip radius
Scratch Parameters: Linear; 1 mm at 0.02 mm/s; Load 20 to 500 mN;
Coating failed at 298 mN
June 5, 2012

22

Linear Scratch

Specimen: 1-mm thick


DLC coating on
Titanium substrate.

Tool: Rockwell
Diamond indenter
200-mm tip radius
Adhesion: 25 N
June 5, 2012

23

Linear Scratch

Specimen: 3.5-mm
thick DLC coating on
Steel substrate.
1.5
1
0.5
0
Z [um]

Tool: Rockwell
Diamond indenter
200-mm tip radius

-0.5
-1
-1.5

Adhesion: 25 N

-2
-2.5
-150

-100

-50

50

100

X [ um ]

June 5, 2012

24

Linear Scratch with Depth Profile

40-mm thick polymer coating on steel; WCmicro-blade (400-mm tip radius)


Scratch depth profile is measured using Zencoder of CETR-UMT. Pre-scan, scratch
(green), post-scan (black) steps are used for
removing the sample-tilt. Image tag displays
scratch width (Y) and depth (D)

June 5, 2012

25

Linear Scratch

Specimen: 10-mm thick Zn-coating on steel.


Tool: Rockwell Diamond indenter 200-mm tip radius
Adhesion: 9.7 N
June 5, 2012

26

Linear Scratch with Depth Profile

Scratch depth profile is


measured using either
Cap sensor or Z-encoder
of CETR-UMT. Pre-scan,
scratch (black), scratch
(blue), and post-scan
(red) steps took care of
sample-tilt. Image tag
displays scratch width
(Y) and depth (D)
June 5, 2012

27

Linear Scratch with Depth Profile

Scratch depth profile of


coated-wire measured with Zencoder of CETR-UMT. Prescan, scratch (black), scratch
(blue), and post-scan (red)
steps take care of sample-tilt.
Image tag displays scratch
width (Y) and depth (D)

June 5, 2012

28

Linear Scratch for Adhesion Energy

25

20

Z [um]

15

10

-5
-300

-200

-100

0
X [ um ]

100

200

300

Specimen: Polymer dots (1.2 mm dia x 25 mm) on ceramic substrate.


Tool: Special Tool-steel micro-blade; Fx increased during delamination of
a polymer dot. Adhesion Energy calculated from area of the triangle under
Fx plot. Adhesion Energy: 490 erg
June 5, 2012

29

3D-Scratch

Specimen: 3.5-mm thick DLC coating on steel substrate.


Tool: Diamond stylus 12.5-mm tip radius
Scratch Parameters: 3D; 1 mm by slider at 0.004 mm/s; 0.15mm stroke
by linear at 0.15 mm/s; Load 20 to 250 mN;
Coating failed at 245 mN
June 5, 2012

30

X-Y Scratch with Reduced Spacing

Specimen: 3.5-mm thick DLC coating on steel substrate.


Tool: Diamond stylus 12.5-mm tip radius
Scratch Parameters: X-Y; 120-mm long; spacing 100, 80, 60, 50, 40, 30,
20, 10 mm; at 0.01 mm/s; Load 250 mN
Coating did not Fail
June 5, 2012

31

X-Y Scratch with Reduced Spacing

Specimen: 3.5-mm thick DLC coating on steel substrate.


Tool: Diamond stylus 12.5-mm tip radius
Scratch Parameters: X-Y; 120-mm long; spacing 60,40,30, 20,15,10,5 mm;
at 0.01 mm/s; Load 250 mN
Coating Failed
June 5, 2012

32

Angular Scratch

Specimen: 3.5-mm thick DLC coating on steel substrate.


Tool: Diamond stylus 12.5-mm tip radius
Scratch Parameters: Angular; X = 48 mm at 2 mm/s; Y = 120 mm at 10
mm/s; Load 250 mN;
Last cycle was not moved and the coating failed.
June 5, 2012

33

Concluding Remarks

Scratch test is a widely used test procedure for


evaluation of coatings.

CETR-UMT can perform advanced scratch tests


(Constant load, Progressive, 3D, X-Y, Angular
etc) to evaluate the adhesion properties of
coating.

CETR-UMT
Test
system
can
perform
comprehensive evaluation of coatings by
automated imaging and profiling of scratch.

June 5, 2012

34

References
ASTM Standard G171 (03) Standard Test Method for Scratch Hardness of
Materials Using a Diamond Stylus.
2. ASTM Standard C1624 (05) Standard Test Method for Adhesion Strength and
Mechanical Failure Modes of Ceramic Coatings by Quantitative Single Point
Scratch testing
3. S. J. Bull, Surf. Coat. Technol. 50 (1991) 25.
4. S. J. Bull, Trib. Inter. 30 (1997) 491.
5. P. Benjamin, C. Weaver, Proc. R. Soc. London, A 254 (1960) 163.
6. B. Ollivier, J. Matthews, J. Adhesion Technol., 8 (1994) 651.
7. S.J. Bull, D.S. Rickerby, A. Matthews, A. Leyland, A.R. Pace, J. Valli, Surf. Coat.
Technol. 36 (1988) 503.
8. M.T. Laugier, Thin Solid Films 76 (1981) 289; 117 (1984) 243.
9. M.T. Laugier, J. Mater. Sci. 21 (1986) 2269.
10. P.J. Burnett, D.S. Rickerby, Thin Solid Films 154 (1987) 403; 157 (1988) 233.
1.

June 5, 2012

35

www.bruker-axs.com
productinfo@bruker-nano.com

May 8, 2012

36