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Abstract
Reliability of MEM (microelectromechanical) devices can be limited by stiction forces that
develop in use. It is desirable to alter the mechanical and interfacial behaviour of the silicon
surfaces by the application of very thin, low surface energy and low stress coatings. In this
publication we report the nanomechanical and nanotribological characterization of a range of
5–150 nm thin films deposited on silicon by filtered cathodic vacuum arc (FCVA) and closed
field unbalanced magnetron sputtering. A method of analysing nano-scratch data with
spherical indenters is proposed. The method suggests the onset of non-elastic deformation in
the nano-scratch test is due to substrate yield rather than film deformation on all but the softest
films studied in this publication. The critical load for total film failure is a marked function of
indenter radius, the ratio of hardness to modulus and the film thickness. The FCVA films were
tested with probes of different radii (1.1, 3.1 and 9.0 µm) and the critical load for film failure
was found to vary strongly with probe radius. The deposition of <100 nm amorphous carbon
films on Si could be a promising strategy for improving the reliability of Si-based MEMS
devices as none of the very thin films tested underwent stress-related delamination failures that
occur behind the indenter during the nano-scratch testing of thicker amorphous carbon films.
on thinner (200 nm) a-C films neither this deformation mode were ultrasonically cleaned with deionized water for 10 min,
nor strong dependence on substrate bias was observed, and followed by drying with a static neutralizing blow off gun. The
films with the highest H /E showed slightly improved scratch samples were placed in the deposition chamber of an industrial
resistance. It was therefore suggested that a suitable strategy filtered cathodic vacuum arc system (Nanofilm Technologies
for optimizing wear resistance for even thinner films for Pte. Ltd.) evacuated to a base pressure lower than 1×10−6 Torr.
MEMS applications is to aim to maximize H /E [7]. In this Prior to deposition, the silicon surface was sputtered by an
current publication we have tested this hypothesis and have argon ion beam from a dc ion beam source for 3 min to
extended the testing to include thinner films and report the remove the native oxide. The substrate holder was in floating
nanomechanical/nanotribological characterization of a range bias. The film thickness of the 20–80 nm films was measured
of 5–150 nm experimental thin films deposited by filtered by a surface profiler and the thickness of the 5 nm film was
cathodic vacuum arc (FCVA) and closed field unbalanced estimated from the deposition rate. Experimental metal-
magnetron sputtering (CFUBMS). Ta-C films deposited by containing molybdenum disulphide (MoST) 70–150 nm and
FCVA have been developed for MEMS applications including 70 nm a-C : H films were deposited on Si wafers using a
capacitive sensors and protective coatings for micromachined teer coatings closed field unbalanced magnetron sputtering
components [8–10]. They have a high sp3 fraction of carbon ion plating (CFUBMSIP) technique. The methodology for
atoms (over 80%) conferring high hardness, but the films producing these films is described in detail elsewhere [13, 14].
can be highly stressed [11, 12]. In contrast, the CFUBMS In contrast to the usual deposition conditions for CFUBMS no
deposition process is capable of producing dense, low stress interlayer was deposited for these experimental samples and
coatings, which are typically somewhat softer than the films their composition was not through-thickness graded.
deposited by FCVA [13, 14]. The nano-scratch and nanowear
resistance of FCVA ta-C films has been studied previously with 2.2. Nanoindentation and nano-scratch testing
spherical probes of 100–1200 nm resulting in critical loads in
the range 0.1–7.5 mN [15–18]. Ichimura and co-workers have Nanoindentation and nano-scratch tests were performed with
noted that the critical load in scratch testing of ∼2.5 µm hard a Micro Materials NanoTest, details of which are provided
coatings on steels with indenter radii 100–400 µm followed a elsewhere [18], fitted with a high resolution NTX controller
complex dependence on probe radius that could be explained enabling indentations at lower forces. Nanoindentation
by equation (1): was performed using a Berkovich indenter at applied loads
of 0.1–10 mN. Nano-scratch tests were performed with a
Lc = 2πRγ δcr Hcr , (1) spheroconical diamond indenter of (3.1 ± 0.1) µm end radius.
The scratch tests were performed as multi-pass tests at
where γ is a proportionality constant, δcr is the critical 2 µm s−1 over a 150 µm track with (1) pre-scratch topographic
depth at failure and Hcr is the composite scratch hardness scan, (2) a levelling distance followed by a ramped scratch
at the same load. Equation (1) shows that the critical load and (3) a post-scratch low load scan. In the pre- and post-
increases proportionally with the indenter radius only when scratch scan the applied load was sufficiently low (0.05 mN)
the contact depth at failure and the composite hardness do not that no wear occurs (‘off-load scans’). In the ‘on-load’ scratch
change [19, 20]. scan the load was ramped after 20 µm travel at 2.5 mN s−1 to
It is of interest to investigate the variation in measured reach 160 mN at the end of the scan. At least three repeat
critical load with the radius of the spherical probe for these tests were performed to test the reproducibility of scratch
thin films. Very small radius probes (100 nm) have been shown behaviour. Additionally, the 20, 60 and 80 nm FCVA samples
to get progressively worn away on repeated testing of hard were also tested with a (9.0 ± 0.1) µm end radius probe.
films [14]. In this publication, larger precision polished probes Conditions were as above except the loading rate was increased
have been used which are less likely to blunt during the testing, to 8.0 mN s−1 so that the maximum load of 500 mN could be
have well-defined radius and produce film failures at higher reached within a 150 µm track length. The probe radii were
forces which are easily observed by optical without recourse determined by spherical indentations into fused silica. There
to post-test SEM imaging. was no evidence of any indenter wear after scratch testing.
We were also interested in comparing the scratch
resistance of films deposited by FCVA and CFUBMS. We 3. Results
investigate the failure mechanisms occurring in the nano-
scratch test, determine the yield pressures, assess film 3.1. Nanoindentation
durability and from the nanoindentation and nano-scratch
data suggest design rules for optimizing film properties for The variation in mechanical properties with increasing
enhanced scratch and wear resistance. indentation depth is shown in figure 1. It is clear from
figure 1 that the hardest samples tested were the 60 and 80 nm
ta-C films, with the 5 and 20 nm ta-C and the 70 nm a-C : H
2. Experimental
films being closer to the silicon substrate and the two MoST
2.1. Preparation of ta-C, MoST and a-C : H films films being considerably softer. As the indentation depth
reaches ∼100 nm the mechanical response of all the thin film
5–80 nm ta-C films were deposited on Si using the FCVA systems becomes increasingly dominated by the Si substrate of
process as described in [8–12]. The p++ silicon substrates hardness of 11.5 GPa, and hence the hardness of all the coated
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J. Phys. D: Appl. Phys. 42 (2009) 065301 B D Beake et al
(a)
ta-c
ta-c
ta-c
ta-c
(b)
ta-c
ta-c
ta-c
ta-c
r
3
J. Phys. D: Appl. Phys. 42 (2009) 065301 B D Beake et al
Ly/mN
Lc1/mN
Lc2/mN
(a)
4
J. Phys. D: Appl. Phys. 42 (2009) 065301 B D Beake et al
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J. Phys. D: Appl. Phys. 42 (2009) 065301 B D Beake et al
(a)
(a)
(b)
(b)
Figure 7. (a) Variation in critical load Lc2 with film thickness for
(c)
FCVA films. (b) Variation in Lc2 critical load with probe radius R.
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J. Phys. D: Appl. Phys. 42 (2009) 065301 B D Beake et al
they do not exhibit the same behaviour, showing that the effect
of film stress is less critical in these very low thickness films.
The thin films did not undergo stress-related delamination that
occurs behind the moving probe during nano-scratching of
thicker amorphous carbon films. Whilst the stress in ta-C is
known to increase with thickness this does not greatly affect
their scratch resistance over the range of thickness studied here.
The yield stress analysis presented above suggests the reason:
onset of yield is due to substrate deformation rather than film
failure. MoST films, popular in other applications due to
their low friction, may not be suitable as MEMS overcoats
as the deformation mechanism in contact involves substrate
yield and, being much softer than Si, they do not protect it
particularly well. In contrast, the 70 nm a-C : H, although
softer and lower H /E than the ta-C films of comparable
Figure 8. Scratch crack propagation resistance and scratch thickness provides reasonable scratch resistance and durability
durability ratio. and the opportunities for tailoring composition in CFUBMS
suggest harder, yet low stress, films deposited by this method
Film durability in mechanical contact is key to many may find applications as MEMS overcoats.
applications. Film durability parameters have been used to
assess the roles of film thickness and deposition route on film
5. Conclusions
durability. The 70 nm a-C : H and the 60 and 80 nm ta-C
films in particular appear to be quite durable; after Lc1 the
Si substrate undergoes plastic (not elastic) deformation—as 1. A method of analysing nano-scratch data with spherical
evidenced by the residual depth being greater than the film indenters is proposed. The method suggests the onset of
thickness—before the films fail completely and the substrate non-elastic deformation in the nano-scratch test is due to
is exposed. Total failure of the 80 nm ta-C requires an applied substrate yield rather than film deformation on all but the
load of 91 mN, significantly higher than its Lc1 of 36 mN. softest films studied in this publication.
Various measures of film durability and toughness in 2. FCVA films were tested with probes of different radii
a scratch test have been proposed recently. Zhang and (1.1, 3.1 and 9.0 µm). The critical load for film failure
co-workers have equated Lc1 with the resistance to the was found to vary with probe radius, roughly following
initiation of cracks and (Lc2 − Lc1 ) as a measure of the Lc ∝ R 1.7 . Greater plastic deformation of the Si substrate
toughness [43, 44]. They defined a parameter representing is possible before total film failure with the larger radius
resistance to crack initiation and also propagation as probes.
Scratch Crack Propagation Resistance = Lc1 (Lc2 − Lc1 ). 3. The 70 nm a-C : H deposited by CFUBMS, although
(7) softer and lower H /E than the ta-C films of comparable
thickness provided reasonable scratch resistance and
The assumption is that the crack systems are linked. Colligon durability.
and co-workers recently proposed the dimensionless scratch
4. The deposition of <100 nm amorphous carbon films on
durability ratio given by equation (8) could be a suitable
Si could well be a promising strategy for improving
parameter [45] for assessing film durability and toughness.
reliability of Si-based MEMS devices. None of the thin
Scratch Durability Ratio = (Lc2 − Lc1 )/Lc1 . (8) films tested underwent stress-related delamination failures
that occur behind the indenter during the nano-scratch
Equation (8) may enable comparison between critical testing of thicker amorphous carbon films.
loads obtained with different indenters more easily due to
the normalizing effect of dividing by the lower critical load.
Values of both parameters are shown in figure 8. For a given Acknowledgments
deposition method (FCVA) values of both indices increase
with film thickness. For a similar thickness range (60–80 nm), Funding from the UK Department of Trade and Industry for
values show some correlation with the ratio of film H /E. The the BTIA Program Project CHBL/C/019/00024 (‘Contact’—
highest durability indices were observed on the 70 nm a-C : H Creation Of Nano-Tribological Advanced Coating Technol-
and the 80 nm ta-C films. ogy) is acknowledged. Provision of ta-C samples from
A distinct deterioration in scratch resistance has been Professor Daniel Lau (Nanyang Technological University, Sin-
observed on hard relatively thick (>600 nm) films of gapore) and CFUBMS samples from Dr Xiaoling Zhang and
a-C : H [46], a-C [7], TiFeN [47] and TiSiN [25] on Si substrate Dr Kevin Cooke (both Teer Coatings Ltd) is acknowledged.
when H /Er is greater than about 0.1. Although the much Dr Norbert Schwarzer (SIOMEC) and Professor Derek Arnell
thinner FCVA films studied here are of similarly high H /E (UCLAN, UK) are thanked for useful discussions.
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J. Phys. D: Appl. Phys. 42 (2009) 065301 B D Beake et al