Industrial Lubrication and Tribology

Diamond-like carbon coatings a new design element for tribological applications

J. BrandC. BeckmannB. BlugG. KonrathT. Hollstein

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To cite this document:
J. BrandC. BeckmannB. BlugG. KonrathT. Hollstein, (2002),"Diamond-like carbon coatings a new design element for
tribological applications", Industrial Lubrication and Tribology, Vol. 54 Iss 6 pp. 291 - 295
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Diamond-like carbon
coatings a new design
element for tribological
applications
J. Brand
C. Beckmann
B. Blug
G. Konrath and
T. Hollstein

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The authors
J. Brand and C. Beckmann are at Fraunhofer Institut fur
Schicht- und Oberflachentechnik IST, Braunschweig,
Germany.
B. Blug, G. Konrath and T. Hollstein are at Fraunhofer
Institut fur Werkstoffmechanik IWM, Freiburg, Germany.
Keywords
Coating, Component manufacture, Metals
Abstract
Diamond-like carbon coatings (DLC) combine high wear
resistance with low friction coefficients. Both properties
enable the protective layers to sustain wide ranges of
loading and environmental conditions. At present, low
friction coatings are commonly used on an empirical basis
but not as a design element. The reason for the empirical
approach is the lack of tools for a description of the
interaction between the coatings and the substrate.
Furthermore it is difficult to obtain information on the
fracture properties of the coating substrate system (e.g.
fracture toughness, adhesion, residual stresses). A spherical
indentation provides a simple technique to measure
quantitatively the fracture toughness and the adhesion of
brittle coatings on a ductile substrate with standard
laboratory equipment. DLC coatings on a 100 Cr 6 steel
substrate are indented by silicon nitride balls with different
diameters and different loads. Fracture patterns (circular and
radial cracks, delamination) are analyzed by finite element
calculation and the fracture toughness of the coating itself
along with the interface toughness are estimated.
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Industrial Lubrication and Tribology

Volume 54 . Number 6 . 2002 . pp. 291295
MCB UP Limited . ISSN 0036-8792

Introduction
Low friction coatings are used today in nearly
all fields where a low coefficient of friction
and a high wear resistance is required. The
applications range from injection nozzles in
diesel engines to different kinds of journal and
ball bearings. The usual approach is to design
the component without taking into account
the properties of the coating and then test the
component in the application. The reason for
this trial and error approach is the difficulty in
determining properties of hard coatings other
than the hardness, Youngs modulus and the
residual stresses. But in most tribological
applications the adherence of the coating to
the substrate and the fracture toughness are
the lifetime determining properties of a
coating substrate system.
Common methods to determine the
adhesion of a coating substrate system are
the blister test, the scratch test, drill test and
the cut test (Drory and Hutchinson, 1996).
These methods all have shortcomings in the
case of very hard brittle coatings. For
example in the scratch test the erosion of the
probe hampers the measuring of the
adherence.
Besides the methods mentioned above,
there are several methods using different types
of indenters ranging from spherical indenters
to pyramids (Drory and Hutchinson, 1996).
The indenters used in this work are
macroscopical spherical indenters made of
silicon nitride (Si3N4) with diameters
between 2.38 and 10mm. With the 2.38mm
Si3N4 ball it is possible to test the adherence
as well as the fracture toughness of the DLC
coating with one single indenter.

Coating
The combination of the mechanical
properties along with the properties of a low
friction coating led to a wide distribution of
diamond like carbon coatings (DLC) in
tribological applications. Depending on the
coating process (PVD, CVD), the
fabrication parameters and different dopants
the hardness may be adjusted between
700HV and 4,000HV and the Youngs
modulus between 70 and 400GPa. Along
with low wear rates and a coefficient of
# Fraunhofer Institute.

291

Diamond-like carbon coatings

Industrial Lubrication and Tribology

Volume 54 . Number 6 . 2002 . 291295

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J. Brand, C. Beckmann, B. Blug, G. Konrath and T. Hollstein

friction adjustable between 0.01 and 0.2

(depending on the tribological partners
(Holmberg and Matthews, 1998)), these
features enable engineers to adapt the DLC
coating to the required properties in
application.
The analysed DLC films were prepared by
using a RF-PECVD process. The RF glow
discharge leads to reactive gas species and
ions in an atmosphere of a hydrocarbon/argon
gas mixture. These high energy particles are
necessary to build a hard carbon coating.
With a typical growth rate of 2-3 microns per
hour the deposition temperature lies below
200C. The coatings were deposited with
constant process parameters.
To facilitate the comparison of
experimental and numerical results a gradient
within the coating and a metallic adherent
layer in the coating interface were omitted.
The use of gradients and metallic adherent
layers would of course increase the
performance of DLC coatings by factors.
The coating had following properties:
Youngs modulus E = 255GPa (measured by
nanoindentation), poisson ratio  = 0.3
(estimated by literature (Cho et al. (1999)),
residual stresses (0 = 1.8GPa (measured by
substrate bending), thickness t = 2m and a
coefficient of friction  = 0.2 (against
Si3N4).

Experimentals
The spherical indentation tests were
conducted with a CK 10 testing machine of
Engineering Systems (Nottingham, UK).
Silicon nitride balls of different diameters
were pressed into the coating substrate system
(DLC, 100 Cr 6 steel) at multiple loads. The
resulting fracture patterns were observed with
an optical microscope.
At loads of lower than the plastic limit of
the substrate only elastic deformation takes
place, there is no lasting deformation of the
coating substrate system. At higher loads the
substrate deforms plastic, but the coating
itself will deform elastic because of the high
yield limit.
When a critical load Fcrit is reached, the
DLC coating will fracture with a circular
crack as is well known from brittle materials
such as ceramics (see Plate 1). Depending on
the loading conditions and the stress state
(determined by the residual stresses, the

Plate 1 Circular cracks in the DLC coating

loading, the coating thickness and the

indentation radius), the crack may nucleate
at the surface or at the interface of the
coating.
The load of the first fracture of the coating
Fcrit was used to estimate the fracture
toughness KIapll of the coating. At least five
ball indentation per load and ball diameter
ensured the validity of the results. Table I
shows the critical load for each tested ball
diameter.
A further increasing of the indentation
load leads to additional circular cone cracks
with an increased diameter. Depending on
the adhesion of the coating an even higher
load will result in radial cracks or in a
circular delamination of the coating or a
combination of both. Coatings with a strong
adhesion will show only radial channel
cracks (Table II).
At a load of F = 9,080N the substrate
showed a delaminated region with an
averaged delamination radius rd = 1.44mm
with a 2.144mm Si3N4 indentation. The
variation in the delamination radius during
different tests was less than 5 per cent.
Table I The load at which the first circular crack
nucleated
Ball diameter d in mm
2.38
4.76
7.14
10.00

Critical load Fcrit in N

501
1,574
3,670
6,350

Table II Average delamination radius rd at a load of

F = 9,080N
Load N
9,080

292

Delamination radius rd mm
1.44

Diamond-like carbon coatings

Industrial Lubrication and Tribology

Volume 54 . Number 6 . 2002 . 291295

J. Brand, C. Beckmann, B. Blug, G. Konrath and T. Hollstein

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Modelling
Finite element model
High indentation loads cause extended
plastic deformation in the substrate.
Therefore the modelling of the substrate
deformation is crucial for determining the
critical fracture stresses (Drory and
Hutchinson, 1996). The ball and the coating
substrate system is modelled with
axisymmetric bilinear elements in
combination with a linear kinematic
hardening evolution law. Figure 1 shows the
finite element model used. The yield stress
and the kinematic hardening modulus were
derived by comparison of measured cross
sections of ball imprints of different loads and
radii with calculated FEM results (see
Figure 2). Each indentation is represented by
a loading and an unloading step. For the
simulation of the indentation test the
following plastic parameters were used:
0 2:25GPa and 0:012 3:25GPa
0 is the yield stress at zero plastic strain and
0:012 is the stress at the plastic strain
Figure 1 The finite-element model of the spherical
indentation test

"pl 0:012. The Youngs modulus of the

substrate was taken as E = 210GPa and the
Poisson ratio as  = 0.3. The elastic constants
of the Si3N4 indenter were E = 310GPa and 
= 0.28. The residual stresses of the coating
were neglected in the calculation. All FEM
calculations were performed with the
commercial FEM software ABAQUS 5.8.
Fracture toughness
To estimate the fracture toughness KIappl of
the DLC coating a model proposed by
(Weppelmann, 1996) for TiAlN PVD
coatings was used. The model assumes an
initial flaw or crack at the surface or the
interface with a initial crack length c which is
small compared to the coating thickness t.
Then the stress intensity factors KI in an
infinitely large plane is calculated
as follows:
p
KI  cYI
1
With KI the stress intensity factor for a mode
I loading,  the stress and YI a geometry
factor.
If the initial flaw is at the interface of the
coating and is perpendicular to the interface,
p
YI 
2
For an initial flaw perpendicular to the surface
which is located at the surface, YI has the
form:
5 p
3
YI p 
20
The stress intensity factors KII for a mode II
loading for a plane crack is:
p
KII rz cYII
4
with rz the shearing stress and YII for plane
cracks and plane surface cracks:
p
YII 1:122 
5

Figure 2 Comparison of a calculated and a measured indentation profile

The stress intensity factor KIappl for a

multidimensional load is then:
2
KI2 KII2 KIappl

 is a weighting factor which accounts for the

fact, that usually KI 6 KII.
Interface toughness
The model used in this analysis deals with a
circular delamination of the coating
accompanied by break up of the detached film
such that a very narrow annular plate of film is
left behind the advancing interface crack
293

Diamond-like carbon coatings

Industrial Lubrication and Tribology

Volume 54 . Number 6 . 2002 . 291295

J. Brand, C. Beckmann, B. Blug, G. Konrath and T. Hollstein

front. The model was introduced by Drory

and Hutchinson (1996). If there is a
compressive residual stress and the coating
thickness t is small compared to the
indentation depth, the critical energy release
rate GInt is given:

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GInt

2coat t
r rd 2
2Ecoat

where r rd 0 rr rd denotes the

combination of the initial residual stress 0
and the radial component of the stress due to
indentation. The radius rd is the radius of the
delaminated film.
The interface toughness int is then
calculated from the critical energy release rate
as follows (Michler et al., 1999):
r
Gint Ecoat
8
int
1 2

Results
Fracture toughness
The significant stresses for cohesive fracture
of the coating are the radial stresses rr and
the shear stresses rz . The radial stresses rr
show at the critical loads a significant tensile
maximum just at the edge of the contact zone
(see Figure 3, the residual stresses are not
included in the simulation).
The maximums of the radial stresses are
situated within a range of 15 per cent (highest
maximum to lowest maximum). The
maximums of the radial stresses in each of the
analysed cases are located at the surface of the
coating and are corrected for the residual
stresses, on average at (rr max = 1.5GPa. That
is far below the theoretical elastic limit of E/10
of the coating. That means, the fracture of the
coating is governed by defects or other
fracture relevant factors such as grain size or
Figure 3 rr stresses at the surface and the interface at the critical load Fcrit

surface roughness. The shear stresses rz are

differently distributed. The maximum tensile
shear stresses are located at the coating
substrate interface (see Figure 4). Whereas a
higher indenter radius leads to a lower shear
stress.
The crack is likely to evolve from the
surface of the coating, because when the shear
stresses are at a maximum, the radial stresses
are already in a compressive mode when the
residual stresses are taken into account (see
Figure 5).
To give an estimate for the mixed mode
fracture toughness KIappl,  = 1.5 was chosen,
the stresses were considered to be constant at
the length of the initial cracks and the cracks
were supposed to be located at the surface
(Table III).
The mode II loading is significantly lower
than the mode I loading. The fracture
toughness ranges from 0.97 to 1.94MPa m1/2
depending on the supposed initial flaw size.
The fracture toughness of ceramics is typically
between 1-10MPa m1/2. Weppelmann (1996)
found for TiAlN coatings values between 1.48
and 1.64MPa m1/2 by nanoindentation.
Figure 4 rz stresses at the surface and the interface at
the critical load Fcritt

Figure 5 Stresses at the surface and the interface at the critical load Fcrit
and the supposed crack radius (residual stresses are not accounted for)

294

Diamond-like carbon coatings

Industrial Lubrication and Tribology

Volume 54 . Number 6 . 2002 . 291295

J. Brand, C. Beckmann, B. Blug, G. Konrath and T. Hollstein

Table III KIappl for different crack length c

c m
0.1
0.2
0.4

1/2

KI MPa m
0.94
1.32
1.87

KII MPa m
0.20
0.28
0.39

Table IV Interface toughness calculated by the delamination radius

1/2

KIappl MPa m

1/2

0.97
1.37
1.94

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In contradiction to the results above are the

observations of Michler et al. (1999), who
found the maximum tensile stresses at first
cracking of several different DLC coatings in
the range of the theoretical elastic limit.
Adhesion of the DLC coating
The indentation depth at a load F = 9,080N
and a radius R = 2.38mm is about 105m,
which means the assumption of a large
indentation depth compared to the film
thickness (t = 2m) is valid. The radial stress
at the delamination radius rd = 1.44mm in
combination of the residual stresses are
compressive, the interface toughness is then
essentially a mode II toughness (Drory and
Hutchinson, 1996). The toughness is the
calculated by equations (6) and (7) (see
Table IV).
The interface toughness with 0.55MPa m1/2
is as expected relative low. Micher et al.
(1999) found for different kinds of DLC
coatings values for interface toughness
between 1-27MPa m1/2.

Conclusions
In this paper the fracture toughness and the
interface toughness of a DLC coating without
an intermetallic layer on a 100 Cr 6 substrate
is determined by simple macroscopic

Load
N

Delam. radius
mm

sr
GPa

Gc
J/m2

MPa m1/2

9,080

1.44

1.74

1.1

0.55

indentation tests and finite element

calculation. The fracture toughness was
found to be in the range between 1-2MPa m1/2
depending on the assumed crack length. The
interface toughness is with 0.55 MPa m1/2 at
the lower end of the interface toughness for
DLC coatings found in the literature. The
simple models used in this publication
provide a fast and simple method to estimate
adhesion and the fracture toughness of hard
coatings on ductile substrates.

References
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``Determination of elastic modulus and Poissons
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