稀土金属离子掺杂硅酸盐基发光材料的制备及性能研究
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摘要
采用水热法和溶胶凝胶法(sol-gel)制备稀土离子Ce和Eu掺杂的Sr_2MgSi_2O_7硅酸盐基发光材料,采用X射线衍射仪(XRD)、透射电子显微镜(TEM)、荧光分光光度计(PL)对样品的晶体结构、形貌及光学性能进行测试。研究不同制备方法、热处理条件和稀土离子掺杂浓度等对硅酸盐基发光材料结构及其光致发光性能的影响。测试结果表明,水热法制备的硅酸盐基发光材料在220℃保温2天开始形成Sr_2MgSi_2O_7相,延长保温时间,Sr_2MgSi_2O_7相含量增加但比较缓慢。对水热反应产物经过800℃的后续热处理,主要成分为Sr_2MgSi_2O_7,仅含少量的SrSiO_3相。采用sol-gel法硅酸盐基发光材料经1000℃热处理的产物中主要存在Sr_2MgSi_2O_7相和少量的Sr_2SiO_4的杂质相。光致发光谱研究表明,经还原气氛处理的Ce离子掺杂Sr_2MgSi_2O_7样品中均存在波长位于371nm的宽带紫外发光,该发光为存在于Sr_2MgSi_2O_7晶体Sr位的Ce~(3+)离子的5d-4f的电子跃迁所产生。sol-gel法制备的Eu掺杂Sr_2MgSi_2O_7样品中,在空气中处理样品的发光为由395nm激发产生的位于590nm和612nm的红色发光,而采用水热法制备的Eu掺杂Sr_2MgSi_2O_7样品经空气中热处理后仅存在由403nm紫光激发产生的604nm的红色发光。经还原气氛处理后两种方法制备的样品的发光均为位于465nm左右的蓝色宽带发光,并且随着处理温度的升高,发光峰强度上升。
Ce and Eu ions doped Sr_2MgSi_2O_7 materials had been prepared by hydrothermal and sol-gel methods. Effects of synthesized methods, annealing temperature and time and concentrations of rare-earth metal ions on the structures and the luminescence properties of the silicate materials were studied using X-ray diffractometer (XRD), transmission electron microscope (TEM) and spectrofluorometers (PL). The results show that the Sr_2MgSi_2O_7 phase can be obtained by the hydrothermal method operated at 220℃for 2d, and the content of the Sr_2MgSi_2O_7 phase increases when increasing the reaction time to 6d. When the hydrothermal products were heat treated at 800℃, the mail phase of the products is Sr_2MgSi_2O_7 with a little bit impurity, i.e., SrSiO_3 phase. The products obtained employing the sol-gel method operated at 1000℃mainly consists of Sr_2MgSi_2O_7 phase and small amount of Sr_2SiO_4 impurity. Studies on the photoluminescence patterns show that the wide UV emission band with the wavelength at 371nm exists in both Ce ions doped Sr_2MgSi_2O_7 samples synthesized by the hydrothermal method and sol-gel method. This emission originates from the 5d-4f electron transition of Ce ions existing in the Sr ions place in the Sr_2MgSi_2O_7 crystals. Two red emission bands with the wavelength at 590nm and 612nm excited at 395nm can be observed in the Eu ions doped Sr_2MgSi_2O_7 samples obtained by sol-gel method, after heat-treated in air. However, only one emission band with the wavelength at 604nm with the excitation band at 403nm exists in the Eu ions doped Sr_2MgSi_2O_7 samples obtained by hydrothermal method, after heat treated in air. In these two kinds of the samples obtained by the sol-gel and hydrothermal methods, a blue emission band with the wavelength at 465nm can be obtained when heat-treated in hydrogen atmosphere, and the intensity of this blue emission increases with the increasing of the heat treating temperature.
Ce and Eu ions doped Sr_2MgSi_2O_7 materials had been prepared by hydrothermal and sol-gel methods. Effects of synthesized methods, annealing temperature and time and concentrations of rare-earth metal ions on the structures and the luminescence properties of the silicate materials were studied using X-ray diffractometer (XRD), transmission electron microscope (TEM) and spectrofluorometers (PL). The results show that the Sr_2MgSi_2O_7 phase can be obtained by the hydrothermal method operated at 220℃for 2d, and the content of the Sr_2MgSi_2O_7 phase increases when increasing the reaction time to 6d. When the hydrothermal products were heat treated at 800℃, the mail phase of the products is Sr_2MgSi_2O_7 with a little bit impurity, i.e., SrSiO_3 phase. The products obtained employing the sol-gel method operated at 1000℃mainly consists of Sr_2MgSi_2O_7 phase and small amount of Sr_2SiO_4 impurity. Studies on the photoluminescence patterns show that the wide UV emission band with the wavelength at 371nm exists in both Ce ions doped Sr_2MgSi_2O_7 samples synthesized by the hydrothermal method and sol-gel method. This emission originates from the 5d-4f electron transition of Ce ions existing in the Sr ions place in the Sr_2MgSi_2O_7 crystals. Two red emission bands with the wavelength at 590nm and 612nm excited at 395nm can be observed in the Eu ions doped Sr_2MgSi_2O_7 samples obtained by sol-gel method, after heat-treated in air. However, only one emission band with the wavelength at 604nm with the excitation band at 403nm exists in the Eu ions doped Sr_2MgSi_2O_7 samples obtained by hydrothermal method, after heat treated in air. In these two kinds of the samples obtained by the sol-gel and hydrothermal methods, a blue emission band with the wavelength at 465nm can be obtained when heat-treated in hydrogen atmosphere, and the intensity of this blue emission increases with the increasing of the heat treating temperature.
引文
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[3]张中太,张俊英编著.无机光致发光材料及应用》,[M].北京,化学工业出版社,2005,69-72
[4]陈丽白,郭震宁,林介本.一维光子晶体微腔在硅基发光材料中的应用研究[J].光学学报,2008, 28(9): 1793-1797
[5]王少艳.长余辉发光材料在陶瓷工艺中的应用[J].河北理工大学学报(自然科学版),2008, 30(02): 49-51
[6]段军强,余兴海,黄京根,蒋健平.新一代碱土铝酸盐系稀土长余辉发光材料的研究进展[J].中国照明电器,2004,25(06):1-6
[7]王元生.具有重要应用前景的新型发光材料:透明玻璃陶瓷[J].功能材料信息,2007,(05):25-28
[8]占文,王周福,周秀坤等.低温固相反应法合成钇铝石榴石粉体的研究[J].武汉科技大学学报,2009,32(2):201-204
[9]季振国,刘坤,向因等.利用固相反应法在硅片上制备硅酸锌发光薄膜及表征[J].半导体学报,2004,25(7):794-797
[10]席俊华,季振国,刘坤等.掺Mn硅酸锌薄膜中微量氧化锌对发光强度的影响[J].无机材料学报,2006,27(06):25-30
[11] H.X. Zhang, S. Buddhudu, C.H. Kam, et al. Luminescence of Eu3+ and Tb3+ doped Zn2SiO4 nanometer powder phosphors[J]. Materials Chemistry and Physics. 2001, 68(2): 31-35
[12] J. Lin, Dirk U. Sanger, M. Mennig, et al. Sol-gel deposition and characterization of Mn2+-doped silicate phosphor films[J]. Thin Solid Films, 2000, 36(1): 39-45
[13]李彬,佟德成,李锦莲.溶胶-凝胶法研究CaO-MgO-Fe_2O_3-SiO_2玻璃粉[J].佳木斯大学学报(自然科学版),2002,22(02):23-26
[14]余家国,熊建锋,程蓓.高活性二氧化钛光催化剂的低温水热合成[J].催化学报,2005,26(09):745-749
[15]白波,赵景联.纳米TiO2的微波水热法制备及其光催化性能研究[J].化学通报,2005,25(10):776-780
[16] Eunyoung Bae, Naoya Murakami, Teruhisa ohno. Exposed crystal surface-controlled TiO2 nanorods having rutile phase from TiCl3 underhydrothermal conditions[J]. Journal of Molecular Catalysis A: Chemical. 2009, 300(3): 72-79
[17]郑燕青,施尔畏,李汶军等.水热条件下二氧化钛晶体同质变体的形成[J].中国科学E辑,2001,45(03) 59-63
[18]张中太,张俊英编著.无机光致发光材料及应用[M].北京,化学工业出版社,138-139
[19]邢明铭,曹望和,付姚.络合沉淀法合成纳米Y2O3: Yb, Er及其上转换发光性能[J].功能材料,2006,37(09):1375-1377
[20]胡俊涛,郭常新,陈建刚,张琳丽.气相沉积法生长不同结构ZnO纳米线及其发光[J].发光学报,2005,26(06):781-784
[21] Lei Zhou, Bing Yan. Novel silicate sources synthesized nanophosphors Zn2SiO4: Eu3+ and luminescent property[J]. Journal of optoelectronics and advanced materials, 2007, 9(9): 2754-2758
[22]席俊华,季振国,刘坤,王超,杜鹃.掺Mn硅酸锌薄膜中微量氧化锌对发光强度的影响[J].无机材料学报,2006,21(06):1506-1510
[23] Jong Su Kin, Pyung Eun Jeon, Yun Hyung Park, et al. White-light generation through ultraviolet-emitting diode and white-emitting phosphor[J]. Applied physics letters. 2004, 85(17): 3696-3698
[24]季振国,刘坤,向因,宋永梁,叶志镇.利用固相反应法在硅片上制备硅酸锌发光薄膜及表征[J].半导体学报,2004,25(07):794-797
[25]杨莺,陈治明,赵高扬.硅衬底上PZT薄膜的制备及其特性分析[J].半导体学报,2004,25(04):404-409
[26]雷炳富,刘应亮,华瑞年等.偏硅酸镉的自激活发光[J].分子科学学报,2004,20(1):57-61
[27] Lei Bingfu, Liu Yingliang, Liu Jie, et a1. Pink light emitting long-lasting phosphorescence in Sm3+-doped CdSiO3[J]. J Solid State Chem, 2004, 177(4-5): 1333-1337
[28] Lei Bingfu, Liu Yingliang, Ye Zeren, et a1. Luminescence properties of CdSiO3:Mn2+ phosphor[J]. J Lumin, 2004, 109 (3-4): 215-219
[29]肖志国.蓄电池发光材料及其制品(第二版)[M].北京化学工业出版社,2002
[30] Lin Yuanhua, Zhang Zhongtai, Tang Zilong, et a1. Luminescent properties of a new long afterglow Eu2+ and Dy3+ activated Ca3MgSi2O8 phosphor[J]. J Euro Ceram Soc, 2001, 21(5): 683-685
[31] Lin Yuanhua, Nan Ce-Wen, Zhou Xisong, et a1. Preparation and characterization of long afterglow M2MgSi2O7-based (M: Ca, Sr, Ba) photoluminescent phosphors[J]. Mater Chem Phys, 2003, 82(3): 860-863
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