Preparation of Novel Rare-Earth-Doped (Oxy)Nitride Phosphor and Evaluation of Characteristics

新型稀土掺杂（氧）氮化物荧光粉的制备及特性评价

基本信息

批准号：
20560630
负责人：
ITATANI Kiyoshi
金额：
$ 2.58万
依托单位：
Sophia University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2008
资助国家：
日本
起止时间：
2008 至 2010
项目状态：
已结题

项目摘要

In this work, Eu^<2+>-doped alkaline earth silicon nitride (Ca_2Si_5N_8 : 1mol% Eu^<2+> ; (Ca_<0.99>Eu_<0.01>)_2Si_5N_8) was synthesized by carbothermal reduction and nitridation of (oxy) nitride/oxide powder prepared by ultrasonic spray pyrolysis (USP-CRN). The starting solution (0.1mol・dm^<-3>) containing Si_3N_4, Ca(NO_3)_2 and Eu(NO_3)_3 ((Ca+Eu)/Si ratio=0.4) was spray-pyrolyzed at 600℃. After the spray-pyrolyzed powder was mixed with carbon (the ratio of carbon amount to stoichiometric amount ; 1.50), the mixture was heated at a temperature between 1400 and 1550℃ for 2h in N_2 atmosphere. A single phase of Ca_2Si_5N_8 could be obtained when the mixture had been carbothermally nitrided at and above 1500℃. Moreover, the synthesis of (Ca_<0.99>Eu_<0.01>)_2Si_5N_8 was conducted by the USP-CRN technique, using colloidal silica (SiO_2 ; CS), and solid-state reaction (SSR) and CRN. When the black light was irradiated to the (Ca_<0.99>Eu_<0.01>)_2Si_5N_8, the orange light was emitted. The relative emission intensities, compared to the case of YAG, i.e., the standard substance : Y_3Al_5O_<12>:Ce^<3+> (YAG), were : 0.494 (SSR-CRN)>0.452 (USP-CRN : utilization of Si_3N_4 as Si source)>0.0371 (USP-CRN ; utilization of CS as Si sourse). The relative emission intensity of (Ca_<0.99>Eu_<0.01>)_2Si_5N_8) prepared by USP-CRN, using Si_3N_4 as Si source, was almost comparable to that prepared by SSR-CRN. SEM micrograph of this powder heated at 1500℃ for 2h in N_2 atmosphere showed the spherical particles with diameters of around 2・m. Such particles are expected to be available as a phosphor for white-light LED.

本工作通过碳热还原和(oxygen)氮化合成了Eu^<2+>掺杂的碱土硅氮化物(Ca_2Si_5N_8 : 1mol% Eu^<2+> ; (Ca_<0.99>Eu_<0.01>)_2Si_5N_8)。）通过超声波喷雾热解制备的氮化物/氧化物粉末（USP-CRN）起始溶液。将含有Si_3N_4、Ca(NO_3)_2和Eu(NO_3)_3((Ca+Eu)/Si比=0.4)的(0.1mol·dm^<-3>)在600℃下喷雾热解。将粉末与碳混合（碳量与化学计量比为1.50），将混合物在1400-1400℃之间加热。在N_2气氛中1550℃保温2h，在1500℃及以上温度下进行碳热氮化，得到Ca_2Si_5N_8单相。此外，根据USP合成了(Ca_<0.99>Eu_<0.01>)_2Si_5N_8。 -CRN技术，使用胶态二氧化硅（SiO_2；CS），以及当黑光照射到(Ca_<0.99>Eu_<0.01>)_2Si_5N_8时，与YAG的情况相比，发出橙色光，即：标准物质：Y_3Al_5O_<12>:Ce^<3+> (YAG)，得：0.494 (SSR-CRN)>0.452 (USP-CRN : 使用 Si_3N_4 作为 Si 源)>0.0371 (USP-CRN ; 使用 CS 作为 Si 源) (Ca_<0.99>Eu_<0.01>)_2Si_5N_8 的相对发射强度。）由 USP-CRN 使用 Si_3N_4 作为 Si 源制备的，几乎与该粉末在N_2气氛中于1500℃加热2h的SSR-CRN显微照片显示，这种颗粒的直径约为2μm，预计可用作白光LED的荧光粉。