激光原位合成Al2O3-TiO2复合陶瓷涂层组织结构与性能

doi:10.11868/j.issn.1001-4381.2016.001453

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摘要

先利用火焰喷涂技术在中国低活化马氏体钢表面制备了CrFeAlTi涂层，然后通过激光原位反应技术在火焰喷涂涂层表面原位合成了Al₂O₃-TiO₂复合陶瓷涂层。分别采用体视显微镜、扫描电子显微镜（SEM）、透射电子显微镜（TEM）、X射线衍射仪（XRD）、显微硬度计、立式万能摩擦磨损试验机以及静态铅铋腐蚀实验装置等分析测试手段对涂层的形貌、微观组织结构、物相组成、显微硬度、干滑动摩擦磨损性能以及耐液态铅铋合金腐蚀性能等进行了研究。实验结果表明：激光原位合成的Al₂O₃-TiO₂复合陶瓷涂层表面整体平整、光滑、致密，基本没有凹坑、裂纹和孔隙等缺陷，与基体之间形成了良好的冶金结合。涂层内部存在完全结晶区和非结晶区，且界面明显。涂层表面主要物相为Al₂O₃，TiO₂，（Al.948Cr.052）₂O₃，Fe₂TiO₅和FeCr等。涂层截面平均显微硬度约为1864.2HV_0.2，比基体CLAM钢提高了约3倍，且沿横截面方向呈平稳过渡的阶梯状分布。与基体CLAM钢相比，涂层具有良好的耐磨性能，其磨损量仅为基体的1/6，并且涂层在液态铅铋中表现出良好的耐腐蚀性能。

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	张曼莉
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关键词 ：火焰喷涂, 激光原位合成技术, Al₂O₃-TiO₂复合陶瓷涂层, 微观组织结构, 性能

Abstract：

The study involves in-situ synthesis of CrFeAlTi composite coating using laser micro-melting processing. The coating was successfully prepared by laser irradiating CrFeAlTi coating prepared by flame spraying on the China low activation martensitic (CLAM) steel substrate, and then Al₂O₃-TiO₂ composite ceramic coating was synthesized by in-situ reaction on the surface of flame sprayed coating. The coating morphology, microstructure, phase composition, micro-hardness, dry sliding wear properties and corrosion resistance in liquid PbBi alloy were analyzed by stereomicroscope, scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), micro-sclerometer, vertical universal friction wear testing machine and static PbBi corrosion test device, respectively. The test results show that the surface of Al₂O₃-TiO₂ composite ceramic coating is smooth, and the microstructure of coating is both homogeneous and dense without defects such as crack, dimple and porosity, etc., a good metallurgical bonding between the composite ceramic coating and the substrate, and the interface is obvious. The phases of the coating surface are mainly composed of Al₂O₃, TiO₂, (Al.948Cr.052)₂O₃, Fe₂TiO₅ and FeCr, etc. The coating shows a high average micro-hardness of approximately 1864.2HV_0.2, which is about three times higher than that of the CLAM steel substrate, and presents gradient distribution with stable transition from the coating surface to the substrate. Comparing with the substrate, the coating presents excellent wear resistance. The wear mass loss of the coating is just one sixth of that of the substrate. Meanwhile, the coating exhibits the best corrosion resistance in the liquid PbBi.

Key words： flame spraying laser in-situ synthesis technology Al₂O₃-TiO₂ composite ceramic coating microstructure property

收稿日期: 2016-09-10 出版日期: 2018-02-01

中图分类号:

TG174.4

基金资助:国家自然科学基金重大研究计划(91326114);湖南省高校重点实验室(湘财教指[2014]85号);湖南省高校科技创新团队支持计划(湘教通[2012]318号);湖南省重点学科建设项目(湘教发[2011]76号)

通讯作者: 邱长军 E-mail: qiuchangjun@hotmail.com

作者简介: 邱长军(1965-), 男, 教授, 博士, 从事金属材料表面改性技术方面的研究, 联系地址:湖南省衡阳市蒸湘区常胜西路28号南华大学机械工程学院(421001), E-mail: qiuchangjun@hotmail.com

引用本文:

张曼莉, 邱长军, 蒋艳林, 郑文权, 夏琰. 激光原位合成Al₂O₃-TiO₂复合陶瓷涂层组织结构与性能[J]. 材料工程, 2018, 46(2): 57-65.
Man-li ZHANG, Chang-jun QIU, Yan-lin JIANG, Wen-quan ZHENG, Yan XIA. Microstructure and Properties of Laser In-situ Synthesized Al₂O₃-TiO₂ Composite Ceramic Coating. Journal of Materials Engineering, 2018, 46(2): 57-65.

链接本文:

http://jme.biam.ac.cn/CN/10.11868/j.issn.1001-4381.2016.001453 或 http://jme.biam.ac.cn/CN/Y2018/V46/I2/57

Fig.1 静态铅铋腐蚀实验装置示意图

Fig.2 Al₂O₃-TiO₂复合陶瓷涂层试样表面形貌(a)与EDS能谱分析结果(b)

Fig.3 Al₂O₃-TiO₂复合陶瓷涂层试样截面组织形貌(SEM)
(a)涂层截面整体形貌；(b)涂层区上部；(c)涂层区中部；(d)涂层底部与基体结合界面

Fig.4 对应图 3(b)中黑色(a)和灰白色(b)组织能谱分析

Fig.5 Al₂O₃-TiO₂复合陶瓷涂层TEM图
(a)涂层区高分辨TEM图; (b)，(c)，(d)分别为A区域、B区域和C区域的高分辨TEM图

Fig.6 复合陶瓷涂层的XRD图谱

Table 1 标准吉布斯自由能对照表(T=1800K左右)

Fig.7 Al₂O₃-TiO₂复合陶瓷涂层截面显微硬度曲线

Fig.8 基体CLAM钢与Al₂O₃-TiO₂复合陶瓷涂层的磨损量

Fig.9 基体(a)与Al₂O₃-TiO₂复合陶瓷涂层(b)的磨损形貌

Fig.10 基体CLAM钢(a)和Al₂O₃-TiO₂复合陶瓷涂层样品(b)腐蚀后SEM形貌

Table 2 图 10中各标记区域Pb，Bi元素含量(质量分数/%)

Fig.11 样品中Pb元素随腐蚀时间的扩散深度

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