Beruflich Dokumente
Kultur Dokumente
Department of Accounting and Information System, Chang Jung Christian University, No. 396, Section 1, Chang Jung Road, Kway Jen, Tainan 711, Taiwan
b Department of Mechanical Engineering, National Cheng Kung University, Tainan 701, Taiwan
c Department of Mechanical Engineering, Air Force Institute of Technology, Gang Shan, Kaoshiung 820, Taiwan
Received 15 July 2004; accepted 25 September 2004
Abstract
In this study, the TiN/AlN nano-multilayer films were prepared using a new sputtering set-up, that was designed and manufactured on the
basis of a newly developed technologythe high-rate reactive sputtering deposition process. This set-up featured an unbalanced magnetron
sputtering system and a balanced magnetron sputtering system. The former was employed to deposit the AlN film, and the latter the TiN film.
The aim of this study was to obtain, through controlled deposition conditions, a group of TiN/AlN nano-multilayer films with various periods
(TiN/AlN twin-layer thickness) first, and then to investigate the influence of periods on their fundamental properties and wear behavior.
Finally, two sets of field tests, micro-drilling and turning, were conducted in order to understand the feasibility of applying the multilayers on
actual machining.
The results revealed that through controlling of the deposition parameters, the TiN/AlN nano-multilayer films with periods ranging from
2.4 to 67.6 nm were obtained. At periods 3.6 nm, the multilayers had extremely high hardness, excellent adhesion and wear performance.
The field tests confirmed the nano-multilayers could provide a significant improvement in actual machining performance, as compared with
the traditional single-layer TiN film.
2004 Elsevier B.V. All rights reserved.
Keywords: TiN/AlN nano-multilayer films; Wear; Turning; Micro-drilling
1. Introduction
Today, studies and developments on nano-scale materials
are attracting attention in every field, for some materials with
nano-scale size showing anomalous properties that are very
different from the bulk state. In the meantime, progress in
the development and utilization of physical vapor deposition
(PVD) facility has made it very easy to tailor precise composition and structure of films according to service requirements
[1]. The studies on the multilayer films with variations in
nano-scale composition have found outstanding mechanical
performances, e.g. high hardness and good wear resistance
[26].
Corresponding author. Tel.: +886 6 2785123x2201;
fax: +886 6 2785683.
E-mail address: shyao@mail.cju.edu.tw (S.H. Yao).
0921-5093/$ see front matter 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2004.09.050
Jensen et al. [7] summarize that a multilayer film overcomes deficiencies of each single-layer film. The advantages
associated with a multilayer film are briefly: (1) it can have a
higher strength and toughness than that of each single-layer
film [8,9]; (2) with limited thickness, it can have mechanical strength equal to or exceeding each single-layer film, and
thus a lower deposition duration is required; (3) with desired
combinations of different kinds and compositions of singlelayer films, it can be tailored depending on application needs;
(4) an increase in the adhesion can be obtained between the
multilayer film and the substrate; (5) the residual stresses can
be reduced inside the multilayer film, and (6) a denser film
structure can be obtained [10].
Titanium nitride (TiN) with the NaCl-type crystal structure, exhibits high hardness, high chemical stability, and excellent adhesion to substrates, that make TiN the most popular
film used on cutting tools and forming molds [1113]. Alu-
S.H. Yao et al. / Materials Science and Engineering A 392 (2005) 340347
341
anced magnetron sputtering system and a balanced magnetron sputtering system, as shown in Fig. 1. In the front view,
at the center is the specimen holder, on the left the unbalanced
magnetron sputtering system, and on the right the balanced
magnetron sputtering system. Each system had two targets.
The specimen holder was kept rotating during deposition to
maintain the uniformity of film thickness. The unbalanced
magnetron sputtering system was connected to an oscillator
operated at a medium frequency (mf), that was half of radio frequency (rf). The manufacturer named this an mf twin
unbalanced and balanced magnetron sputtering system. The
set-up was designed with two different systems for users to
choose a suitable system depending on the target materials.
Moreover, both systems could be operated simultaneously to
prepare multilayer films.
2.2. Deposition
In this study, Ti targets were used in the balanced magnetron sputtering system, and Al in the unbalanced magnetron
sputtering system. Both systems were operated simultaneously to grow the TiN/AlN nano-multilayer films (referred
henceforth as multilayer) with various periods. The periods
were varied by controlling the deposition conditions. Prior
to growth of the multilayer, a Ti interlayer was deposited on
the substrate to enhance the adhesion of the multilayer to the
substrate.
The substrate materials were Si wafer, and high-speed
steel (SKH51, JIS) and medium carbon steel (S45C, JIS) bars.
To avoid the substrate effects, (1 0 0) Si wafers were used to
grow multilayers for the quantitative analyses. SKH51 and
S45C substrates were machined to the desired shapes and then
heat-treated to Rockwell hardnesses of HRc 55 and HRc 28,
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Table 1
Deposition conditions for TiN/AlN nano-multilayers
Code
N10
N13
N15
N17
N20
0.5
10
13
15
17
20
R1
R2
R3
R4
R5
TiN
1
2
3
20
4
5
Multi-arc plasma-aided PVDa
Refer to [19].
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Table 2
Compositions, thicknesses and periods of TiN/AlN nano-multilayers
Code
Element (at.%)
Thickness (m)
Period (nm)
Ti
Al
N10
N13
N15
N17
N20
5
20
26
31
35
49
46
45
41
41
46
34
29
28
24
2.9
3.8
3.6
3.1
1.6
50.6
67.3
67.6
54.6
27.3
R1
R2
R3
R4
R5
44
45
48
50
50
38
39
34
34
33
18
16
18
16
17
1.5
1.5
1.3
1.3
1.4
12.7
6.4
3.6
2.7
2.4
TiN
47
53
as the flow rate of nitrogen gas increased, the N content increased, and the Ti content slightly decreased, while the Al
content decreased significantly. The N content in N10 was
very low, that might be due to very low nitrogen gas flow
rate. The R1R5 analyses showed that as the rotation speed
increased, the N and Ti content slightly increased and decreased, respectively, and the Al content almost remained
constant. In particular, when the elemental compositions for
N10N20 and R1R5 are compared, it is found that Al content and to some extent the Ti content in the films R1R5 has
decreased and the N content increased. It can be rationally
inferred that the increase in the N content resulted from the
increase in the rotation speed. When the rotation speed increased, the number of layers of a film increased; thus, there
were more possibility and space for N atom to be trapped
as interstitial atoms. However, the actual reason needs to be
investigated further.
The thickness of films N13N20 decreased with increasing the flow rate, with the biggest value for N13. It was noted
that the thickness reduced abruptly for N20. The N20 thickness was very low, even lower than half of thickness of N15.
The R1R5 analyses results showed that the thicknesses were
almost not affected by the changes in the rotation speeds.
According to the reports of Setoyama et al. [6] and Kim et
al. [20], the period () of a nano-multilayer can be calculated
using the relationship between the overall thickness of a nanomultilayer film and the rotation speed. The calculated periods
are also listed in Table 2. As can been seen, by controlling
the flow rates and the rotation speeds, the multilayers with
periods ranging from 2.4 to 67.6 nm were obtained.
Fig. 4 shows the X-ray diffraction patterns of the multilayers that were grown under different deposition conditions.
The diffraction pattern of N10 showed that elemental Ti and
Al are present, confirming that the nitrogen gas flow rate
is too small. Thus, the formation of TiN and AlN was not
complete. The diffraction pattern of N13 was similar to that
of N10, in which the elemental Ti and Al can be seen. In
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hardness increases to a high value. All the multilayers possess hardness higher than AlN. The hardness of single-layer
TiN lies between R2 and R3.
Fig. 6 shows the relationship between the critical loads
of the multilayers and the periods. As can been seen, except
N10 and N13, the Lc value of the multilayer increases with
a decrease in the period. The Lc values of N10 and N13
are relatively much lower. When the period is shorter than
3.6 nm (R3), the Lc value increases drastically. The adhesion
of single-layer TiN is near to that of R2.
The XRD analyses (Fig. 4) indicate that N10 and N13
multilayers contain Ti and Al. Fig. 5 and Fig. 6 show that the
hardness and adhesion of N10 and N13 is relatively much
lower. Therefore, these two multilayers will not be considered
in the following studies.
3.4. Wear test
Fig. 7 shows the dependence of wear depth and friction
coefficient of the multilayers on the period. It is clear that the
wear resistance of the multilayers increases with a decrease
in the period. The R3R5 multilayers with periods shorter
than 3.6 nm possess excellent wear resistance. The value of
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345
the friction coefficients decreased gradually as the period decreased. For R3R5, the friction coefficient dropped abruptly;
the values are nearly equivalent to that of the single-layer
TiN. However, the wear depth values of R3R5 multilayers
are merely one third of that of the single-layer TiN, and one
fourth of that of the uncoated specimen.
The wear tests show that R3, R4 and R5 multilayers have
remarkably excellent wear performance. Thus, these three
multilayers were chosen for growth on micro-drills and turning cutters to perform field tests with an aim to approve the
feasibility of applying these multilayers on actual machining.
3.5. Micro-drilling test
Fig. 8 shows the experiment result of the micro-drilling
test. Comparing the result of R3, R4 and R5, although R4
shows a little better drilling performance, the three multilayers may be regarded as equal competitors. The multilayers
provide more improvement in drilling performance than the
single-layer TiN film. Remarkably, the multilayers largely
Fig. 8. Corner wear of micro-drills with different coatings vs. drilled holes.
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4. Discussion
Fig. 10. Flank wear of turning cutters with different coatings after turning
test.
Fig. 11. Wear morphology of turning cutters with different coatings after turning tests observed under SEM: (a) flank wear, single-layer TiN; (b) flank wear,
R4 TiN/AlN nano-multilayer film; (c) cutting edge wear, single-layer TiN; and (d) cutting edge wear, R4 TiN/AlN nano-multilayer film.
S.H. Yao et al. / Materials Science and Engineering A 392 (2005) 340347
than 3.6 nm, the hardness (Fig. 5), adhesion (Fig. 6) and wear
performance (Fig. 7) increase remarkably, which results from
the transformation of AlN to cubic form in the multilayers.
The X-ray diffraction analyses shows that the period 3.6 nm
(Fig. 4(e)) is the value at which the AlN starts to transform
from Wurtzite-type to NaCl-type. As the period decreases,
the fraction of Wurtzite-type AlN decreases gradually. When
the period is as short as 2.4 nm (Fig. 4(f)), the Wurtzite-type
AlN almost transforms to NaCl-type AlN. At this period, the
hardness reaches the maximum value. These findings concerning AlN transformation with the periods have been reported before by Setoyama et al. [6] and Kim et al. [20], and
are confirmed again here.
According to the works of Paney et al. [21], Christensen et
al. [22], and Ueno et al. [23], AlN transforms from Wurtzitestructure to NaCl-structure under pressure of 16.622.9 GPa.
This is accompanied by 18% volume reduction. On the basis
of calculation of Christensen et al. [23], the bulk modulus
increases from 205 to 270 GPa, when the structure of AlN
changes from Wurtzite-type to NaCl-type. Experimentally,
hardness increases with bulk modulus, so that NaCl-type AlN
is harder than Wurtzite-type AlN.
Thus, the ultra-high hardness, excellent adhesion and wear
resistance of the R3R5 multilayers with periods 3.6 nm results from the formation of NaCl-type AlN. R3R5 multilayers applied on micro-drills for hole-drilling on circuit boards
and on turning cutters for turning medium carbon steel bars,
shows that the multilayers can be utilized on machining applications and a 40% wear improvement can be achieved.
From the practical point of view, the end users replace the
uncoated micro-drills after drilling 5000 holes. Our experience shows that the hole tolerance is too large to be accepted
after drilling to some degree more than 5000 holes. In Fig. 8,
the corner wear of uncoated micro-drills corresponding to
5000 holes is about 35 m. For the R4 multilayer-coated
micro-drills, the corner wear is only 32 m after 20,000 holedrilling. That is, the R4 multilayer-coated micro-drills have
four times longer service life than the uncoated micro-drills.
5. Conclusion
In this study, a newly developed technologythe highrate reactive sputtering deposition processwas employed to
deposit the TiN/AlN nano-multilayer films. Through controlling the nitrogen gas flow rates and the specimen holder rotation speeds, the multilayer films with periods ranging from
2.4 to 67.6 nm were obtained. At the periods 3.6 nm, the
347