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采用CaxSi合金前驱物和Eu B6常压氮化制备了Ca Al Si N3∶Eu2+氮化物红色荧光粉。研究了不同烧结温度、添加助熔剂及二次烧结对发光性能的影响。通过扫描电子显微镜(SEM)、X射线衍射(XRD)、荧光分光光度计对发光材料的形貌、晶体结构、发光性能与热稳定性进行了研究。分析结果表明:通过合金前驱物常压氮化法得到的氮化物荧光粉具有Ca Al Si N3结构,空间群为Cmc21。Ca Al Si N3∶Eu2+红色荧光粉的最佳烧结温度为1 550℃。添加质量分数为6%的Sr F2助熔剂后,荧光粉发光强度的提升效果最好。添加6%Sr F2助熔剂及二次烧结后得到的荧光粉的晶粒生长更加完整,颗粒度明显改善,发射光谱的相对强度也明显提高,比未加助熔剂单次烧结的荧光粉相对强度提高了近一倍。将发射峰位在640 nm的Ca0.98Al Si N3∶0.02Eu2+红色荧光粉应用在白光LED的封装中,获得了色温为3 109 K、显色指数为92.5以及色温为4 989K、显色指数为95.8的高显色白光LED,说明本文合成的氮化物红色荧光粉可以实现暖白光和正白光高显色的白LED发光器件。
CaAlSiN3:Eu2 + nitride red phosphor was prepared by CaxSi alloy precursor and Eu B6 atmospheric pressure nitriding. The effects of different sintering temperature, flux addition and secondary sintering on the luminescent properties were studied. The morphology, crystal structure, luminescent properties and thermal stability of the luminescent materials were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD) and fluorescence spectrophotometer. The analysis results show that the nitride phosphor obtained by the atmospheric pressure nitriding of the alloy precursor has a CaAlSiN3 structure and the space group is Cmc21. The optimum sintering temperature of Ca Al Si N 3:Eu 2+ red phosphor is 1 550 ℃. After adding Sr F2 flux with mass fraction of 6%, the luminous intensity of phosphor is the best. The addition of 6% Sr F2 flux and the phosphor obtained after the secondary sintering have more complete grain growth, significantly improved grain size, and significantly improved relative intensity of the emission spectrum. The relative intensities of the phosphors without single flux sintering Nearly doubled. The Ca0.98Al Si N3: 0.02Eu2 + red phosphor with peak emission at 640 nm was used in the encapsulation of white LED. The color temperature was 3 109 K, the color rendering index was 92.5 and the color temperature was 4 989 K. The color rendering index was 95.8 high color rendering white LED, indicating that this article synthesized nitride red phosphor can achieve warm white and white is high color rendering white LED light-emitting devices.