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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、SEM、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10-2pa真空度下1500℃保温1h,以100℃/h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(wt%)降低到0.1(wt%)。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±0.5?/s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(wt%)。CeF3膜层性能测试表明,在波长为550nm处,折射率为1.6,吸收系数为3×10-4。
Using CeF3 powder as raw material, CeF3 crystal was prepared by temperature gradient method in vacuum carbon tube furnace. The products under different influencing factors were characterized by X-ray diffraction, SEM, EDS and other methods. The CeF3 crystal was coated and the optical properties of the obtained film were tested. The results show that CeF3 crystals with good crystallinity can be prepared by tungsten crucible under the vacuum of 10-2pa at 1500 ℃ for 1h and at a temperature gradient of 100 ℃ / h. Addition of NH4HF2 as a deoxidizer can reduce the oxygen content in the product from 0.54 (wt%) to 0.1 (wt%). The experiments show that the lower the oxygen content, the lower the oxygen content is, the more stable the fluctuation rate of the coating rate is and the variation is between ± 0.5 μs / s, indicating that the reduction of oxygen content can significantly improve the evaporation characteristics of the material ; Coating residue from the black, white, black and white over three parts, the black part of the oxygen content of up to 7.92 (wt%). CeF3 film performance tests showed that at a wavelength of 550nm, the refractive index of 1.6, the absorption coefficient of 3 × 10-4.