本文通过温度梯度法在5.5 GPa和1 300 ℃的条件下合成了硼、氮共掺杂金刚石单晶。随后分别在5.0 GPa，2 000 ℃和2 100 ℃的条件下对合成金刚石进行了高温高压(HPHT)退火处理。傅里叶红外光谱(FT-IR)测试表明高温高压退火后晶体内部单一替代形式的C心氮转变成了聚集态A心氮，且随着退火温度的升高A心氮的含量提高。晶体内部带正电荷的氮离子N+的含量并未受到退火处理的影响。经过高温退火后晶体内部出现了NV0和NV-色心，但是继续提高退火温度时NV色心消失。高温高压退火并未对金刚石晶体的结构及内应力产生明显的影响。高温高压退火处理后金刚石晶体的热稳定性能提高，其起始氧化温度、剧烈氧化温度以及质量急剧减少的温度点分别提高了65 ℃、55 ℃以及61 ℃。本文对高温高压退火处理应用到硼、氮共掺杂金刚石提供了指导。

In this paper, boron and nitrogen co-doped diamond was synthesized under the condition of 5.5 GPa and 1 300 ℃ by temperature gradient growth method. Then the synthetic diamond was annealed under the pressure of 5.0 GPa and the temperature of 2 000 ℃ and 2 100 ℃. FT-IR spectra demonstrate that the singly substituted form nitrogen (C-center) in the crystal after high pressure and high temperature (HPHT) annealing is transformed into the aggregation form nitrogen (A-center), and the concentration of A-center nitrogen increases with the annealing temperature. The concentration of positively charged nitrogen ion (N+) in the crystal is not affected by HPHT annealing treatment. After high temperature annealing, NV0 and NV- center appear in the diamond, but disappear when the annealing temperature continues to increase. HPHT annealing has no obvious effect on the structure and internal stress of diamond crystal. After HPHT annealing treatment, the thermal stability of diamond is improved, the initial oxidation temperature, intense oxidation temperature and the temperature point where the mass sharply decrease are increased by 65 ℃, 55 ℃ and 61 ℃, respectively. This paper provides guidance for the HPHT annealing treatment application to boron and nitrogen co-doped diamond.