采用微波法合成了Na3La1-x(VO4)2:xEu3+(0<x≤0.40)系列红色荧光粉,探讨了微波反应时间、Eu3+浓度等对荧光粉的结构、形貌和发光性质的影响.结果表明:以MnO2为微波吸收剂,微波功率约为560 W,中高火,反应时间为15~30 min,可合成正交晶系Na3La(VO4)2:Eu3+的纯相,且结晶良好.样品的微观形貌呈不规则块状,尺寸为微米级,且随着反应时间的延长,粒径逐渐增大.Na3La(VO4):Eu3+主激发峰位于320 nm处,最强发射峰位于620 nm处,呈红光发射.微波反应20 min时,主发射峰强度最大.随着Eu3+浓度不断增加,样品的主发射峰强度呈先增强后减弱的趋势,当Eu3+摩尔分数x为0.32时,强度达到最大,此后逐渐减弱,主要由电偶极-电四极相互作用引起.Na3La0.68(VO4)2:0.32Eu3+在不同温度下的发射光谱显示,在473 K温度下,样品主发射峰强度约为室温时的68%,说明样品具有良好的热稳定性.基于Eu3+在538 nm(5D1→7F1)和594 nm(5D0→7F1)的荧光强度比,计算出样品的最大绝对灵敏度Sa和最大相对灵敏度Sr分别为1.23×10-3/K和2.94%/K,表现出良好的温度传感特性.
A series of Na3La1-x(VO4)2:xEu3+(0<x≤0.40)red phosphors were synthesized by microwave radiation method. The effects of microwave reaction time and Eu3+ concentration on the structure, morphology and luminescence properties of the phosphors were investigated. The results show that the pure phase of orthorhombic Na3La(VO4)2:Eu3+ with high crystallinity can be synthesized by selecting MnO2 as the microwave absorbent, microwave power of about 560 W and reaction time of 15~30 min. The micromorphology of the sample is irregular, the particle size is in the level of micron, and the size increases gradually with the extension of reaction time. The main excitation peak of Na3La(VO4)2: Eu3+ is located at 320 nm, and the strongest emission peak is located at 620 nm, showing red emission. When the microwave reaction time is 20 min, the intensity of the main emission peak reaches the maximum.- DOI:10.3969/j.issn.1000-1565.2025.04.004红色荧光粉Na3La(VO4)2:Eu3+的微波合成及光学温度传感性能李子璇,陈金润,邸紫萌,王腾越,程飞扬,翟永清(河北大学 化学与材料科学学院,河北 保定 071002)摘 要:采用微波法合成了Na3La1-x(VO4)2:xEu3+(0<x≤0.40)系列红色荧光粉,探讨了微波反应时间、Eu3+浓度等对荧光粉的结构、形貌和发光性质的影响.结果表明:以MnO2为微波吸收剂,微波功率约为560 W,中高火,反应时间为15~30 min,可合成正交晶系Na3La(VO4)2:Eu3+的纯相,且结晶良好.样品的微观形貌呈不规则块状,尺寸为微米级,且随着反应时间的延长,粒径逐渐增大.Na3La(VO4):Eu3+主激发峰位于320 nm处,最强发射峰位于620 nm处,呈红光发射.微波反应20 min时,主发射峰强度最大.随着Eu3+浓度不断增加,样品的主发射峰强度呈先增强后减弱的趋势,当Eu3+摩尔分数x为0.32时,强度达到最大,此后逐渐减弱,主要由电偶极-电四极相互作用引起.Na3La0.68(VO4)2:0.32Eu3+在不同温度下的发射光谱显示,在473 K温度下,样品主发射峰强度约为室温时的68%,说明样品具有良好的热稳定性.基于Eu3+在538 nm(5D1→7F1)和594 nm(5D0→7F1)的荧光强度比,计算出样品的最大绝对灵敏度Sa和最大相对灵敏度Sr分别为1.23×10-3/K和2.94%/K,表现出良好的温度传感特性.关键词:钒酸盐;微波法;红色荧光粉;白光LED;光学温度传感中图分类号:O611;O614 文献标志码:A 文章编号:1000-1565(2025)04-0361-11Microwave synthesis and optical temperature sensing properties of red phosphors Na3La(VO4)2:Eu3+LI Zixuan, CHEN Jinrun, DI Zimeng, WANG Tengyue, CHENG Feiyang, ZHAI Yongqing( College of Chemistry and Materials Science, Hebei University, Baoding 071002, China)Abstract: A series of Na3La1-x(VO4)2:xEu3+(0<x≤0.40)red phosphors were synthesized by microwave radiation method. The effects of microwave reaction time and Eu3+ concentration on the structure, morphology and luminescence properties of the phosphors were investigated. The results show that the pure phase of orthorhombic Na3La(VO4)2:Eu3+ with high crystallinity can be synthesized by selecting MnO2 as the microwave absorbent, microwave power of about 560 W and reaction time of 15~30 min. The micromorphology of the sample is irregular, the particle size is in the level of micron, and the size increases gradually with the extension of reaction time. The main excitation peak of Na3La(VO4)2: Eu3+ is located at 320 nm, and the strongest emission peak is located at 620 nm, showing red emission. When the microwave reaction time is 20 min, the intensity of the main emission peak reaches the maximum.- 收稿日期:2025-01-10;修回日期:2025-02-06 基金项目:国家自然科学基金项目(22175052);中央引导地方科技发展资金项目(246Z7759G);国家级大学生创新创业训练计划项目(DC2024391;202410075039) 第一作者:李子璇(1998—),女,河北大学在读硕士研究生,主要从事稀土掺杂钒酸盐发光材料的研究.E-mail:likeyzixuan@163.com 通信作者:翟永清(1970—),女,河北大学教授,博士,主要从事稀土发光材料的研究.E-mail:zhaiyongqinghbu@163.com 第4期李子璇等:红色荧光粉Na3La(VO4)2:Eu3+的微波合成及光学温度传感性能河北大学学报(自然科学版) 第45卷Increase of Eu3+ concentration results in the increase of main emission peak intensity of the sample, followed by the gradual decrease. The highest intensity is achieved at the Eu3+ concentration x of 0.32. This is attributed to the electric dipole-electric quadrupole interactions. The emission spectra of Na3La0.68(VO4)2:0.32Eu3+ recorded at different temperatures show that the main emission peak intensity of the sample at 473 K is about 68% of that at room temperature, indicating that the sample has good thermal stability. Based on the fluorescence intensity ratio of Eu3+ at 538 nm(5D1→7F1)and 594 nm(5D0→7F1), the maximum absolute sensitivity Sa and relative sensitivity Sr of the sample were calculated to be 1.23×10-3/K and 2.94%/K, respectively, showing good temperature sensing characteristics.
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