利用高纯度的硼粉和硫粉，在1 300 ℃的高温真空环境下，通过扩散装置制备出硼(B)、硫(S)共掺杂单晶金刚石。扫描电子显微镜、X射线能谱、拉曼光谱等测试结果表明，随着两种元素的掺入，金刚石的形貌和晶体质量发生变化。掺杂后的金刚石形貌复杂，蚀坑和沟壑内部形貌呈阶梯状，随着掺杂量的增加出现断层，并在蚀坑处检测出较高的硼原子和硫原子含量，掺杂B-S质量比为0.5的金刚石蚀坑处的硼原子和硫原子含量最高。随着杂质原子的渗入，拉曼半峰全宽值增大，金刚石的晶体质量下降。室温下进行霍尔检测结果表明，掺杂后的金刚石电阻率降低。B-S质量比为1和2的样品导电类型表现为p型；B-S质量比为0.5时，样品的霍尔系数为负值，导电类型为n型。

The boron (B)-sulfur (S) co-doped single crystal diamond was prepared by diffusion device using high purity boron powder and sulfur powder at 1 300 ℃ under a high temperature vacuum. In this paper, scanning electron microscopy, X-ray energy spectroscopy, Raman spectroscopy, and other tests show that the morphology and crystal quality of diamond change with doping of the two elements. The co-doping diamond crystal surface morphology is complex, and the internal morphology of etch pits and gully is stepped. With the doping amount increases, the steps appear to fracture, and high content of boron and sulfur atoms is detected at the etch pits. The diamond with B-S mass fraction of 0.5 have the highest content of boron and sulfur atoms at the etch pits. With the impurity atoms infiltration, full width at half maximum of Raman increases, and crystal quality of the diamond decreases. Hall testing at room temperature reveals that the diamond resistivity decreases after doping. The samples with the B-S mass fraction of 1 and 2 exhibit p-type conductivity. While the sample with the B-S mass fraction of 0.5, the Hall coefficient is negative and shows n-type conductivity.