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采用直流热阴极PCVD技术,在CH4-H2气氛常规制备微米晶金刚石膜的参数条件下,通过人工干预实现二次形核,制备纳米晶金刚石膜。金刚石膜周期性生长过程分为沉积阶段和干预阶段,沉积阶段时间为20 min,干预阶段将沉积温度降低到600℃,时间为1 min,然后恢复到生长温度,一个生长周期为21 min,总的沉积时间为6 h。实验分为高、低气压和高、低温度的四种组合,并与连续生长模式进行了对比。采用拉曼光谱仪、SEM对样品进行了分析,除高气压和高温度条件外,其它三组实验的金刚石膜的1332 cm-1拉曼峰展宽明显、金刚石膜晶粒小于100 nm,样品都具有纳米晶特征。结果表明直流热阴极PCVD技术的人工干预方法,可以导致金刚石膜生长过程的二次形核行为发生,制备出纳米金刚石膜。
The direct current hot cathode PCVD technique was used to fabricate nanocrystalline diamond films by the artificial intervention under the condition of conventional preparation of microcrystalline diamond films in CH4-H2 atmosphere. The periodic growth of diamond film is divided into depositional stage and interventional stage. The depositional time is 20 minutes. The depositional temperature is reduced to 600 ℃ for 1 min and then returned to the growth temperature for 21 min. The total growth period is 21 min. The deposition time is 6 h. The experiment is divided into four combinations of high, low pressure and high and low temperature, and compared with the continuous growth mode. The samples were analyzed by Raman spectroscopy and SEM. Except for the conditions of high pressure and high temperature, the 1332 cm-1 Raman peaks of the diamond films of the other three groups were obviously widened, and the diamond crystal grains were less than 100 nm. The samples all had Nanocrystalline features. The results show that the artificial intervention method of DC hot cathode PCVD technology can lead to the secondary nucleation of diamond film during the growth process, to prepare a nano-diamond film.