Pulsed DC unbalanced magnetron sputtering of hard solid lubricant

coating for dry machining of aluminium alloy

1
Gangopadhyay S., 2Acharya R., 3Chattopadhyay A. K., 3Paul S.
1
Research Scholar, Department of Mechanical Engineering, IIT Kharagpur, PIN: 721 302
E-mail: soumya@mech.iitkgp.ernet.in
2
M.Tech student, Department of Mechanical Engineering, IIT Kharagpur, PIN: 721 302
E-mail: acharya.ranadip@gmail.com
3
Professor, Department of Mechanical Engineering, IIT Kharagpur, PIN: 721 302
E-mail: akc@mech.iitkgp.ernet.in
E-mail: spaul@mech.iitkgp.ernet.in

Abstract:- Low friction, hard and wear resistant TiN-MoSx composite coating was
deposited by closed-field unbalanced magnetron sputtering (CFUBMS) with simultaneous
activation of Ti and MoS2 targets in N2 gas environment. Ti-MoSx composite and pure MoSx
coatings were also deposited for comparison of coating properties. The deposited films
were characterized using Field Emission Scanning Electron Microscopy (FESEM), Grazing
Incidence X-Ray Diffraction (GIXRD), scratch adhesion test, Vickers microhardness test
and pin-on-disc test. The performance test of the coated tools was evaluated in dry turning
of ISO: AlSiMg alloy. Analysis of the coated tools after machining by optical microscopy,
FESEM and Energy Dispersive Spectroscopy (EDS) clearly showed reduced formation of
built-up material over the rake surface of the coated insert compared to that of uncoated
insert. This resulted in better surface finish of the machined workpiece. All the results
clearly suggest the superior performance of TiN-MoSx composite coating over pure MoSx
and Ti-MoSx composite coating.

Keywords: TiN-MoSx composite coating, CFUBMS, aluminum alloy, surface finish.

1. INTRODUCTION [2]. The historical use of MoS2, the most commonly

The costs of maintaining and eventually
disposing of cutting fluids, combined with the health
and safety concerns and stricter environmental
regulation, have led to a heightened interest in either
eliminating cutting fluid altogether, referred to as dry
machining, or limiting the amount of cutting fluid
applied in case of near dry machining or minimum
quantity lubrication (MQL). Advances in the types of
coatings applied to cutting tools have been the major
factor in improving the feasibility of dry machining
[1]. However, desirable performance can be expected
if it is possible to develop a coating having excellent
resistance to thermal and mechanical wear while
generating less frictional heat during machining.
Solid lubrication has been known and used for
decades in specialized applications where liquid or
grease lubrication is either undesirable or ineffective
used solid lubricant material, in spacecraft can,
therefore, be extended to industrial environments
such as in dry machining or MQL. The superior anti-
adhesive properties of MoS2 coating, in particular,
has made it an attractive choice for machining sticky
materials like aluminium and aluminium alloys under
dry or near dry environment. However, it is a
considerable challenge to sustain a soft coating like
MoS2 with its low strength and poor oxidation
resistance under atmospheric and humid condition
along with lower coating adhesion. A great deal of
research work has been carried out to enhance the
tribological properties of MoS2 coating in humid
environment by incorporation of different metal
dopants like Au, Pb, Ti, W, Cr, Zr etc. [3,4]. Though
some of these coatings have been found to be
effective in drilling and milling operation [5,6], these
could not be successfully used in continuous turning
operation because of higher machining temperature
encountered [7]. Therefore, TiN being one of the
versatile coating material for cutting tools owing to
its high hardness and excellent wear resistance
properties can be thought of a promising candidate
for co-deposition with MoS2. Though, TiN-MoS2
composite coating with Ti-TiN graded interlayer has
been reported to have good mechanical
characteristics [8], its exploit as a coating material for
cutting tools especially in dry machining application
is yet to be studied.
Closed-field unbalanced magnetron sputtering
(CFUBMS) has become one of the widely used PVD
technologies because of close compositional and
microstructural control, good adherence and coating
uniformity [4]. Recent advancement in pulsed dc
magnetron sputtering has further widened the scope
of improvement of properties of functional coatings
mainly in terms of densification of coating and film-
substrate adhesion due to effective arc suppression
and higher substrate ion current density during
deposition [9]. This deposition technology is
particularly beneficial in reactive sputtering of
oxides, nitrides (e.g. Al2O3, TiN etc.) [9,10] and non-
reactive sputtering of dielectric materials like MoS2
[11].
In the present study, TiN-MoSx composite
coating was deposited by closed-field unbalanced
magnetron sputtering (CFUBMS) using separate
MoS2 and Ti target in N2 gas environment. Pulsed DC
power supply was used for both the targets and
substrate bias. Pure MoSx and Ti-MoSx composite
coating have also been deposited for comparison of
properties with TiN-MoSx composite coating. The
coatings deposited on cemented carbide turning
inserts were used in dry turning of ISO: AlSiMg
aluminium alloy. The formation of built up layer on
the tool surface and surface finish of machined
workpiece have also been studied for both uncoated
and coated tools.
2. EXPERIMENTAL DETAILS
2.1 Deposition of Coating
Deposition was carried out on cemented carbide
inserts (ISO K10 grade, make: Widia, geometry:
SPUN 12 03 08), C 40 steel discs for tribological
studies and M2 grade HSS test coupons for other
characterization tests. The steel substrates were
polished to a roughness value of Ra = 0.05 µm and
then thoroughly cleaned ultrasonically with
trichloroethylene and isopropyl alcohol prior to
deposition. Ti-MoSx and TiN-MoSx composite
coatings were deposited by simultaneous activation
of vertically mounted Ti and MoS2 target with or
without N2 gas environment. A hard TiN underlayer
was also deposited prior to co-deposition to improve
the load bearing capacity of the coating. Pure MoSx
coating was also deposited for comparison of coating
properties. However, in all cases a thin (~100 nm) Ti
interlayer was deposited to promote improved film-
substrate adhesion. All the coatings were deposited
by a dual cathode closed-field unbalanced magnetron
sputtering system (TOOL COATER, VTC-01A)
manufactured by Milman Thin Films Pvt. Ltd., India.
Both the targets as well as the substrate bias were
powered with three pulsed DC power supplies, each
of 10 kW with variable voltage and current
controllers. The power supplies were operated with a
pulse frequency (f) of 35 kHz and duty cycle of 90%
both for the cathodes as well for the substrate bias
throughout the entire deposition cycle and for all the
coating architectures. Ar and N2 gas flow were
individually controlled by mass flow controllers. All
coating architectures were deposited at a working
pressure of 0.3 Pa, substrate temperature of 2000C
and pulsed substrate bias voltage of -50 V.
2.2 Physical Characterization
Surface morphology and structure of the
coatings were studied by a high resolution Carl Zeiss,
Supra 40 field emission scanning electron
microscope (FESEM). The composition of the as-
deposited films was determined by energy dispersive
spectroscopy (EDS) coupled with FESEM. Grazing
Incidence X-ray Diffraction (GIXRD) was used for
the verification of the crystal phases of the coatings.
Diffraction studies were carried out with a high
resolution Philips, PANalytical PW 3050/60 X’Pert
PRO instrument using Cu Kα radiation at an incident
angle of 20. A 2θ scan range from 100 to 800 (for Ti-
MoSx and TiN-MoSx composite coatings) and 100 to
600 (for pure MoSx coating) were selected. The
voltage and current settings were 45 kV and 40 mA
respectively. The samples were continuously scanned
with a step size of 0.050 (2θ) and a count time of 2s
per step. The data were later analysed with X’pert
High score software and peaks were identified by
comparing with standard JCPDS data files.
2.3 Scratch Adhesion Test
The film-substrate adhesion was studied by a
TR-101M5, DUCOM scratch tester. The scratch tests
were performed with a Rockwell C diamond stylus
(0.2 mm radius) drawn across the surface of the
coating at a constant linear speed of 12 mm/min. The
normal load was varied linearly from 5 to 70 N.
Adhesion performance is usually quantified as the
normal load required to delaminate the coating and is
referred to as critical load Lc. This corresponds to the
abrupt change in the friction or tangential force
required to drive the diamond stylus across the
coating. Hence, Lc was determined from the plot of
friction force (or coefficient of friction) with respect
to scratch length. However, further analysis by
optical microscopy and EDS was also carried out to
show the exact location of coating failure in order to
confirm the critical load for each test.
2.4 Vickers Microhardness Test
Vickers microhardness tests were carried out in
order to determine composite film hardness using a
LM-700 Digital Indentation Tester, LECO with a
Vickers Indenter, LECO (standardized in accordance
with ASTM E92). At least five indentations were
considered under 0.1 N load for each sample
followed by observation under FESEM for better
accuracy of measurement.
2.5 Pin-on-Disc Test
Pin-on-disc tests were carried out using a
tribometer (TR-201-M3, DUCOM) to investigate
friction and wear properties of various coating
architectures studied. The material for the pin has
been selected similar to that of workpiece selected for
machining trial i.e. AlSiMg alloy. C 40 steel discs,
each of 25 mm diameter, were deposited with
different coating architectures studied. The tests were
performed at 20 N loads at track diameter of 20 mm.
The tests were continued for 15 min. with a linear
speed of 30 m/min. (720 m of track length) or until
coating failure. All the tests were carried out at room
temperature (25-270C) and 50±5% relative humidity.
The wear tracks were later studied with FESEM and
EDS.
2.6 Performance Test in Dry Machining
The performance test of the coated cemented
carbide inserts was evaluated in dry turning of
AlSiMg alloy and then compared with the
performance of an uncoated tool. The tests were
carried out in a CNC turning centre (LMW, Pilatus
20T). The four different cutting speeds, V of 150,
200, 250, 300 m/min. were selected for the present
study with constant feed, f of 0.1 mm/rev and depth
of cut, d of 1 mm. The cutting tools after machining
were analysed by optical microscopy and energy
dispersive spectroscopy (EDS). The surface
roughness of the machined workpiece was measured
by a surface profilometer (Make: Taylor Hobson,
Model: Surtronic 3+).
3 RESULTS AND DISCUSSION
3.1 Physical Characterization
Figure 1 shows the FESEM fractograph and
surface morphology of different coating
architectures. It depicts the coating thickness in the
range of 1- 1.5 µm and the formation of
nanocrystalline grains during pulsed dc sputtering at
the given conditions. Bulk EDS analysis on the top
surface of the coating indicates the presence of
around 25-30% of Ti (atomic %) in both TiN-MoSx
and Ti-MoSx composite coating. However, other
literatures available on TiN-MoSx composite coating
reported much lower presence of MoSx phase (around
8%) [8, 12]. The GIXRD spectra for different coating
architectures, as shown in Fig. 2, clearly reveals that
application of pulsed power supply both at the targets
as well as for the substrate bias during magnetron
sputtering resulted in strong basal orientation of (002)
plane even for pure MoSx coating with little trace of
edge planes e.g. (102) and (103). However, co-
deposition with Ti or TiN led to the suppression of
reactive edge planes as evident from Fig. 2. Such
Coating
Coating Surface
Architec
fractograph morphology
tures
MoSx
TiN/
Ti-
MoSx
TiN/
TiN-
MoSx
Fig. 1. Coating fractograph and surface morphology
of different coating architectures
basal orientation of MoS2-based solid lubricant
coatings is particularly more effective for tribological
performance [11]. Figure 2 also indicates that the
TiN-MoSx composite coating contains peaks for
different TiN phases ((111), (200), (220)) as well as
one hexagonal MoSx (002) phase. Hence it can be coating architectures. Figure 4 shows a representative
concluded that MoSx and TiN phase tend to maintain optical micrograph showing the initiation of coating
separate entity in the proposed coating architecture delamination in a scratch test for TiN-MoSx
and distinct presence of MoSx phase in the spectrum composite coating.
exhibits the existence of MoSx in compound form and
not only as elemental Mo and S as suggested in other
literatures [12]. However, in case of Ti-MoSx Scratch direction
composite coating no separate peak for elemental Ti
could be detected. This signifies that Ti could not be
present in free form in co-deposited matrix [4].

5000
a : M o S 2 (0 0 2 ) Coating delamination
a b : M o S 2 (1 0 2 )
4000 c : M o S 2 (1 0 3 )
Fig. 4. Optical micrograph of scratch track showing
Intensity (a.u.)

d : T iN (1 1 1 )
3000
e : T iN (2 0 0 )
f: T iN (2 2 0 )
the initiation of coating delamination
s : s u b s tra te
d
2000
es f
3.3 Vickers Microhardness Test
1000 b c M o S 2 -T iN c o d e p o s itio n
M o S 2 -T i c o d e p o sitio n The composite hardness of different coating
0 P u re M o S 2 architectures as obtained from Vickers microhardness
0 10 20 30 40 50 60 70 80 90 test is shown in Fig. 3. It signifies that poor hardness
2θ of pure MoSx coating could be substantially
augmented by Ti-MoSx or TiN-MoSx co-deposition.
Fig. 2. GIXRD spectra of different coating It is also evident that the microhardness obtained for
architecture the TiN-MoSx composite coating (>10 GPa) is higher
than the microhardness obtained using DC magnetron
3.2 Scratch Adhesion Test sputtering (around 7.50 GPa), the latter containing
even higher atomic percentage of TiN [8]. This
Figure 3 shows average critical loads for improvement in hardness can be attributed to the
different coating architectures. Each coating showed denser coating structure resulted from higher energy
critical load in excess of 50 N. This improved film- ion flux associated with pulsed DC sputtering. A
substrate adhesion may be attributed to the enhanced typical Vickers indentation on TiN-MoSx composite
ion coating is shown in Fig. 5.

Critical Load 10.1

100 10
Vickers Microhardness (GPa)

Vickers Microhardness
80 7.9 8
72
Critical Load (N)

68
60 6
52

40 4
2.55
20 2

0 0
MoS2 Ti-MoS2 TiN-MoS2
Coating Architecture Fig.5. FESEM micrograph showing a Vickers
indentation on TiN-MoSx composite
Fig. 3. Plot for critical load (obtained in scratch coating
test) and Vickers microhardness for
different coating architectures 3.4 Pin-on-Disc Test

current density at the substrate by the application of Figure 6 shows the resulting representative
pulsed DC power for cathodes as well as for substrate coefficient of friction (μ) for different coating
bias. It is evident from Fig. 3 that adhesion of pure architectures against sliding distance under laboratory
MoSx coating could be improved by composite air condition while sliding against pin of AlSiMg
alloy. It is shown that though pure MoSx coating
exhibited lowest coefficient of friction it failed after a on the rake surface of the tools also confirms this
sliding distance of around 200 m which was evident observation. The excellent anti-sticking property of
by the rise in friction curve. However, no such failure MoSx phase present through out the
could be observed for composite coatings after a
sliding distance of 720 m. A representative FESEM
micrograph for TiN-MoSx composite coating is
shown in Fig. 7. EDS analysis on wear track confirms
the presence coating elements. Figure 6 also depicts
that μ value of TiN-MoSx composite coating was less
compared to that of Ti-MoSx coating. Superior
tribological performance of composite coating could (a) (b)
be attributed due to presence of self-lubricating MoSx
phase through out the coating combined with
excellent mechanical properties like adhesion and
hardness because of the presence of hard and wear
resistant TiN phase.

(c) (d)
0 .9
Coefficient of friction (μ)

Fig. 8. Optical micrographs of (a) uncoated and

0 .6 coated cemented carbide inserts with (b)
T i- M o S x
pure MoSx, (c) Ti-MoSx, (d) TiN-MoSx
composite coating after dry turning of
T iN - M o S x
0 .3 AlSiMg alloy
M oSx

0 .0 Uncoated
0 100 200 300 400 500 600 700 2.5 Pure MoSx
S lid in g D is t a n c e ( m ) Ti-MoSx
TiN-MoSx
Fig. 6 Pin-on-disc test results showing the 2.0
plot of coefficient of friction vs sliding
Ra(μm)

distance while sliding against a pin of

1.5
AlSiMg alloy

1.0

150 180 210 240 270 300

Cutting Speed (m/min)

Fig. 9 Plot of surface roughness vs. cutting speed in

dry turning of AlSiMg alloy

composite coating combined with superior

mechanical properties due to presence of TiN phase
Fig. 7 FESEM micrograph of a wear track for TiN- is primarily responsible for this. However, there is
MoSx composite coating little tendency of aluminium sticking on the surface
of pure MoSx coated tool. The comparatively poor
3.5 Performance Test in Dry Machining adhesion and oxidation resistance of pure MoSx
coating might lead to partial removal of coating at
Figure 8 shows the condition of uncoated and reasonably high cutting velocity. The reduced
coated cemented carbide inserts after machining of tendency of formation of built-up material on the
AlSiMg alloy with V of 300 m/min., f of 0.1 mm/rev coated tools was also reflected on the surface finish
and d of 1 mm. The optical micrographs clearly of the machined workpiece as indicated in Fig. 9. It
indicate that the maximum built-up of material can also be seen that increase in cutting speed from
occurred on uncoated tool and it was minimum for 150 to 200 m/min. for pure MoSx coated tool resulted
TiN-MoSx composite coating. Detailed EDS analysis
in some increase in surface roughness of machined
surface. This is possibly due to partial removal of
coating at higher cutting velocity. However, presence
of a thin layer of solid lubricant coating, as detected
by EDS analysis, even at higher cutting speed
resulted in better surface finish compared to its
uncoated counterpart. The best surface finish was all
along obtained for TiN-MoSx composite coating
because of minimum built-up material over the rake
surface of the tool.
4. CONCLUSIONS
Remarkable improvement in mechanical and
tribological properties could be achieved for TiN-
MoSx composite coating deposited by pulsed dc
magnetron sputtering thereby overcoming the
limitation of pure MoSx coating like poor adhesion,
low hardness and unacceptable tribological
performance in humid atmosphere. The presence of
TiN phase in the composite coating with superior
mechanical properties like hardness, wear and
oxidation resistance at elevated temperature makes it
a better choice than Ti-MoSx composite coating.
Encouraging result was also obtained in dry turning
of aluminium alloy with TiN-MoSx composite
coating where formation of built-up material could be
successfully reduced finally resulting in much
improved surface finish of the machined workpiece.
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