以磷化铁为添加剂沿(111)面生长磷掺杂金刚石大单晶

人工晶体学报 ›› 2022, Vol. 51 ›› Issue (4): 587-593.

以磷化铁为添加剂沿(111)面生长磷掺杂金刚石大单晶

聂媛¹, 许安涛², 李尚升¹, 胡美华¹, 赵法卿³, 赵桂平³, 黄国锋⁴, 李战厂⁴, 周振翔⁵, 王蒙召¹, 陈珈希¹, 周绪彪¹

1.河南理工大学材料科学与工程学院,河南省深地材料科学与技术重点实验室,焦作 454003;
2.焦作师范高等专科学校,焦作 454000;
3.焦作市东星炭电极有限公司,焦作 454150;
4.赤峰学院,内蒙古自治区高压相功能材料重点实验室,赤峰 024000;
5.中材人工晶体研究院有限公司,北京 100018

收稿日期:2022-01-24 出版日期:2022-04-15 发布日期:2022-05-16
通讯作者: 李尚升,博士,副教授。E-mail:lishsh@hpu.edu.cn
作者简介:聂媛(1997—),女,河南省人,硕士研究生。E-mail:203488098@qq.com
基金资助:
国家自然科学基金(52072113);内蒙古自治区高压相功能材料重点实验室开放课题(cfxygy202003);河南省自然科学基金(182300410279);河南省科技攻关项目(182102210311);河南理工大学博士基金(B2017-54)

Growth of P-Doped Diamond Large Single Crystals Along (111) Surface with Fe₃P as Additive

NIE Yuan¹, XU Antao², LI Shangsheng¹, HU Meihua¹, ZHAO Faqing³, ZHAO Guiping³, HUANG Guofeng⁴, LI Zhanchang⁴, ZHOU Zhenxiang⁵, WANG Mengzhao¹, CHEN Jiaxi¹, ZHOU Xubiao¹

1. Henan Key Laboratory of Materials on Deep-Earth Engineering, School of Materials Science and Engineering, Henan Polytechnic University, Jiaozuo 454003, China;
2. Jiaozuo Teachers College, Jiaozuo 454000, China;
3. Jiaozuo Dongxing Carbon Electrode Co., Ltd, Jiaozuo 454150, China;
4. Inor Mongolia Key Laboratory of High-Pressure Phase Functional Materials, Chifeng University, Chifeng 024000, China;
5. Sinoma Snythetic Crystals Co., Ltd., Beijing 100018, China

Received:2022-01-24 Online:2022-04-15 Published:2022-05-16

摘要/Abstract

摘要： 掺杂是调控金刚石性能的一种重要手段。本文采用温度梯度法,在5.6 GPa、1 312 ℃的条件下,选用Fe₃P作为磷源进行磷掺杂金刚石大单晶的合成。金刚石样品的显微光学照片表明,随着Fe₃P添加比例的增加,金刚石晶体的颜色逐渐变深,包裹体数量逐渐增加,晶形由板状转变为塔状直至骸晶。金刚石晶形的变化表明Fe₃P的添加使生长金刚石的V形区向右偏移,这是Fe₃P改变触媒特性的缘故。红外光谱分析表明,Fe₃P的添加使金刚石晶体中氮含量上升,这说明磷的进入诱使氮原子更容易进入金刚石晶格中。激光拉曼光谱测试表明,随着Fe₃P添加比例的增加,所合成的掺磷金刚石的拉曼峰位变化不大,其半峰全宽(FWHM)值变大,这说明磷的进入使得金刚石晶格畸变增加。XPS测试结果显示,随着Fe₃P添加比例的增加,金刚石晶体中磷相对碳的原子百分含量也会增加,这意味着添加Fe₃P所合成的金刚石晶体中有磷存在。

关键词: Fe₃P, 掺杂, (111)面, 金刚石大单晶, 温度梯度法, 超硬材料

Abstract: Doping is an important means to control the properties of diamond. In this paper, the P-doped diamond large single crystals were synthesized by temperature gradient method at 5.6 GPa and 1 312 ℃ using Fe₃P as the phosphorus source. The results of the optical micrographs of diamond samples show that as the amount of Fe₃P additve increases, the color of diamond crystals becomes darker, the number of inclusions increases in the crystals, and the crystal shape transforms from plate to tower, even to skeletal. It indicates that the V-shaped growth region shifts to the right when Fe₃P is added. This is due to Fe₃P has effect on the properties of the catalyst. IR spectra of P-doped diamond reveal that the concentrations of nitrogen impurity in the diamond crystals increases with the increase of the Fe₃P content. It indicates that the entry of phosphorus induces nitrogen atoms to enter the diamond lattice more easily. Raman spectra results show that with the increase of Fe₃P content, the Raman peak positions of the synthesized diamond change little, but the FWHM becomes larger. This suggests that the entry of phosphorus increases the crystal lattice distortion of diamond. XPS test results show that with the increase of Fe₃P, the content of P relative to C in diamond crystal also increases. It means that phosphorus are present in the diamond crystals synthesized by Fe₃P addition.

Key words: Fe₃P, doping, (111) surface, large diamond single crystal, temperature gradient method, superhard material

中图分类号:

TQ163
O78

聂媛, 许安涛, 李尚升, 胡美华, 赵法卿, 赵桂平, 黄国锋, 李战厂, 周振翔, 王蒙召, 陈珈希, 周绪彪. 以磷化铁为添加剂沿(111)面生长磷掺杂金刚石大单晶[J]. 人工晶体学报, 2022, 51(4): 587-593.

NIE Yuan, XU Antao, LI Shangsheng, HU Meihua, ZHAO Faqing, ZHAO Guiping, HUANG Guofeng, LI Zhanchang, ZHOU Zhenxiang, WANG Mengzhao, CHEN Jiaxi, ZHOU Xubiao. Growth of P-Doped Diamond Large Single Crystals Along (111) Surface with Fe₃P as Additive[J]. JOURNAL OF SYNTHETIC CRYSTALS, 2022, 51(4): 587-593.

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