N_2气流量比对磁控溅射Mo-N涂层结构和性能的影响
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摘要
目的研究N_2气流量比对直流反应磁控溅射Mo-N涂层结构、力学性能和摩擦性能的影响。方法采用直流反应磁控溅射技术在304不锈钢基体表面制备Mo-N涂层,对涂层结构进行X射线衍射(XRD)分析,对涂层形貌和磨痕形貌进行扫描电镜(SEM)分析,采用维氏显微硬度计测试涂层的显微硬度,采用划痕法表征涂层的结合强度,采用球盘式摩擦磨损试验仪评价涂层的摩擦磨损性能。结果随着N_2气流量比R从0.3增加至0.7,涂层主要由面心立方γ-Mo2N相构成,当R为0.7时,制备的涂层中出现少量的六方δ-MoN相。涂层的显微硬度先降低后增加,最高硬度可达3060HV。结合强度先增加后降低,当R为0.4和0.5时,涂层的结合力较高,约为40N,且具有较好的摩擦学性能,平均摩擦系数约为0.22,磨损形式主要为磨粒磨损。结论在基体温度为300℃时制备涂层,N_2气流量比在0.3～0.7的范围变化对涂层相结构的影响较小。硬度相对较高时,结合力越好,摩擦学性能越好。
The work aims to study the effect of N_2 flow ratio(R=N_2/(Ar+N_2)) on structure and mechanical and tribologicalproperties of molybdenum nitride(Mo-N) coatings by DC reactive magnetron sputtering. Mo-N coatings were deposited on 304 stainless steel substrates by DC reactive magnetron sputtering. The structure, surface morphology and wear morphology, micro-hardness, adhesion strength, friction and friction and wear properties of Mo-N coatings were analyzed, characterized and evalu-ated by SEM, XRD, Vicker microhardness meter, Rockwell indenter and ball-on-disk tribometer, respectively. With the increaseof nitrogen flow ratio(R) from 0.3 to 0.7, the coating was mainly composed of γ-Mo2 N face-centered-cubic(fcc) phase. When Rwas 0.7, a small volume of δ-MoN hexagonal phase appeared in the coating. The microhardness of the coating decreased firstand then increased, and the maximum hardness reached 3060 HV. The adhesion strength of the coating first increased and thendecreased. When R was 0.4 and 0.5, the coatings exhibited higher adhesion strength(40 N) and better tribological properties.The average friction coefficient was about 0.22 and the coating wear was mainly abrasive wear. For the coating prepared on 300 ℃substrate temperature, N_2 gas flow ratio(0.3～0.7) has a little effect on the phase structure of the coating when changing between0.3～0.7. When the hardness is relatively high, the better adhesion strength is, the better tribological properties are.
The work aims to study the effect of N_2 flow ratio(R=N_2/(Ar+N_2)) on structure and mechanical and tribologicalproperties of molybdenum nitride(Mo-N) coatings by DC reactive magnetron sputtering. Mo-N coatings were deposited on 304 stainless steel substrates by DC reactive magnetron sputtering. The structure, surface morphology and wear morphology, micro-hardness, adhesion strength, friction and friction and wear properties of Mo-N coatings were analyzed, characterized and evalu-ated by SEM, XRD, Vicker microhardness meter, Rockwell indenter and ball-on-disk tribometer, respectively. With the increaseof nitrogen flow ratio(R) from 0.3 to 0.7, the coating was mainly composed of γ-Mo2 N face-centered-cubic(fcc) phase. When Rwas 0.7, a small volume of δ-MoN hexagonal phase appeared in the coating. The microhardness of the coating decreased firstand then increased, and the maximum hardness reached 3060 HV. The adhesion strength of the coating first increased and thendecreased. When R was 0.4 and 0.5, the coatings exhibited higher adhesion strength(40 N) and better tribological properties.The average friction coefficient was about 0.22 and the coating wear was mainly abrasive wear. For the coating prepared on 300 ℃substrate temperature, N_2 gas flow ratio(0.3～0.7) has a little effect on the phase structure of the coating when changing between0.3～0.7. When the hardness is relatively high, the better adhesion strength is, the better tribological properties are.
引文
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[2]WU W Y,WU C H,XIAO B H,et al.Microstructure,mechanical and tribological properties of CWNr films deposited by DC magnetron sputtering[J].Vacuum,2013,87:209-212.
[3]隋旭东,李国建,王强,等.钛合金切削用Ti1-xAlxN涂层的制备及其切削性能研究[J].金属学报,2016,52(6):741-746.SUI Xu-dong,LI Guo-jian,WANG Qiang,et al.Preparation of Ti1-xAlxN coating in cutting titanium alloy and its cutting performance[J].Acta metallurgica sinica,2016,52(6):741-746.
[4]MUSIL J,NOVáK P,HROMáDKA M,et al.Mechanical and tribological properties of sputtered Mo-O-N coatings[J].Surface and coatings technology,2013,215:386-392.
[5]GILEWICZ A,JEDRZEJEWSKI R,KOCHMANSKA AE,et al.Structure of MoCN films deposited by cathodic arc evaporation[J].Thin solid films,2015,577:94-96.
[6]WARCHOLINSKI B,GILEWICZ A,KUZNETSOVA TA,et al.Mechanical properties of Mo(C)N coatings deposited using cathodic arc evaporation[J].Surface and coatings technology,2017,319:117-128.
[7]HAZAR H.Characterization of MoN coatings for pistons in a diesel engine[J].Materials&design,2010,31(1):624-627.
[8]MUDHOLKAR M S,THOMPSON L T.Control of composition and structure for molybdenum nitride films synthesized using ion beam assisted deposition[J].J appl phys,1995,77:5138-5143.
[9]MAOUJOUD M,BINST L,DELCAMBE P,et al.Deposition parameter effects on the composition and the crystalline state of reactively sputtered molybdenum nitride[J].Surf coat technol,1992,52:179-185.
[10]ZIN V,MIORIN E,DEAMBROSIS S M,et al.Mechanical properties and tribological behaviour of Mo-Ncoatings deposited via high power impulse magnetron sputtering on temperature sensitive substrates[J].Tribology international,2018,119:372-380.
[11]INUMARU K,BABA K,YAMANAKA S.Synthesis and characterization of superconductingβ-Mo2N crystalline phase on a Si substrate:An application of pulsed laser deposition to nitride chemistry[J].Chem Mater,2005,17:5935-5940.
[12]ROBERSON S L,FINELLO D,DAVIS R F.Growth of MoxN films via chemical vapor deposition of MoCl5 and NH3[J].Surf coat technol,1998,102:256-259.
[13]URGEN M,ERYILMAZ O L,CAKIR A F,et al.Characterization of molybdenum nitride coatings produced by arc-PVD technique[J].Surf coat technol,1997,94-95:501-506.
[14]GILEWICZ A,WARCHOLINSKI B,MURZYNSKI D.The properties of molybdenum nitride coatings obtained by cathodic arc evaporation[J].Surf coat technol,2013,236:149-158.
[15]CARRERI F C,OLIVEIRA R M,OLIVEIRA A C,et al.Phase formation and mechanical/tribological modification induced by nitrogen high temperature plasma based ion implantation into molybdenum[J].Appl surf sci,2014,310:305-310.
[16]RUDNIK P J,GRAHAM M E,SPROUL W D.High rate reactive sputtering of Mo Nx coatings[J].Surface and coatings technology,1991(49):293-297.
[17]鞠洪博,喻利花,许俊华.制备工艺对磁控溅射Mo-N薄膜微结构和性能的影响[J].真空科学与技术学报,2014,34(5):469-472.JU Hong-bo,YU Li-hua,XU Jun-hua.Synthesis and characterization of phase structures and properties of Mo-N coatings[J].Chinese journal of vacuum science and technology,2014,34(5):469-472.
[18]WANG Tao,ZHANG Guo-jun,REN Shuai,et al.Effect of nitrogen flow rate on structure and properties of MoNx coatings deposited by facing target sputtering[J].Journal of alloys and compounds,2017,701:1-8.
[19]黄珂,杨伏良,陈力学,等.划痕法测定TiAlN涂层结合强度的研究[J].表面技术,2013,42(5):107-111.HUANG Ke,YANG Fu-liang,CHEN Li-xue,et al.Study on the adhesion strength of a TiAlN coatings by scratch tester[J].Surface technology,2013,42(5):107-111.
[20]韦春贝,唐明,林松盛,等.Cr Al Si N涂层与不同材料配副时的摩擦学特性[J].表面技术,2018,47(6):181-187.WEI Chun-bei,TANG Ming,LIN Song-sheng,et al.Tribological properties of cralsin coatings sliding against different counterparts[J].Surface technology,2018,47(6):181-187.