Pr<sub>6</sub>O<sub>11</sub>对合成金刚石单晶各向异性的刻蚀

doi:10.11868/j.issn.1001-4381.2021.001231

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摘要

为了探究稀土氧化物对合成金刚石单晶的各向异性刻蚀，在氮气保护下，在750~950℃内用Pr₆O₁₁对合成金刚石单晶进行刻蚀。采用扫描电子显微分析、热重分析、X射线衍射和拉曼光谱等技术对刻蚀后金刚石单晶不同晶面的表面形貌、物相组成和刻蚀机理进行表征与分析。采用最大刻蚀深度、单颗粒抗压强度和冲击韧性来表征刻蚀前后金刚石性能的变化。结果表明：Pr₆O₁₁对金刚石{100}面和{111}面的刻蚀程度和形貌均不同；当温度为750℃时，Pr₆O₁₁对金刚石单晶已有一定程度的刻蚀，随刻蚀温度的增加，刻蚀加剧，且金刚石{111}面的刻蚀程度比{100}面严重；{111}面刻蚀坑形貌从三角形变为层状结构三角形，{100}面由轻微的四边形变为类蜂窝状刻蚀坑；{111}面最大刻蚀深度从1.12 μm增加到12.54 μm，而{100}面只从0.30 μm增加到2.11 μm；金刚石单颗粒的抗压强度由未刻蚀金刚石的576.25 N降低到最小530.06 N，冲击韧性由92.94 J/cm²减小到88.53 J/cm²；Pr₆O₁₁对金刚石单晶的刻蚀机理在885℃前为催化石墨化，885℃后为催化石墨化和氧化。

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	朱振东
	肖长江
	马金明
	栗正新

关键词 ：金刚石单晶, 氧化镨, 各向异性刻蚀, 刻蚀机理, 性能

Abstract：

The work aims to explore the anisotropic etching of synthetic diamond single crystal by rare earth oxide. Under the protection of nitrogen, synthetic diamond single crystals were etched by Pr₆O₁₁ powder at 750-950℃. The surface morphology, phase composition and etching mechanism of different crystal surfaces of diamond single crystal after etching were characterized and analyzed by means of scanning electron microscopy, thermogravimetric analysis, X-ray diffraction and Raman spectroscopy, and the changes of diamond properties before and after etching were characterized by surface roughness, single particle compressive strength and impact toughness. The results show that the etching degree and morphology of {100} faces and {111} faces of diamond by Pr₆O₁₁ are different. When the temperature is 750℃, Pr₆O₁₁ etches slightly diamond crystals. The etching intensifies with the increase of etching temperature, moreover the etching degree of diamond {111} faces is more serious than that of {100} faces. The morphologies of the etching pits of diamond {111} faces change from triangular etching pits to layered triangular ones, and {100} faces change from slight quadrilateral to honeycomb-like etching pits. The maximum etching depth of {100} face increases from 1.12 μm to 12.54 μm, while the maximum etching depth of {111} face increases from 0.3 μm to 2.11 mm. The compressive strength of single diamond particle decreases from 576.25 N of unetched diamond to the smallest value of 530.06 N, and the impact toughness decreases from 92.94 J/cm²to 88.53 J/cm². The etching mechanism of diamond single crystal by Pr₆O₁₁ is catalytic graphitization before 885℃, and the catalytic graphitization and oxidation after 885℃.

Key words： diamond single crystal Pr₆O₁₁ anisotropic etching etching mechanism property

收稿日期: 2021-12-28 出版日期: 2022-11-17

中图分类号:

TG732

基金资助:2022年度省教育厅重点科研项目(22B4300152)

通讯作者: 肖长江 E-mail: cjxiao@haut.edu.cn

作者简介: 肖长江(1969—), 男, 副教授, 博士, 主要研究方向: 超硬材料及其制品, 联系地址: 河南省郑州市高新区莲花街100号河南工业大学材料科学与工程学院(450001), E-mail: cjxiao@haut.edu.cn

引用本文:

朱振东, 肖长江, 马金明, 栗正新. Pr₆O₁₁对合成金刚石单晶各向异性的刻蚀[J]. 材料工程, 2022, 50(11): 173-181.
Zhendong ZHU, Changjiang XIAO, Jinming MA, Zhengxin LI. Anisotropy etching of synthetic diamond single crystals by Pr₆O₁₁ powder. Journal of Materials Engineering, 2022, 50(11): 173-181.

链接本文:

http://jme.biam.ac.cn/CN/10.11868/j.issn.1001-4381.2021.001231 或 http://jme.biam.ac.cn/CN/Y2022/V50/I11/173

Fig.1 不同温度Pr₆O₁₁刻蚀金刚石{111}面后的表面形貌
(a)750 ℃；(b)800 ℃；(c)850 ℃；(d)900 ℃；(e)950 ℃

Fig.2 不同温度Pr₆O₁₁刻蚀金刚石{100}面后的表面形貌
(a)750 ℃；(b)800 ℃；(c)850 ℃；(d)900 ℃；(e)950 ℃

Fig.3 不同处理条件下金刚石刻蚀过程中的TG曲线

Fig.4 不同温度下Pr₆O₁₁和金刚石混合物的XRD图

Fig.5 原始Pr₆O₁₁粉末900 ℃处理前后的XRD图

Fig.6 Pr₆O₁₁刻蚀后金刚石的拉曼光谱图
(a){111}面；(b){100}面

Fig.7 金刚石单晶的原子排布
(a){111}面；(b){100}面

Fig.8 金刚石表面原子层数与表面能的关系

Fig.9 金刚石的原子排布图
(a)金刚石原子的三维取向图；(b){111}面；(c){100}面

Fig.10 Pr₆O₁₁刻蚀后金刚石表面刻蚀坑转变示意图
(a){111}面；(b){100}面

Fig.11 Pr₆O₁₁刻蚀后金刚石{111}面和{100}面的最大刻蚀深度

Fig.12 Pr₆O₁₁刻蚀后的金刚石单颗粒抗压强度

Table 1 不同温度下Pr₆O₁₁刻蚀后金刚石的冲击韧性

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