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1. 内蒙古师范大学 物理与电子信息学院, 内蒙古 呼和浩特 010022
2. 内蒙古自治区功能材料物理与化学重点实验室, 内蒙古 呼和浩特 010022
3. 吉林大学 口腔医学院, 吉林 长春 130021
4. 大连路明发光科技股份有限公司,辽宁 大连,116025
Received:17 April 2017,
Revised:22 May 2017,
Published:05 October 2017
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刘文全, 史瑞新, 段如霞等. Ca<em><sub>x</sub></em>Si合金前驱物常压氮化制备Ca<sub>1-<em>x</em></sub>AlSiN<sub>3</sub>:<em>x</em>Eu<sup>2+</sup>红色荧光粉及发光性能研究[J]. 发光学报, 2017,38(10): 1295-1301
LIU Wen-quan, SHI Rui-xin, DUAN Ru-xia etc. Preparation and Luminescence Properties of Ca<sub>1-<em>x</em></sub>AlSiN<sub>3</sub>:<em>x</em>Eu<sup>2+</sup> Red Phosphors by Atmospheric Nitriding Method with Ca<em><sub>x</sub></em>Si Alloy Precursors[J]. Chinese Journal of Luminescence, 2017,38(10): 1295-1301
刘文全, 史瑞新, 段如霞等. Ca<em><sub>x</sub></em>Si合金前驱物常压氮化制备Ca<sub>1-<em>x</em></sub>AlSiN<sub>3</sub>:<em>x</em>Eu<sup>2+</sup>红色荧光粉及发光性能研究[J]. 发光学报, 2017,38(10): 1295-1301 DOI: 10.3788/fgxb20173810.1295.
LIU Wen-quan, SHI Rui-xin, DUAN Ru-xia etc. Preparation and Luminescence Properties of Ca<sub>1-<em>x</em></sub>AlSiN<sub>3</sub>:<em>x</em>Eu<sup>2+</sup> Red Phosphors by Atmospheric Nitriding Method with Ca<em><sub>x</sub></em>Si Alloy Precursors[J]. Chinese Journal of Luminescence, 2017,38(10): 1295-1301 DOI: 10.3788/fgxb20173810.1295.
采用Ca
x
Si合金前驱物和EuB
6
常压氮化制备了CaAlSiN
3
:Eu
2+
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CaAlSiN
3
结构,空间群为
Cmc
2
1
。CaAlSiN
3
:Eu
2+
红色荧光粉的最佳烧结温度为1550℃。添加质量分数为6%的SrF
2
助熔剂后,荧光粉发光强度的提升效果最好。添加6% SrF
2
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Ca
0.98
AlSiN
3
:0.02Eu
2+
红色荧光粉应用在白光LED的封装中,获得了色温为3109 K、显色指数为92.5以及色温为4989 K、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。
CaAlSiN
3
:Eu
2+
red phosphors were synthesized through nitrating process under atmospheric pressure with Ca
x
Si alloy as precursor and EuB
6
powder as activator. The influences of different sintering temperature
fluxing agent and secondary sintering on the characteristics of morphology
crystalline structure
luminescent properties and thermal stability of CaAlSiN
3
:Eu
2+
red phosphors were investigated by scanning electron microscopy (SEM)
X-ray diffraction (XRD) and fluorescence spectrophotometer. It displays that the nitride synthetic has CaAlSiN
3
structure with space group
Cmc
2
1
and its optimum sintering temperature is 1550℃. The performance of its luminous intensity was significantly enhanced when the mass fraction of SrF
2
flux was 6%. In the secondary sintering
the relative intensity of emission spectrum was nearly doubled
the grain size was optimized
and the relative intensity of the emission spectrum was also improved. Appling Ca
0.98
AlSiN
3
:0.02Eu
2+
red phosphor with 640 nm emission wavelength in white LED packaging
the devices with high color rendering index of 92.5 and 95.8
corresponding color temperature of 3109 K and 4989 K were obtained
respectively. The results indicate that the white LED emitting devices with high rendering index of positive white and warm white can be achieved by applying nitride synthetic.
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