稀土掺杂四硼酸钇铝荧光粉的制备与性能研究
摘要
四硼酸铝钇(YAl_3(BO_3)_4, YAB)以其优异的力学、热学和光学性能,而在发光材料和激光材料领域具有广阔的应用前景。本论文对稀土离子掺杂的YAB红光及绿光荧光粉进行了研究,讨论了粉体合成、制备工艺、结构与性能之间的关系,取得的结果如下:
1、分别采用固相合成法、硝酸盐热分解法和溶胶-凝胶燃烧法制备了YAB粉体。通过X射线衍射(XRD)和扫描电镜(SEM)分析了所得粉体的物相和形貌。结果表明:三种方法合成YAB纯相的最低温度依次为:1200℃、1100℃和1000℃,且制备过程中硼酸的最佳用量分别为140%、120%和120%。另外,对溶胶-凝胶燃烧法中硝酸盐和柠檬酸的比值对合成粉体的影响进行了研究。SEM分析显示,当为二者比值为1:1.5时合成的YAB粉体粒度均匀,且粉体具有较好的分散性。
2、采用上述三种方法分别合成了(Y,Gd)Al3(BO3)4:Eu~(3+)荧光粉,研究了合成方法,稀土离子的性质和浓度等因素对其粉体发光性能的影响。结果表明:溶胶-凝胶燃烧法、硝酸盐热分解法和固相合成法所合成的荧光粉发光强度依次降低;对于溶胶-凝胶燃烧法所制备的(Y,Gd)Al3(BO3)4:Eu~(3+)荧光粉,Eu~(3+)的最佳掺杂浓度为18%;且随着Gd~(3+)浓度的增加,Eu~(3+)的发射强度先增大而后减小,当掺杂浓度为75%时强度最大。
3、采用溶胶-凝胶燃烧法在1100℃下合成了纯相(YGd)Al3(BO3)4:Tb~(3+)粉体,研究了Tb~(3+)和Gd~(3+)掺杂量对荧光粉性能的影响。结果表明:随着Tb~(3+)浓度的增大,所合成粉体的发光强度先增大后减小,Tb~(3+)的猝灭浓度为25%;在Tb~(3+)浓度确定时,其发射强度随着Gd~(3+)掺杂量的增大而增大。
Yttrium aluminium both borate (YAl_3(BO_3)_4, YAB) have good properties of mechanics, thermotics and optics, which have a wide applications in the matrix materials of luminescent powder and laser. In this paper, rare earth ions doped YAB phosphors were investigated. Results are obtained as follows:
1 YAB powders were synthesized by solid state reaction, pyrogenic decomposition of nitrate, sol-gel combustion methods, respectively. Results of X-ray powder diffractometry (XRD) and scanning electron microscopy (SEM) show that:
For these three methods, the lowest temperatures at which the single phase powders were synthesized were 1200℃, 1100℃and 1000℃, respectively.And in order to obtain the single phase of YAB, 40%,20% and 20% of excess H3BO3 were used in the three methods, respectively. SEM shows that the powder synthesized by sol-gel combustion method has the particles with the size of about 400nm and good dispersivity when the molar ratio of nitrate to citric acid is 1: 1.5.
2 (Y,Gd)Al3(BO3)4:Eu~(3+) phosphors were synthesized by those three methods respectively. The XRD and SEM result show that the powder synthesized by sol-gel combustion has good dispersivity and need low temperature. The effects of doping with Gd~(3+) ion were studied.It is found that the emission intensity of Eu~(3+) increases firstly, and then decreases under the excitation of UV with the increasing Gd~(3+) concentration. An optimum Gd~(3+)doping concentration of 75% is obtained.
3 The powders of (Y,Gd)Al3(BO3)4:Tb~(3+) were synthesized by sol-gel combustion method at 1000℃. It is found that the quenching concentration of Tb is about 25%. Emission spectra show that the luminescence intensity of Tb~(3+) increases with the increasing Gd~(3+) doping concentration due to the fact that there exists the energy transfer of Gd~(3+)→Tb~(3+) (6P7/2→5DJ) in (YGd)Al3(BO3)4:Tb~(3+).
1、分别采用固相合成法、硝酸盐热分解法和溶胶-凝胶燃烧法制备了YAB粉体。通过X射线衍射(XRD)和扫描电镜(SEM)分析了所得粉体的物相和形貌。结果表明:三种方法合成YAB纯相的最低温度依次为:1200℃、1100℃和1000℃,且制备过程中硼酸的最佳用量分别为140%、120%和120%。另外,对溶胶-凝胶燃烧法中硝酸盐和柠檬酸的比值对合成粉体的影响进行了研究。SEM分析显示,当为二者比值为1:1.5时合成的YAB粉体粒度均匀,且粉体具有较好的分散性。
2、采用上述三种方法分别合成了(Y,Gd)Al3(BO3)4:Eu~(3+)荧光粉,研究了合成方法,稀土离子的性质和浓度等因素对其粉体发光性能的影响。结果表明:溶胶-凝胶燃烧法、硝酸盐热分解法和固相合成法所合成的荧光粉发光强度依次降低;对于溶胶-凝胶燃烧法所制备的(Y,Gd)Al3(BO3)4:Eu~(3+)荧光粉,Eu~(3+)的最佳掺杂浓度为18%;且随着Gd~(3+)浓度的增加,Eu~(3+)的发射强度先增大而后减小,当掺杂浓度为75%时强度最大。
3、采用溶胶-凝胶燃烧法在1100℃下合成了纯相(YGd)Al3(BO3)4:Tb~(3+)粉体,研究了Tb~(3+)和Gd~(3+)掺杂量对荧光粉性能的影响。结果表明:随着Tb~(3+)浓度的增大,所合成粉体的发光强度先增大后减小,Tb~(3+)的猝灭浓度为25%;在Tb~(3+)浓度确定时,其发射强度随着Gd~(3+)掺杂量的增大而增大。
Yttrium aluminium both borate (YAl_3(BO_3)_4, YAB) have good properties of mechanics, thermotics and optics, which have a wide applications in the matrix materials of luminescent powder and laser. In this paper, rare earth ions doped YAB phosphors were investigated. Results are obtained as follows:
1 YAB powders were synthesized by solid state reaction, pyrogenic decomposition of nitrate, sol-gel combustion methods, respectively. Results of X-ray powder diffractometry (XRD) and scanning electron microscopy (SEM) show that:
For these three methods, the lowest temperatures at which the single phase powders were synthesized were 1200℃, 1100℃and 1000℃, respectively.And in order to obtain the single phase of YAB, 40%,20% and 20% of excess H3BO3 were used in the three methods, respectively. SEM shows that the powder synthesized by sol-gel combustion method has the particles with the size of about 400nm and good dispersivity when the molar ratio of nitrate to citric acid is 1: 1.5.
2 (Y,Gd)Al3(BO3)4:Eu~(3+) phosphors were synthesized by those three methods respectively. The XRD and SEM result show that the powder synthesized by sol-gel combustion has good dispersivity and need low temperature. The effects of doping with Gd~(3+) ion were studied.It is found that the emission intensity of Eu~(3+) increases firstly, and then decreases under the excitation of UV with the increasing Gd~(3+) concentration. An optimum Gd~(3+)doping concentration of 75% is obtained.
3 The powders of (Y,Gd)Al3(BO3)4:Tb~(3+) were synthesized by sol-gel combustion method at 1000℃. It is found that the quenching concentration of Tb is about 25%. Emission spectra show that the luminescence intensity of Tb~(3+) increases with the increasing Gd~(3+) doping concentration due to the fact that there exists the energy transfer of Gd~(3+)→Tb~(3+) (6P7/2→5DJ) in (YGd)Al3(BO3)4:Tb~(3+).
引文
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[3]KimE J , Kang Y C. UV and VUV characteristics of (YGd)2O3:Eu phosphor particles prepared by spray pyrolysis from polymeric precursors. Materials Research Bulletin. 2003, 38(3):515-524.
[4]郑子樵,李红英.稀土功能材料.化学工业出版社.2003.9
[5]北京有色院课题组.稀土发光材料(研究报告摘要).四川稀土.2004,4:2-9
[6]LevineA.K, PAlillaF.C.APPI.Phys.Lerrers.1964, 5:118.
[7]Royce M.R.US patent 3.418.216.1968.
[8]李强,高潇,严东升.纳米Y2O3:Eu3+的荧光特性.无机材料学报.1999,14(1):150– 154
[9]蒋凯,余兴海,叶明新等.溶胶-凝胶法制备小颗粒(Y,Gd)BO3:Eu及其表征.发光学报.2004 25(1):50-60.
[10]姚疆,孙聆东,钱程等.稀土纳米复合氧化物RE2O3:Eu(RE=Y,Gd)的制备及特性.中国稀土学报. 2001, 19(5):427-429
[11]Sang D.H, Pkhatkar S. etal . Combustion synthesis and Luninescent properties of Eu3+-doped LnAlO3 (Ln=YandGd) phosphors.Materials Science and Engineering B.2005.
[12]Ekambaram S,Maaza M. Combustion synthesis and Luminescent propertiesn of Eu3+-activated cheap red phosphors.J of alloys and compounds.2005, (395);132– 134
[13]J.M.P.J.Verstegen. A Survey of a Group of Phosphor, Based on Hexagon Alaluminate and Gallate Host Lattices. J Electrochem Soc,1974,121:1623
[14]Kwang-Bok Kim, Yong-Kim, Hui-Gon Chun. Structural and Optical Properties of BaMgAl10O17:Eu2+ Phosphors. Chem..Mater..2002,14(12):5045-5052.
[15]C.Koshio, H Taniguchi, Amemiya Ketal. New High Luminance 50 inch ACPDPs with an Improved Panel Structure Using T-Shaped Electrode and Waffle structured Ribs.Asia Display IDW,2001:781.
[16]杨智,任敏,林建华等.稀土硼酸盐的结构及其真空紫外(VUV)荧光性质.高等学校化学学.2000, 21(9):1339-1343.
[17]You H P , Hong G Y , Zeng X Q , et al.VUV excitation properties of LnA13B4O12:Re (Ln=Y,Gd; Re=Eu,Tb). Journal of Physics and Chemistry of Solids. 2000, 61:1985-1988.
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