D/oAMOND RELATED MATERIALS

ELSEVIER
Diamond and Related Materials 7 (1998) 944-950

Residual stress and debonding of D L C films on metallic substrates 1

X.L. Peng, T.W. Clyne *
Department of Materials Sciences and Metallurgy, Cambridge University, Pembroke Street, Cambridge, CB2 3QZ, UK
Received 21 July 1997: accepted 13 November 1997

Abstract

Hydrogenated diamond-like carbon (DLC) films have been prepared using 13.56 MHz capacitively coupled RF glow discharge in a methane atmosphere. Film structure was characterised by FTIR and Raman spectroscopy. Deposition temperatures, which were measured using irreversible self-stick thermax, varied from 40 to 182 C. Stress levels were measured by monitoring the curvature changes of thin (125 gin) Ti foil after depositing thick (several lain) DLC films, using an A1 bonding layer. This intrinsic (deposition) stress was compressive and varied from -0.3 to -2.0 GPa. It increased initially with the average energy of the bombarding ions, reached a maximum and then decreased. Debonding behaviour of DLC coatings on four metallic substratesl with the interfaces being prepared in various ways, has been investigated. Films with a range of thicknesses have been prepared and specimens have been subjected to changes in temperature. From a knowledge of the residual stress levels in these films as a function of temperature, the strain energy release rate for interfacial debonding has been monitored during deposition and subsequent temperature changes. The value of the strain energy release rate at a point when interfacial debonding occurred has been taken as the interfaciai toughness (fracture energy). It is concluded from these observations that the interracial toughness is low for DLC films deposited onto mechanically polished surfaces of titanium, mild steel or stainless steel, but quite high on aluminium. Precleaning by bombardment with energetic argon ions raises the interracial toughness for the steels and for aluminium, but not for titanium. These observations have been related to the nature of the oxide films on these substrates. A thin sputtered interlayer of aluminium was found to raise the interfacial toughness significantly for the steels and for titanium. 1998 Elsevier Science S.A.

Keywords: Diamond-like carbon (DLC); RF discharge; Intrinsic stress; Interfacial toughness

1. Introduction Diamond-like carbon films (hydrogenated or nonhydrogenated) have been the subject of intensive research over the past 20 years or so. Various deposition techniques [1-6] have been employed. Bombardment by energetic species during growth (which is necessary for obtaining DLC structures) tends to generate high intrinsic compressive stresses. This is primarily a result of implantation of carbon atoms into the growing film during bombardment. This intrinsic stress is expected to be sensitive to the impact energies [7, 8], Although Zelez [9] reported relatively low intrinsic stress levels (+70 to - 7 5 0 MPa), most studies [7,10-14] have indicated high compressive stress levels in the range - 0 . 5 to - 1 2 . 5 GPa. Differential thermal contraction during
* Corresponding author. Fax: 0044 I223 334 567; e-mail: twcl0@cam.ac.uk This paper was presented at the Diamond 1997 Conference in Edinburgh, Scotland, August 3-8, 1997. 0925-9635/98/$19.00 1998 Elsevier Science B.V. All rights reserved. PH S 0 9 2 5 - 9 6 3 5 ( 9 7 ) 0 0 3 3 1 - 2

cooling also tends to make the stress in the film more compressive, particularly with metallic substrates. These high stress levels have several consequences in terms of the performance of the coating. Prominent among these is the fact that, particularly when the coating is relatively thick, there is a strong driving force for it to become detached. This driving force is best expressed as the strain energy release rate for interfacial debonding, Gi, and/or the associated stress intensity factor, Ki. When these parameters reach appropriate values, which characterise the toughness of the interface, then debonding is expected to occur [15-19]. For example, debonding is expected to occur when G i reaches the critical interfacial strain energy release rate, or interfacial fracture energy, Gic. In practice, there may be some barrier to initiation of the interfacial crack [20-22], so that a higher driving force than that predicted might, in fact, be necessary. However, initiation of debonding may occur readily from edges, where flaws are inevitably present [22]. There are also various issues concerning

X.L. Peng. T, W. Clyne / Diamondand Related Materials 7 (1998) 944-950

945

the exact mechanisms by which the film may become detached, including the possibility of gas accumulation at the interface promoting the initial debonding [2327]. DLC films have also been observed [28] to buckle when exposed to air for prolonged periods. There has also been interest [29-31] in the development of throughthickness cracks within coatings as a result of residual stresses. The formation of these may also affect the onset of debonding. There has been very little systematic work on the residual stress levels, corresponding strain energy release rates and interracial toughnesses of substrate/DLC coating systems. There have, however, been various attempts to explore in a qualitative or semi-quantitative way the factors which affect interracial adhesion. For example, it has been shown that adhesion of DLC films to certain substrates can be improved by surface pretreatments [32] and by using thin interlayers such as silicon [33] or aluminium [34,35], or by generating DLC/metal multilayer structures [36]. In the present paper, the mechanical stability of DLC films prepared by RF methane glow discharge is studied over a range of temperature and as a function of the residual stress levels and interfacial structure.

Some of the Al-coated substrates were then exposed to air. The deposition chamber was pumped down to below 10 .6 Pa and a pure methane atmosphere introduced for DLC deposition. The DLC film thickness was measured directly on the cross-section, using image display software on a JOEL 5800LV SEM. Specimens were also examined at various stages using optical microscopy, SEM, Raman and F T I R spectroscopy. Most of the DLC deposition for debonding studies was carried out at - 1 0 5 V negative bias and 10 Pa pressure, since these parameters generated the highest intrinsic stress (around - 2 GPa) and therefore the highest driving force for debonding at a given film thickness.
2.2. Deduction of stresses from curvature measurements

2. Experimental procedures
2.1. Spec#nen preparation and structural exam#Tation

DLC films have been prepared using 13.56MHz capacitively coupled R F glow discharge in a methane atmosphere. Table 1 lists the deposition parameters. Substrates of titanium ( S x 3 0 x 2 m m ) , aluminium (8 x 30x 1.5 ram), 316 stainless steel, mild steel (both 8 x 30 x 1.5 mm) and Si wafer (8 x 30 x 0.38 mm) were polished to a mirror finish (0.25 gm diamond), ultrasonically cleaned for 20rain in acetone, blown dry and placed in the deposition chamber. Selected substrates were then subjected to bombardment from an Ar plasma for 10 rain and/or deposition of an A1 bonding layer, using a DC magnetron sputtering source in an Ar atmosphere. The sputtering target was aluminium, of 99.9% purity, cleaned by in situ presputtering for t0 min. Table 1 Experimental conditions used for all DLC deposition RF power (W) Cathode area (cma) Base pressure (Pa) Pre-cleaning gas Working gas Gas flow rate (sccm) Working pressure (Pa) Deposition time (min) 5-150

The Stoney equation [37] is commonly used to calculate a film stress from a measured curvature. However, the equation is accurate only in the limit where the film thickness tends to be zero. Unfortunately, in this limit the curvature must also tend to be zero. It has been pointed out by Brenner and Senderoff [38] that the experimental error arising from the curvature being too small to measure accurately tends to exceed the error introduced via the approximation incorporated into the Stoney equation, when the ratio of the thickness of the coating to that of the substrate is less than about 5%. In the current work the thickness ratios and hence curvatures, were relatively large, but the stress was calculated using the exact expressions [22] which relate curvatures and stress distributions to the thicknesses and physical properties of substrate and coating--see Table 2,
2.3. Measurement of inte~faciaI toughness

Residual stresses, and hence strain energy release rates for interfacial debonding, are generated during deposition and also during subsequent temperature changes (provided the coating and substrate have different thermal expansivities). The strain energy release rate, Gi, is also dependent on the thickness of the film (and of the substrate, unless it can be taken as being infinitely thick). Table 2 Thermophysical property data [40,4I] used in stress and curvature calculations Property DLC 2.3 139.2 0.2 CP-Ti 8.5 106 0.36

20 <10-~ Ar or (Ar + 10% CH4) CH4 3-5

Thermal expansivity, c~(x 10-6 K -1) Young's modulus, E (GPa) Poisson's ratio

1-40
5-200

The Young's modulus of DLC was obtained from Blech's value [40] for the biaxial Young's modulus of I74 GPa, by assuming a Poisson ratio of 0.2.

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X.L. Peng, T.W. Clyne / Diamond and Related Materials 7 (1998) 944-950

The following expression [39] can be used.

Gi = fh

-H E'(y)

o'(Y)2 dy- f"

Gr(y) - 2 dy -H E'(y)

( 1)

where h and H are the thicknesses of film and substrate, E'(y) is the effective Young's modulus as a function of depth and ~(y), at(y) are the stress distributions before and after debonding. In the absence of comprehensive data on this, the effective Young's moduli of all the DLC films produced in the present work have been taken here as 174 GPa, which is the value reported by Blech and Wood [40]. For an effectively infinite substrate ( h < H ) , in which the variation with depth of the stress in the film can be neglected, this expression reduces to:
Gi --

that promotion of debonding by this method should, in principle, be possible, at least for most metallic substrates. The cooling operations were carried out using a liquid nitrogen cooling device. Typically, the specimen cooled from room temperature down to about -193 C over a period of approx. 30 rain. This is convenient for continuous observation and for accurate recording of the temperature at which any debonding might occur.

3. Results and discussions

3.1. Residual stresses

/,4

(2)

This approximation has been used in the present work.

Provided the generation of residual stress can be predicted with confidence (i.e., the deposition stress and deposition temperature are known), information about the critical strain energy release rate, G~o (interracial fracture energy) can be obtained by observing whether a film with a particular thickness has debonded by the time it cools to room temperature. If the assumption is made that Gie is given by the value of Gi when debonding occurs, then an observation that a particular coating remains attached to the substrate provides a lower bound on Gi~, whereas if detachment has occurred, an upper bound can be deduced. A series of experiments was, therefore, carried out by simply depositing films of various thickness and observing whether or not they had debonded when the chamber was opened after deposition and cooling. For some experiments, the sputtering target flange was replaced by a glass viewing window [37]. This allowed direct in situ observation of debonding during deposition. When debonding occurred, deposition was stopped and the film thickness was measured. This allowed the value of Sic to be determined from a knowledge of the deposition stress under the conditions concerned. For specimens which had not debonded after deposition and cooling to room temperature, further information about the interfacial toughness can be obtained by observing the specimen during subsequent cooling below room temperature. Since in most cases the thermal expansivity of the substrate is greater than that of the DLC coating, such cooling will generate compressive stress in the DLC, enhancing the deposition stress and raising the value of G~. Cooling through 200 C will, for a typical expansivity mismatch of 10 x t 0-6 K - l , generate a film stress (on an infinite substrate) of about -0.35 GPa (=kc~ AT E" DLC). This is significant compared with typical stress levels at room temperature, so

Experimental data are presented in Table 3. These include measured curvatures, corresponding misfit strains and, after subtraction of the thermal component, the intrinsic stress ~i which would be produced by deposition on an infinitely thick substrate. The quoted o-i values should be suitable for comparison with data from other work, in which thermal stresses were negligible (glass or Si substrates) and the substrates close to being infinitely thick. It can be seen that the values obtained in the present work range up to about 2 GPa (compressive). This is in broad agreement with previous work, although the very high values (> 3 GPa) obtained in some studies [10-12, 14] have not been recorded. The intrinsic stress is plotted in Fig. 1 as a function of negative bias voltage. Initially, the stress rapidly becomes strongly compressive as I~ rises. This is the result of pronounced implantation of bombarding carbon ions, once they have enough energy to penetrate the structure. Further increases in bombardment energies lead to intensive local heating (thermal spike), an increase in the substrate temperature and consequent reduction in the compressive stress as the structure undergoes thermal relaxation. It was also found that the stress level progressively reduces as the methane pressure is increased. Increasing this pressure leads to a sharp decrease in the mean free path of ions bombarding the specimen. This tends to inhibit implantation by reducing the energy of ions reaching the specimen surface and hence to reduce the stress levels. These results are similar to those reported by Zou et al. [10].
3.2. Debonding behaviour

Observations on the conditions under which debonding occurred are summarised in Table 4, which gives inferred values of, or bounds on, Gic (taken as equal to Gi at the point of debonding). These results are also presented in Fig. 2. Several features are immediately apparent. For the titanium and for both types of steel, the toughness of the interface formed by depositing DLC directly onto the substrate is low (Gi~ ~ 7 J m-2). It is very difficult to deposit films of more than about

X.L. Peng, T. W, Clyne / Diamond and Related Materials 7 (1998) 944-950

947

Table 3 E x p e r i m e n t a l d a t a f o r fihn thickness, r o o m t e m p e r a t u r e c u r v a t u r e , c a l c u l a t e d misfit strains a n d intrinsic stress b y a s s u m i n g it is entirely a c c o m m o d a t e d in the film (infinite s u b s t r a t e case) f o r v a r i o u s D L C films d e p o s i t e d o n t o 125/am t h i c k C P - T i s u b s t r a t e s Spec. code Bias voltage (V) T24 T25 T26 T7 T18 T3I T 13 T14 T5 T6 T8 Tt 1 T12 -40 -40 -40 - 105 - t05 - I05 - 195 - 195 -285 - 285 -345 -345 - 345 21 21 21 40 40 40 71 71 1 I8 I 18 182 i82 182 T, ':C DLC thickness h (~tm) 2.4 2.4 2.4 1.05 1.03 1.7 5.8 5.6 4.16 4.03 6 5.8 5.2 Measured curvature K (m-1) -2.36 - 3.19 -2.21 -4.7 -5.01 - 6.82 - 17.35 - 10.67 -7.3 - 9.2 - 10 -5.82 - - 10.6 N e t misfit strain, 2xe (millistrain) -2.59 -3.50 -2.43 - 11.40 - 12.40 - 10.40 - 8,57 -5.43 -4.83 - 6.26 -4.80 -2,87 - 5.75 Thermal misfit s t r a i n , A % (millistrain) 0 0 0 -0.09 -0.09 - 0.09 - 0.28 -0.28 -0.58 - 0.58 -0.97 -0.97 - 0.97 I n t r i n s i c misfit strain, ke~ (mitlistrain) -2.59 -3.50 -2.43 - 11.31 - 12,31 - 10.31 - 8.29 -5.15 -4.25 - 5.68 -3.82 - 1.90 -4.78 Intrinsic stress cri ( G P a ) -0.45 - 0.6i -0.42 - 1.97 -2.I4 - 1.79 - 1.44 -0.90 -0.74 - 0.99 -0.66 -0.33 - 0.83

0.5 lam in thickness without them spontaneously debonding. On aluminium, however, the adhesion is much better, with a value of Gio in excess of 100 J m -2. This is probably due to the different nature of the oxide film on aluminium, which is normally very thin and coherent. In the case of titanium, this tow toughness was not significantly affected by introduction of an Ar ion bombardment precleaning of the substrate. However, for the two steels, and especially for the stainless steel, such precteaning effected a large increase in Gic. This observation is presumably related to the nature of the surface oxide films formed in these systems. Such a film is apparently difficult to eliminate from titanium by a simple bombardment process for a relative short time (10 min); in fact, it is probable that it is at least partly removed, but a relatively thick oxide film reforms quickly. For aluminium, the high value of Gio observed in the absence of precleaning was increased significantly via argon bombardment to over 350Jm-2: This is
-2.5

~"
t~

-2

-1.5
I..,

.'-.2-

-I

_,=
-0.5
?.. _

Pr

I~

]r

I I I I

I I p

' 1 1 1

'

,I

0 0

50

1(30

I50

I o n e n e r g y , E = 0.5 e V b (eV) Fig. 1. I n t r i n s i c stress levels m e a s u r e d e x p e r i m e n t a l l y , f o r films d e p o s ited a t 10 P a p r e s s u r e w i t h v a r i o u s n e g a t i v e bias pressures.

presumably associated with removal of general contamination and possibly with a small reduction in oxide film thickness. In view of the excellent adhesion exhibited on aluminium, an A1 interlayer offers promise as a method of improving the bonding. It was indeed found that a thin (80 nm) layer of A1 deposited on the substrate prior to DLC deposition raised the interfacial toughness substantially for titanium and for both steels. The importance of surface oxide in contact with the DLC was highlighted for this case also by introducing a stage in which the aluminium interlayer was exposed to air, allowing formation of a thin surface oxide. (In fact, in view of the very high affinity of A1 for oxygen, and the unavoidable presence of at least some oxygen in the chamber, there would probably be at least a monolayer of oxide present in any event, but this would tend to thicken appreciably on exposure to air.) Introduction of the oxidation stage resulted in the measured interfacial toughness falling to values close to those in the absence of the interlayer or precleaning step. In fact, there is evidence that oxidation of the A1 interlayer changed the location of the debonding event. Fig. 3 shows EDX spectra taken from free surfaces before deposition of the DLC film and after it had debonded, for specimens with and without the interlayer oxidation stage. It can be seen that an A1 peak has disappeared after debonding with the unoxidised A1 interlayer--see Fig. 3a, while this A1 peak is still present when the interlayer was previously oxidised--see Fig. 3b. It follows that debonding occurred between the interlayer and the titanium substrate with the unoxidised A1 interlayer, but that the adhesion between the interlayer and the DLC film was weakened by the oxidation, and the interlayer was left adhering to the titanium substrate in this case. The measured toughness

948

X.L. Peng, T. W. Clyne / Diamond and Related Materials 7 (t998) 944-950

Table 4 Values of and bounds on the critical strain energy release rate of the interface, G,~, obtained by observing the conditions under which debonding occurred during deposition or subsequent cooling Specimen details Substrate
(mm) Ti, 2.0 Ti, 2.0 Ti, 2.0 Ti, 2.0 Ti, 2.0 MS, 1.5 MS, 1.5 MS, 1.5 M S , t .5 M S , 1,5 SS, 1.5 SS, 1.5 SS, 1.5 SS, 1.5 A1, 1.5 A1, 1.5 Ar preclean x ~" ~ t,~ ~" x t~" t~" tl ~ x I,,," ~" ~ ~" x A1 (gm) 0 0 0.08 0.08 0.08 0 0 0.08 0.08 0.08 0 0 0.08 0.08 0 0 Oxidise

Specimen state at debonding

DLC (gin) 0.30 0.40 1.81 1.20 0.50 0.33 9.56 0.93 1.86 1.3 0.30 13.5 0.50 2.1 16.0 5.1

Temp.
(~'C) 40 25 >25 < - 193 40 40 40 40 >25 <-193 40 40 40 >25 40 40

Ae (millistrain) - - 11.31 - 11.4 > - 11.4 < - 12.75 - 11.31 - 11.31 - 11.3i - 11.31 > - 11.46 <-I3.62 - 11.3i - 11.31 --11.31 >-11.65 -11.31 - I1,31

af (GPa) - 1.97 - 1.98 > -I.98 < -2.22 - 1.97 - 1.97 - 1.97 - 1.97 > - 1.99 <-2.37 - 1.97 - 1.97 -1.97 >-2.03 -1.97 -I.97

G~ (J m - " ) 6.7 9.0 <4i > 34 8.1 7.3 213 20.7 <42.5 >41,9 6.7 301 8.1 <49.7 357 114

Deb.

location
DLC/Ti DLC/~AI/Ti DLC/A1DLC/MS DLC/MS DLC/AI AI/MS DLC/SS DLC/SS DLC/SS A1/SS AI/DLC AI/DLC

--x x ~ --~" x x --tl ---

Residual stress levels (and hence strain energy release rates) were calculated using deposition stress values (see Table 3) and the following thermal expansivity data [41]:.XDLC=2.3 X t0 - 6 K - ~ , evi = 8 . 5 x 1 0 - - 6 K - z , ~Ms = 12.2 x 10 - 6 K - t , ~ s s = I6 x 10 -6 K - 1 , c~aa=24 x I 0 - ~ K - 1 . T h e D L C deposition conditions for all of these specimens were: i0 P a a n d - 1 0 5 V bias voltage.

400, 350
2

3O0 250

Ti MS ss AI

e-,

"g 200 e
150 'U

10o
50

As-polished

Pre-cleaned A1 Interlayer Interface

Oxidised

Fig. 2. Experimental data showing the effect of various treatments of the substrate prior to deposition of DLC on the interfacial toughness, for different substrates.

was thus one between the DLC and an oxide layer, as for the cases of metal substrates not subjected to precleaning or interlayer deposition.

4. Conclusions The following conclusions can be drawn from this work. (1) DLC films deposited from methane RF glow discharge showed high intrinsic stress in the range from - 0 . 5 to - 2 . 0 GPa, which increased with the

average energy of the impinging ions at first and then decreased. (2) When DLC coatings are deposited under standard conditions onto mechanically polished substrates of titanium, mild steel or stainless steel, debonding tends to take place readily. The interracial toughness for all these cases has been estimated at about 7 J m -2. This low value is attributed to the presence of oxide layers. For aluminium, on the other hand, the toughness was quite high, at over 100 J m-:. In this case, the oxide layer was presumably very thin and coherent, so that it did not readily promote debonding. (3) For the two steels, an in situ precleaning process applied to the substrate, involving bombardment by argon ions, raised the interfacial toughness considerably, to values in excess of 2 0 0 J m -a. This is presumed to be associated with the effective removal of the oxide layers. In the case of aluminium, the toughness was raised to a very high value of over 300 J m -a. This may have been caused by a small reduction in oxide layer thickness and general removal of contamination. For the titanium substrate, on the other hand, the precleaning process did not significantly affect the interfacial toughness. Apparently, a relatively thick oxide tends to reform quickly in this system, inhibiting good bonding. (4) For the titanium and the two steels, the introduction of an aluminium interlayer by sputter deposition has been found to effect a significant increase in the interfacial toughness, to around 40-50 J m -z. This

X,L. Peng, T.W. Clyne / Diamond and Related Afaterials 7 (1998) 944-950

949

(a)
"T.

Ti
After deb~?nding of DLC film .......

Before deposition of D L C film I

Ti ,.A,.
:' ........

A1

Ti

"'1 . . . . . . . . . . . . . . . . .

1'"

~:

' .........

.....................

2
I

4 6 Energy (keV) Ti
......... - -

10

(b)

Before deposition ()t D LC film After debondlng of DL C fiim

! "~

"'7.

>

Ti

AI

Ti

i,L ........

............

F'

'" . . . . . . . . I. . . . . . . . . . . . . . . .

r .....

"-

6 Energy (keV)

10

Fig. 3. EDX spectra from free surfaces produced with titanium substrates and aluminium interlayers (a) without and (b) with prior oxidation of the interlayer prior to DLC deposition.

is consistent with the good bonding observed between DLC and A1 substrates and with a sputtered A1 layer adhering well to a cleaned metallic substrate. However, when the sputtered A1 layer was exposed to air before the DLC was deposited, then the interfacial toughness was reduced to values fairly close to those in the absence of any precleaning or interlayer deposition.

Acknowledgement
Financial support has been provided for one of the authors (XLP) by the Cambridge Overseas Trust (COT) and ORS.

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