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第 36 卷第 5 期                             精   细   化   工                                  Vol.36, No.5
             201 9 年 5 月                             FINE CHEMICALS                                 May    2019


              功能材料
                                                                                         3+
                         发光增强的红色荧光粉 Li Zr O :Eu 的
                                                                             2
                                                                                 7
                                                                       6
                                                微波固相合成


                           隆金桥,韦金雷,欧阳思铭,孙榕励,谭能文,舒   韦

                                     (百色学院  化学与环境工程学院,广西  百色    533000)

                                                                                                      3+
                 摘要:以硝酸锆、硝酸锂、Eu(NO 3 ) 3 6H 2 O 为原料,采用微波固相烧结法合成了系列红色荧光粉 Li 6 Zr 2 O 7 :Eu 。
                                                                                            3+
                 利用 XRD 和荧光光度计对样品的组成和发光性能进行了表征。考察了烧结时间、烧结温度及 Eu 的含量对荧光
                                                           3+
                 粉发光性能的影响。XRD 分析结果表明,Li 6 Zr 2 O 7 :Eu 荧光粉为纯相晶体结构。根据离子电负性标度可知,Eu                       3+
                                             4+
                                                                                                     3+
                 (1.433)会优先取代电负性相近 Zr 的位置(1.610)。当微波烧结时间为 10  min、烧结温度为 500 ℃、Eu 在
                 晶体中的含量为 14%时(以 Li 6 Zr 2 O 7 的物质的量为基准,下同),在 465 nm 激发下,制备得到的 Li 6 Zr 2 O 7 :0.14Eu    3+
                 荧光粉在 615 nm 处产生最强的红光发射,且发射光谱在 615 nm 的强度是激发光谱在 465 nm 强度的 1.54 倍。
                 此时荧光粉色坐标为 X=0.65,Y=0.35,具有很高的色纯度,与商用红色荧光粉(0.63,0.34)相比更接近国家标准
                 (0.67,0.33)。
                 关键词:微波固相;发光增强;红色荧光粉;功能材料
                 中图分类号:TB39;O482.31      文献标识码:A      文章编号:1003-5214 (2019) 05-0807-06



                        Microwave Solid Phase Synthesis of a Red-emitting Phosphor
                                               3+
                                Li 6Zr 2O 7:Eu with Luminescence Enhancement

                    LONG Jin-qiao, WEI Jin-lei, OUYANG Si-ming, SUN Rong-li, TAN Neng-wen, SHU Wei
                       (College of Chemistry & Environment Engineering, Baise University, Baise 533000, Guangxi, China)

                                                                 3+
                 Abstract: A series of red-emitting phosphors Li 6Zr 2O 7:Eu  were synthesized by microwave solid phase
                 sintering using zirconium nitrate, lithium nitrate and Eu(NO 3) 3·6H 2O as raw materials. The composition and
                 luminescence  properties  of  the  samples  were  characterized  by  XRD  and  fluorescence  photometer.  The
                                                                       3+
                 effects of sintering time, sintering temperature and content of Eu on the luminescence properties of the
                                                                                                      3+
                 phosphors  were  investigated.  The  results  showed  that  the  samples  had  crystal  phases  of  Li 6Zr 2O 7:Eu .
                                                                                                       4+
                                                      3+
                 According to ionic electronegativity scale, Eu  (1.433) ions gave priority to replacing the position of Zr
                 (1.610)  ions,  which  had  similar  electronegativity.  When  the  sintering  time  was  10  min,  the  sintering
                                                     3+
                 temperature was 500  ℃, the content of Eu ions was 14% of molar amount of Li 6Zr 2O 7, under 465 nm
                                                           3+
                 excitation, the prepared phosphor Li 6Zr 2O 7:0.14Eu  generated the strongest red emission at 615 nm. Its
                 emission spectrum at 615 nm was 1.54 times stronger than that of excitation spectrum at 465 nm. At this
                                                                                           3+
                 point, its fluorescence pink coordinate was X=0.65, Y=0.35. The phosphor Li 6Zr 2O 7:0.14Eu had very high
                 color purity, closer to the national standard (0.67, 0.33) than the commercial red-emitting phosphor (0.63, 0.34).
                 Key  words:  microwave  solid  phase;  luminescence  enhancement;  red-emitting  phosphor;  functional
                 materials
                 Foundation items: National Natural Science Foundation of China (21661006); Key Project of Scientific
                 Research in Colleges and Universities in Guangxi (KY2015ZD117); National College Students Innovation
                 and Entrepreneurship Plan Project in 2017 (201710609004)

                 收稿日期:2018-07-18;  定用日期:2019-01-02; DOI: 10.13550/j.jxhg.20180531
                 基金项目:国家自然科学基金(21661006);广西高校科研重点项目(KY2015ZD117);2017 年国家级大学生创新创业计划立项项目
                 (201710609004)
                 作者简介:隆金桥(1970—),男,副教授,E-mail:long_403@163.com。
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