厚类金刚石碳基薄膜的制备及摩擦与腐蚀性能的表征
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摘要
目的设计多层掺Si交替沉积的厚DLC薄膜,改善SUS304不锈钢的耐磨性与耐蚀性,拓展其使用范围。方法使用等离子增强化学气相沉积(PECVD)技术,在C_2H_2-SiH_4气氛中,通过Si_x-DLC与Si_y-DLC交替沉积的制备方法,以SUS304不锈钢为基底,制备了厚度为20.0、34.9、41.6μm的三种不同调制比(1∶5、1∶1、4∶1)的厚类金刚石碳基薄膜。利用扫描电子显微镜、原子力显微镜、拉曼光谱、纳米压痕仪、RST3划痕仪,分析了厚DLC薄膜的微观结构与力学性能。利用CSM摩擦磨损试验机评价厚DLC薄膜的摩擦学性能,并用能谱仪对磨斑成分进行分析。利用电化学工作站分析厚DLC薄膜的腐蚀行为,并用扫描电镜观察腐蚀形貌。结果厚DLC薄膜结构致密,强化效果明显,硬度最高达13.8GPa,结合力在21～29N范围内。SUS304不锈钢的摩擦系数在跑和阶段急速升高至0.5,随着滑动次数的增加,呈上升趋势,1 h后,磨损率无法用轮廓仪测量。厚DLC薄膜在低载荷与高载荷下的摩擦系数始终保持在0.05～0.2之间,磨损率低至9.4×10~(-17) mm~3/(N·m)。电化学测试表明,SUS304不锈钢的腐蚀电位为-0.49V,腐蚀电流密度为1.46×10~(-6) A/cm~2。与SUS304不锈钢相比,三种厚度的DLC薄膜腐蚀电位正移、极化电阻升高,腐蚀电流密度最大可降低3个数量级。结论厚DLC薄膜的应用可以有效降低摩擦磨损,腐蚀倾向相比于不锈钢明显降低,具有良好的耐腐蚀性。
The work aims to design multilayer Si-doped DLC film to improve the wear resistance and corrosion resistance of SUS304 stainless steel and extend the application scope. Three kinds of thick diamond-like carbon based films with different modulation ratios(1∶5, 1∶1, 4∶1) of 20.0, 34.9, and 41.6 μm were deposited on SUS304 stainless steel in the C_2H_2-SiH_4 system by alternately depositing Six-DLC layer and Siy-DLC layer through plasma enhanced chemical vapor deposition(PECVD).The microstructure, mechanical properties, tribological properties wear scar composition, corrosion behavior and corrosion morphology of thick DLC films were characterized and analyzed by scanning electron microscope, atomic force microscope,Raman spectroscopy, nano-indentation tester, RST3 scratch tester, CSM tribometer and electrochemical station, respectively. The thick DLC films had dense microstructure, obvious strengthening effect and the highest hardness up to 13.8 GPa. The adhesion strength was in the range of 21 to 29 N. The friction coefficient of SUS304 stainless steel increased rapidly to 0.5 in the running stage, and still increased with the increase of the number of sliding times. The wear rate could not be measured by the profilometer after 1 h. The friction coefficient under low load and high load was between 0.05～0.2, and the wear rate was as low as 9.4×10~(-17) m~3/(N·m). Electrochemical tests showed that SUS304 stainless steel corrosion potential was -0.49 V and corrosion current density was 1.46×10~(-6) A/cm~2. Compared with stainless steel, the corrosion potential of the three thick DLC films shifted positively and the polarization resistance increased. The corrosion current density was reduced by up to three orders of magnitude. The application of thick DLC film can effectively reduce friction and wear and the corrosion tendency is significantly lower than that of stainless steel and has good corrosion resistance.
The work aims to design multilayer Si-doped DLC film to improve the wear resistance and corrosion resistance of SUS304 stainless steel and extend the application scope. Three kinds of thick diamond-like carbon based films with different modulation ratios(1∶5, 1∶1, 4∶1) of 20.0, 34.9, and 41.6 μm were deposited on SUS304 stainless steel in the C_2H_2-SiH_4 system by alternately depositing Six-DLC layer and Siy-DLC layer through plasma enhanced chemical vapor deposition(PECVD).The microstructure, mechanical properties, tribological properties wear scar composition, corrosion behavior and corrosion morphology of thick DLC films were characterized and analyzed by scanning electron microscope, atomic force microscope,Raman spectroscopy, nano-indentation tester, RST3 scratch tester, CSM tribometer and electrochemical station, respectively. The thick DLC films had dense microstructure, obvious strengthening effect and the highest hardness up to 13.8 GPa. The adhesion strength was in the range of 21 to 29 N. The friction coefficient of SUS304 stainless steel increased rapidly to 0.5 in the running stage, and still increased with the increase of the number of sliding times. The wear rate could not be measured by the profilometer after 1 h. The friction coefficient under low load and high load was between 0.05～0.2, and the wear rate was as low as 9.4×10~(-17) m~3/(N·m). Electrochemical tests showed that SUS304 stainless steel corrosion potential was -0.49 V and corrosion current density was 1.46×10~(-6) A/cm~2. Compared with stainless steel, the corrosion potential of the three thick DLC films shifted positively and the polarization resistance increased. The corrosion current density was reduced by up to three orders of magnitude. The application of thick DLC film can effectively reduce friction and wear and the corrosion tendency is significantly lower than that of stainless steel and has good corrosion resistance.
引文
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[3]陈青云,施凯敏,苏敏华,等.类金刚石膜研究进展[J].材料工程,2017,45(3):119-128.CHEN Qing-yun,SHI Kai-min,SU Min-hua,et al.Progress of diamond-like carbon films[J].Journal of materials engineering,2017,45(3):119-128.
[4]SHARMA R,BARHAI P K,KUMARI N.Corrosion resistant behavior of DLC films[J].Thin solid films,2008,16(16):5397-5403.
[5]UEMATSU Y,KAKIUCHI T,TERATANI T,et al.Improvement of corrosion fatigue strength of magnesium alloy by multilayer diamond-like carbon coatings[J].Surface and coatings technology,2011,205(8):2778-2784.
[6]胡芳,代明江,林松盛,等.含氢掺硅类金刚石薄膜的制备及性能表征[J].中国表面工程,2012,25(6):47-52.HU Fang,DAI Ming-jiang,LIN Song-sheng,et al Preparation and characterization of hydrogen containing Si-doped DLC film[J].Chinese surface engineering,2012,25(6):47-52.
[7]ROBERTSON J.Diamond-like amorphous carbon[J].Material science and engineering,2002,37(4):129-281.
[8]WANG J,PU J,ZHANG G,et al.Interface architecture for superthick carbon-based films toward low internal stress and ultrahigh load-bearing capacity[J].Applied materials and interfaces,2013,5(11):5015-5024.
[9]GUO T,KONG C,LI X,et al.Microstructure and mechanic-al properties of Ti/Al co-doped DLC films:Dependence on sputtering current,source gas,and substrate bias[J].Applied surface science,2017,410:51-59.
[10]DAI W,GAO X,LIU J,et al.Microstructure,mechanical property and thermal stability of diamond-like carbon coatings with Al、Cr and Si multi-doping[J].Diamond and related materials,2016,70:98-104.
[11]CUI M J,PU J,WANG L,et al.Corrosion and tribocorrosion performance of multilayer diamond-like carbon film in NaCl solution[J].Royal society of chemistry,2015,5:104829-104840.
[12]崔明君,任思明,樊小强,等.调制比对多层DLC涂层摩擦及电化学行为的影响[J].机械工程学报,2018,54(6):25-30.CUI Ming-jun,REN Si-ming,FAN Xiao-qiang,et al.Influence of modulation ratio on the friction and electrochemical behavior of multilayer DLC coatings[J].Journal of mechanical engineering,2018,54(6):25-30.
[13]PU J B,WANG J,DONG Q,et al.Corrosion and tribocorrosion behavior of super-thick diamond-like carbon films deposited on stainless steel in Na Cl solution[J].Surface and interface analysis,2016,48:360-367.
[14]DUMINICAL F D,BELCHI R,LIBRALESSO L,et al.Investigation of Cr(N)/DLC multilayer coatings elaborated by PVD for high wear resistance and low friction applications[J].Surface and coatings technology,2018,337:396-403.
[15]王军军.超厚类金刚石碳基薄膜多层界面特征及其摩擦学特性[D].兰州:中国科学院兰州化学物理研究所,2015.WANG Jun-jun.Multilayer interfaces characteristics and tribological performances of super-thick diamond-like carbon based films[D].Lanzhou:Lanzhou Institute of Chemical Physics,Chinese Academy of Sciences,2015.