退火和氧化性酸处理对HFCVD法制备金刚石薄膜质量的影响

Effects of annealing and oxidizing acid treatment on quality of diamond film fabricated by chemical vapor deposition method

以H2和CH4为反应气源,采用热丝化学气相沉积法（hot filament chemical vapor deposition,缩写HFCVD）,于不同温度下,在金属Mo表面上制备金刚石薄膜,并分别对薄膜进行退火和氧化性酸处理。采用场发射扫描电镜（FESEM）、拉曼光谱（Raman）及物相分析（XRD）,研究沉积温度与后处理工艺对薄膜质量和薄膜表面内应力的影响。结果表明,在700℃下沉积的薄膜晶型良好,晶粒尺寸大且均匀,平均粒径为0.5μm,薄膜中存在2.72 GPa的压应力;该薄膜在氢气气氛中退火后质量得到提升,金刚石的Raman特征峰强与石墨的Raman特征峰强的比值从2.780 0上升至4.451 6,薄膜中无定型碳和石墨成分的总含量（质量分数）下降37.6%;采用过氧化氢氧化处理后,薄膜中无定型碳和石墨的总含量（质量分数）下降26.8%,薄膜中69.0%~73.0%（质量分数）的trans-PA被氧化处理掉,热应力得到释放。

Using H2 and CH4 as reaction gas source,the diamond film was prepared on Mo substrate under different temperatures by hot filament chemical vapor deposition method（HFCVD）.The morphology,quality properties of post-treatment process were analyzed by field emission scanning electron microscopy（FESEM）,Raman spectrometer system（RS） and X-ray diffraction.The results indicate that the film with good crystal form,bigger and homogeneous grains with average grain size of 0.5 m can be obtained under 700 ℃ depositing;the residual stress is 2.72 GPa;after annealing in a hydrogen atmosphere,Raman peaks intensity ratio of diamond and graphite increases from 2.780 0 to 4.451 6,the relative content of sp2carbon decreases by 37.6%（mass fraction）,which shows film quality enhancement;,the content of sp2carbon decreases by 26.8% and 69.0% ~73.0% of trans-PA is removed after H2 O2（aq） treatment,and the thermal stress is released.