张纪福,刘艳梅,张涛,柯培玲,张翔宇,丁洋,Kim Kwang Ho,王铁钢.还原性气氛制备Zr-B-N纳米复合涂层的结构及性能分析[J].表面技术,2022,51(9):83-90, 101.
ZHANG Ji-fu,LIU Yan-mei,ZHANG Tao,KE Pei-ling,ZHANG Xiang-yu,DING Yang,KIM Kwang，Ho,WANG Tie-gang.Structure and Properties of Zr-B-N Nanocomposite Coatings Prepared in Reducing Reactive Atmosphere[J].Surface Technology,2022,51(9):83-90, 101 |
| 还原性气氛制备Zr-B-N纳米复合涂层的结构及性能分析 |
| Structure and Properties of Zr-B-N Nanocomposite Coatings Prepared in Reducing Reactive Atmosphere |
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| DOI：10.16490/j.cnki.issn.1001-3660.2022.09.008 |
| 中文关键词: 还原性反应气氛 Zr-B-N涂层 磁控溅射 纳米复合涂层 微观结构 力学性能 |
| 英文关键词:reducing reactive atmosphere Zr-B-N coating magnetron sputtering nanocomposite coating microstructure mechanical property |
| 基金项目:国家自然科学基金(51301181, 51875555);天津市科技重大专项(18ZXJMTG00050);天津市自然科学基金(19JCYBJC17100);天津市科技特派员项目(20YDTPJC01460) |
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| Author | Institution |
| ZHANG Ji-fu | Tianjin Key Laboratory of High Speed Cutting and Precision Manufacturing, Tianjin University of Technology and Education, Tianjin 300222, China |
| LIU Yan-mei | Tianjin Key Laboratory of High Speed Cutting and Precision Manufacturing, Tianjin University of Technology and Education, Tianjin 300222, China |
| ZHANG Tao | Tianjin Key Laboratory of High Speed Cutting and Precision Manufacturing, Tianjin University of Technology and Education, Tianjin 300222, China |
| KE Pei-ling | Key Laboratory of Marine Materials and Related Technologies, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Zhejiang Ningbo 315201, China |
| ZHANG Xiang-yu | Tianjin Key Laboratory of High Speed Cutting and Precision Manufacturing, Tianjin University of Technology and Education, Tianjin 300222, China |
| DING Yang | Tianjin Key Laboratory of High Speed Cutting and Precision Manufacturing, Tianjin University of Technology and Education, Tianjin 300222, China |
| KIM Kwang，Ho | Global Frontier R&D Center for Hybrid Interface Materials, Pusan National University, Busan 609-735, South Korea |
| WANG Tie-gang | Tianjin Key Laboratory of High Speed Cutting and Precision Manufacturing, Tianjin University of Technology and Education, Tianjin 300222, China |
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| 中文摘要: |
| 目的 制备高纯度、超硬、高耐磨的Zr-B-N纳米复合涂层。方法 在反应气体中掺入还原性气体H2，利用氢元素强还原性去除真空室以及反应气氛中残留的O杂质，采用脉冲直流磁控溅射技术，通过调节N2+H2混合气体流量制备高纯度Zr-B-N涂层。利用扫描电镜、纳米压痕仪、摩擦磨损试验机等设备对涂层的微观结构、力学性能和摩擦性能进行测试，并分析其变化机理。结果 随着N2+H2流量的增加，Zr-B-N涂层内N含量在N2+H2流量为10 mL/min时达到最高。从截面形貌可以看出，涂层结构由粗大的柱状晶逐步转变为玻璃状细小柱状晶结构，涂层更加致密，呈现典型的纳米复合结构。微量H元素的掺入，减少了涂层制备过程中O相关化学键的生成，制备出的Zr-B-N涂层晶粒的生长环境得到改善。在N2+H2流量为 10 mL/min时，涂层的硬度和弹性模量达到最大值40.26 GPa和532.98 GPa，临界载荷最大约为60.1 N，摩擦系数较小，为0.72，磨损率在此时最低，为1.12×10–5mm3/(N.m)。结论 当N2+H2流量为10 mL/min时，制备出了超硬Zr-B-N纳米复合涂层。适量氢元素的掺入，充分去除真空室内氧杂质，改善了涂层中晶粒的生长环境，有效地提高涂层的硬度及摩擦磨损性能。 |
| 英文摘要: |
| ZrB2 coatings have been widely used in industrial fields due to their interesting intrinsic characteristics, such as high melting point, high hardness, excellent oxidation resistance and corrosion resistance, etc. However, they are still restricted to apply on the cutting tool surface owing to their high brittleness. The addition of nitrogen atoms is expected to cause a further improvement on the film toughness through forming nanocomposite microstructure, namely the nanocrystallines ZrN or ZrB2 are surrounded by amorphous BN phase. Usually, high purity nitrogen used as reactive gas is produced by physical liquid phase separation method. It is inevitable that small amount of oxygen impurity is remained in it. Because boron is easy to react with oxygen to form amorphous boron oxide. As a result, a large amount of amorphous boron oxide and boron nitride phases existing in the coatings severely affects their mechanical properties. To resolve the above problem, the oxygen impurities in the Zr-B-N coating must be removed. In this work, a new method to prepare high-purity, super-hard and highly wear-resistant Zr-B-N nanocomposite coatings was proposed. Namely, an appropriate amount of reducing hydrogen was mixed into the reactive gas during the coating deposition. Through reduction reaction, the combination of oxygen with elements other than hydrogen would be prohibited, and the oxygen impurities in the vacuum chamber could be removed. Therefore, the purity of the Zr-B-N coating and its related properties could also be improved. In addition, the use of reducing gas in the process of reactive deposition also lowered the technological requirements of coating equipment. A large amount of vacuum pumping time was saved. The coating efficiency was improved and the production cost is reduced. |
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