摘要
以自制的CeF3粉体为原料,在真空碳管炉中采用温度梯度法制备了CeF3晶体。通过X射线衍射(XRD)、扫描式电子显微镜(SEM)、能谱分析(EDS)等分析方法对不同影响因素下的产物进行表征,CeF3晶体进行镀膜实验,并对所得膜层进行光学性能测试。结果表明:采用钨坩埚,在1×10^-2Pa真空度下1500℃保温1 h,以100℃·h^-1的温度梯度降温,可制备得结晶性能良好的CeF3晶体。添加NH4HF2作为脱氧剂可以使产物中氧含量从0. 54%(质量分数)降低到0. 1%。采用两种氧含量的CeF3晶体分别进行镀膜实验,氧含量较低的晶体,其镀膜速率波动曲线较稳定,在±0. 05 nm·s^-1之间波动,说明氧含量的降低可显著改善材料的蒸发特性;镀膜残余由发黑、发白、黑白过度三部分组成,其发黑部分氧含量最高为7. 92%。CeF3膜层性能测试表明,在波长为550 nm处,折射率为1. 6,吸收系数为3×10^-4。
CeF3 crystal was prepared by temperature gradient method in vacuum carbon tube furnace with self-made CeF3 powder as raw material. The products under different influence factors were characterized by X-ray diffraction（ XRD）,scanning electron microscope（ SEM）,energy dispersive spectrometer（ EDS）. CeF3 crystals were subjected to coating experiments,and the optical properties of the films were tested. The results showed that CeF3 crystal with good crystallinity could be prepared using tungsten crucible,keeping it at 1500 ℃ for 1 h and the vacuum was 1 × 10-2 Pa,the temperature gradient was 100 ℃·h-1. The addition of NH4 HF2 as a deoxidizer reduced the oxygen content of the product from 0. 54% to 0. 1 %（ mass fraction）. The CeF3 crystals with two kinds of oxygen content were used for the coating experiment. The crystal with low oxygen content was stable and fluctuated between ± 0. 05 nm·s-1,which indicated that the decrease of oxygen content could improve the evaporation characteristics of the material; the coating residue was composed of black part,white part,black and white part,and the oxygen content of the black part was 7. 92%. The CeF3 film performance test showed that the refractive index was 1. 6 and the absorption coefficient was 3 × 10-4 at a wavelength of 550 nm.
作者
吴心平
张碧田
彭程
Wu Xinping;Zhang Bitian;Peng Cheng(Division of Rare Metals Metallurgy and Materials,Beijing General Research Institute for Nonferrous Metal,Beijing 100088,China)
出处
《稀有金属》
EI
CAS
CSCD
北大核心
2018年第12期1287-1293,共7页
Chinese Journal of Rare Metals
基金
国家自然科学基金项目(51171029)资助
关键词
CeF3晶体
温度梯度法
光学镀膜材料
CeF3crystal
temperature gradient method
optical coating material
