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high temperature friction and wear behavior of [mos.sub.2]/nb coating in ambient air.
Summary of FSCT and OCCA 2009 [MoS. sub. 2]
Known for its solid lubricant properties and used as
Lubricants in vacuum and inert gas environments, and this coating is not used in atmospheric conditions due to its deteriorating friction.
Friction performance [MoS. sub. 2]
Through a small amount of co-deposition of another metal, the solid lubricant coating in different atmospheres has been improved.
The friction behavior of [in this study]MoS. sub. 2]
The/Nb coating was studied in ambient air up to 500 [degrees]C by usinghigh-Temperature pinon-
The disk friction tester and the aluminum oxide ball are used as side surfaces. [MoS. sub. 2]
/Nb coatings are deposited on the silicon wafer and the AISI 52100 steel base by closed-deposition
Field unbalanced magnetic sputtering.
Structural analysis of the coating using x-
Technology of ray diffraction and scanning electron microscopy.
Hardness is measured using a micro hardness tester. Keywords [MoS. sub. 2]-
Introduction to Nb, solid lubricant, high temperature, friction and wear [MoS. sub. 2]
Good solid lubrication coating
Established in industrial communities.
Now, in the deposition of [the], the sputtering technology has been the most widely usedMoS. sub. 2]coatings. (1)
However, [resistance]MoS. sub. 2]
Insufficient anti-humidity coating and friction properties [MoS. sub. 2]
Under wet conditions, the coating will degrade, resulting in an increase in the friction coefficient and a shorter working life. Furthermore, [MoS. sub. 2]
The coating is easily oxidized at high temperature. (2-6)
Therefore, we have made considerable efforts to improve the friction performance [MoS. sub. 2]
Coating in wet environment.
The researchers pointed out that the addition of metal has improved the wear resistance [MoS. sub. 2].
Various metals such as Ni, Pb, Ta, Au, Ce and Cr, especially Ti, were studied. (7-11)Recently, [MoS. sub. 2]-
Ti coating provides excellent industrial results for a wide range of cutting and molding applications.
Research on [MoS. sub. 2]
/Metal composite coatings are usually concentrated on the content of the selected metal, the structural representation, and the friction behavior at room temperature and atmospheric conditions.
However, there are few studies on the friction behavior [MoS. sub. 2]
/Metal composite coating at high temperature in the literature. As is known, [MoS. sub. 2]
Metal composites are used as solid lubricants in cutting tools and are re-added to high temperatures during processing.
At these temperatures, the friction properties of the coating are negatively affected ,(12)
This limits the use and performance of the tool coating.
Improve the friction performance [MoS. sub. 2]
Nb coating was added to [under atmospheric conditions]MoS. sub. 2]
In this study, as a different additive metal than mentioned earlier.
As far as we know, there are very few studies on [MoS. sub. 2]
A composite coating of Nb was added to the literature. (13)Therefore, [MoS. sub. 2]
Coating with pulse deposition/Nbcomposite
Closed DC magnetic sputtering technology
Field Non-equilibrium magnetic sputtering (CFUBMS)ring.
The friction properties of the coating were evaluated at room temperature and at high temperature.
Details of the experiment 【MoS. sub. 2]
/Nb composite coating was deposited on AISI 52100 polished steel ([R. sub. a][
Less than or equal to]0. 12 [micro]m)
Cfubms using pulses-dc technique.
Experimental parameters are given in Table 1.
Samples were splashed before deposition
Clean with advanced energy (AE)
900 v dc magnetic control driver[MoS. sub. 2]
/Nb composite coating using the CFUBMS system shown in Figure 1
By rotating these sublayers between three MoS. sub. 2]
A target and a nb target in the argonatmosphere atmosphere. [MoS. sub. 2]
Deposit/Nb coating with niobiuminterlayer and then splash from three [MoS. sub. 2]
The target is carried out simultaneously with 1 nb target.
DC power supply (AE)
Operating in constant current mode and another pulse power mode (AE-
Pinigao plus 5 KW)
Single polarity pulse-
The dcpower on the substrate is used in this work, where the line form of the single-pole pulse used is shown in Figure 1 for example
2, and pulse ground voltage between normal operating voltage and ground voltage.
All running pulse parameters are fixed. [
Figure 1 slightly][
Study on phase change [MoS. sub. 2]
/Nb composite coating as a function of temperature, in-situ X-
The temperature connection was carried out with Cu [on the anRigaku 2200D/Max diffraction machine]K[alpha]([lambda]= 1. 5404)
Source of launch. In situ X-
Ray diffraction (XRD)
Studies were conducted at room temperature and at temperatures of 100, 300 and 500 [degrees]
C. In a vacuum where the chamber pressure is [10. sup. -2]Pa.
The heating duration at each annealing temperature is 20 minutes and the heating rate is 20 [degrees]C/min.
The microstructure [MoS. sub. 2]
/Nb composite coating, wear trajectory and the surface of the secondary surface after the wear test pass through JEOL-
6400 scanning electron microscope (SEM)
Determination of the composition of the coating by energy dispersion analysis method (EDS). The high-
Temperature friction behavior [MoS. sub. 2]
/Nb composite coating using pin-on-
CD test equipment (CSM high-
Temperature three treasures-tester).
All the experiments were done with oneAl. sub. 2][O. sub. 3]
Sliding Contact ball with a diameter of 6mm.
In the case of a linear speed of 30 mm/s, at room temperature, at temperatures of 100, 300, and 500 [tested at a load of 5 N]degrees]
Under atmospheric conditions
[Surface profile of the worn track]MoS. sub. 2]
Measuring/Nb composite coating with Sanfeng surface profile measuring instrument.
The wear volume is calculated using the profile obtained from the cross section of the wear track, so K = V /(w [period]s)
Equation where K is the value of wear rate, V is the volume of wear, w is the normal load, and s is the distance of movement.
Results and discussion of SEM micrograph [MoS. sub. 2]
/Nb composite solid lubrication coating using pulse deposition
In Figure 1, the DC magnetic sputtering technology is given. 3.
The coating thickness is about 3 [micro]
M, depending on the process time and parameters of the coating.
The Sincepulsed bias of the substrate during deposition increases the oxidation grade and ion-to-
The neutral ratio, the composite coating grows as the dense, tight, non-cylindrical structure and the characteristic coating surface as shown in the figure. 3a and 3b.
The micro-hardness of the coating is 800 HV. [
Figure 3 slightly]Fig.
3: SEM image display (a)
Cross section, and (b)
The ecological surface [MoS. sub. 2]
Composition of/Nb composite solid lubrication coating [MoS. sub. 2]
The/Nb coating was determined by EDS.
Figure 1 gives the results of EDS analysis. 4.
When the quantitative evaluation [MoS. sub. 2]
The chemometric ratio of/Nb coating was evaluated [N. sub. s]/[N. sub. Mo]
The ratio of sulfur atoms to molybdenum atoms is about 1. 64.
This proportion indicates that there is a composition close to [the coating deposition]MoS. sub. 2]stoichiometry. (14)[
Figure 4 slightly]
In order to better understand the results of friction tests performed at higher temperatures, in-situ X-ray diffraction studies were performed at room temperature and at temperatures of 100, 300 and 500 degrees]C.
The X-ray spectrum obtained from these studies is shown in the figure. 5.
The pattern obtained at room temperature includes the base surface (002)and (001)and the (101)
Edge plane of hexagonal crystal structure.
X-ray diffraction tests at room temperature show that a randomly oriented coating is deposited on the substrate.
Reflection on 2 [theta]= 13[degrees]
Display base surface (002)
Parallel to the substrate. Fleischauer (15)
Indicates that the plan provides a low
Friction coefficient between sliding surfaces.
However, the broad response reached approximately 2 [theta]=33[degrees]
It corresponds (001)and to (101)
Thinking about [theta]= 37[degrees]
Observed in [MoS. sub. 2]
Nb coating at room temperature.
In addition, the relatively broad 【Nb. sub. 1-x]
S peakis was observed in X-ray diffraction tests at room temperature.
On the other hand, there are no Nb peaks in the X-ray spectrum.
The situation is similar. MoS. sub. 2]
As shown in the literature, Ti was added ,(6)
Nb in place of [replacing] MolybdenumMoS. sub. 2]
Matrix and/or become a gap solid solution of Nb in the direction of lattice parameters [MoS. sub. 2]. [
Figure 5 Slightly]Fig.
5: in situ X-ray spectra at different temperatures [MoS. sub. 2]
/Nb composite solid lubrication coating [
Figure 6 slightly]Fig.
6: Change of friction coefficient at high temperatureMoS. sub. 2]
The function of/Nb composite solid lubrication coating as a circle in situ X-ray diffraction study at 100, 300 and 500 [j]degrees]
C, the peak obtained at room temperature was detected to change and a new peak was formed.
Base surface (002)
At these temperatures transfer to a smaller angle, and (001)peak reduced.
However, there is no big change in the rate (101)peak.
On the other hand, somesignificant observed X-in rats-
500 [ray pattern]degrees]
Cas [peak]Nb. sub. 1-x]
Reflection of S crystal is about 2 [theta]=27[degrees]and 2[theta]= 53[degrees].
This leads to the formation of a new phase of sulfur atoms diffuse according to the temperature of Nb atoms.
Figure 1 gives the relationship between the friction coefficient and the ring at room temperature and at different temperatures6 for [MoS. sub. 2]
/Nb composite coating.
From the research of pinon-
In order to determine the friction behavior of the coating at high temperature, a disk friction test was carried out, and it was observed that the friction coefficient changed significantly with the change of temperature.
It is also determined that when a very stable coefficient of friction is measured near [mu]= 0.
072 from the wear test performed at room temperature, the unstable friction coefficient was observed from the test performed at 300 [degrees]C.
This unstable coefficient of friction changes between 0. 035 and 0. 061.
The cause of this unstable behavior of friction coefficient is related to the formation [MoO. sub. x]
Through rapid oxidation [MoS. sub. 2](001)
Plane, sensitive to oxidation as the temperature rises.
In addition, the formation [Nb. sub. 1-x]
S phase has lower solid lubrication properties compared [MoS. sub. 2](16), (17)
Observed from high
Temperature friction test at 500 [degrees]
The C coating exhibits rather insufficient friction behavior.
The friction coefficient at this temperature is measured as 0.
At the beginning, the contact with Haji \'an gradually increased to about 1000 laps.
In this interval, the friction coefficient of the coating was observed from 0. 067 to 0. 14.
After about 1000 laps, the coating was completely out of strategy.
On the other hand, the present study determined the most stable and lowest coefficient of friction from the tribo test conducted at 100 [degrees]C.
The average friction coefficient at this temperature is [mu]= 0. 014.
This low coefficient of friction may be due to non-existence [Nb. sub. 1-x]
S phase at this temperature.
Observation from in situ X-ray diffraction (although[Nb. sub. 1-x]
In the S phase of 300 [formation]degrees]
C and at500 [Intensivedegrees]C)
The sulfur does not spread to the coating at100 [degrees]
C. Therefore ,[Nb. sub. 1-x]
No S phase was formed.
According to this fact ,[Nb. sub. 1-x]
At this temperature, the S phase is not formed, resulting in a stable and low friction coefficient.
The stability and instability behavior of the friction coefficient is also supported by the image of the wear track and the surface of the ball.
Figure 1 gives the image of the wear track and the image of the ball contact area at different temperatures.
7 and 8, respectively.
It is observed that wear rails at room temperature and at 100 [degrees]
C is very smooth without any debris.
Fine grinding particles determined along the track are few (Figs. 7a and 7b).
In addition, a thin and uniform film was observed on [Al. sub. 2][O. sub. 3]
Ball after needleon-
Disk tribo test was performed at room temperature and no transfer film was detected at 100 [degrees]C (Fig. 8).
On the other hand, the wear trajectory is widened at 300 and 500 [degrees]
C as shown in the figure. 7c and 7d.
Debris was found in orbit 300 [degrees]
C, this leads to an increase in the coefficient of friction (Fig. 7c).
A very dense and uneven transfer film on [Al. sub. 2][O. sub. 3]
The ball is observed at this temperature (Fig. 8b). For 500[degrees]
C. Dense wear details on the wear track and dense debris on the track were observed, and the coating fell off the substrate (Fig. 7d).
Also, from the image of the ball in the picture
8c at this temperature, the transfer film made of randomly dispersed coarse particles and not glued to the surface is determined.
These particles increase the grinding effect between the coating and the ball, causing the coating to disengage from the surface in a short period of time, and the friction coefficient increases rapidly.
On the other hand, different values of wear rate are obtained according to the test temperature. A samplewear-
Figure 1 shows the trajectory profile and wear rate at different temperatures9 as a graphic.
The coefficient of friction, the value of the wear track image and the ball image can also see the change of the wear rate.
The minimum wear rate at the end of the 5000 lap is determined in the test conducted at 100 [degrees]C.
The wear rate at room temperature and 300 [also increaseddegrees]C.
On the other hand, in the test conducted by 500 [degrees]
C, the coating falls off from the bottom layer after 1000 laps, so the wear rate of the coating cannot be calculated because the ball wears the substrate until about 2000 laps. [
Figure 7 Slightly]Fig.
7: SEM image of wear trajectory on [MoS. sub. 2]/Nbcoatings: (a)
Room temperature; (b)100[degrees]C; (c)300[degrees]C; and(d)500[degrees]C [
8: SEM images from the contact area on the ball (a)
Room temperature ,(b)300[degrees]C, and (c)500[degrees]C [
Figure 9 omittedFig.
9: wear rate [MoS. sub. 2]
/Nb composite solid lubrication coating and sample wear trajectory profile in addition, the comparison of this study with pure [j]MOS. sub. 2]
Given in Table 2.
High temperature wear test results of pure [MoS. sub. 2]
Implemented by Kubart and others. , (18)
Indicates the friction coefficient and wear rate at a temperature of 100 [degrees]
C is lower than room temperature.
Then, they increase as the temperature rises.
Although similar behavior was observed in our study, Nb-doped [MoS. sub. 2]
Compared with the determination of pure [MOS. sub. 2].
Temperature friction behavior [MoS. sub. 2]
A/Nb solid lubricant coating was studied to optimize the limited use [MoS. sub. 2]
The results of the preparation of solid lubricating coatings under atmospheric conditions and at higher temperatures are summarized.
Noncolumnar, dense, compact plating due to ofpulsed-
Dc rf sputtering technology.
Studies from in situ X-ray diffraction ,(002)plane of [MoS. sub. 2]
The reason for the low friction coefficient does not change as the temperature rises.
However, it is observed that as the temperature increases, the additional [Nb. sub. 1-x]
S phase formed by the combination of sulfur and Nb.
At this stage of the formation of degrees]
Considering the friction behavior without film failure, the optimum temperature is determined to be 100 [degrees]
C. High temperature tribo test at room temperature and at different temperatures.
The coefficient of friction is about [mu]=0.
At this temperature.
At temperatures of 300 and 500 [degrees]
C. Rapid oxidation of coating with temperature and formation [Nb. sub. 1-x]
With high S stage
Comparison of friction coefficient]MoS. sub. 2]
Resulting in an increase in the friction coefficient.
Wear details from the wear track and [observed]Al. sub. 2][O. sub. 3]
Image of the ball in 500 [degrees]
The friction coefficient is increased by C and non-uniform transfer film.
In addition, although the minimum wear rate was determined from the wear test of 100 [degrees]
C, it is determined that this rate will increase at other temperatures.
As a result [MoS. sub. 2]
The coating of/Nb composite solid lubricant presents a fairly low friction coefficient at100 [degrees]
C, suitable for industrial applications at temperatures in atmospheric conditions. E. Arslan [Message]
University of Ataturk, El zurum, Turkey
Email: earslan @ atauniedu. tr Y. Totik, O. Bayrak, I. Efeoglu, A.
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