Li_2B_4O_7薄膜的制备与掺杂及其光学性质的研究
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摘要
Li_2B_4O_7材料在被辐射照射后会储存接受的辐射信息,以光释光或热释光的形式释放出来,其数目与接受的辐射剂量密切相关。这一特性可应用于辐射剂量的测量。并且,该物质的有效原子序数Ze=7.26,十分接近人体组织的有效原子序数(Ze=7.13),因此在检测射线强度和分辨射线种类方面都有很好的使用前景。在研究热释光与光释光性质之前,对材料的光学性质的研究是十分有必要的,通过光学性质的研究我们可以获得薄膜材料的能级结构、禁带宽度等信息。我们研究了掺杂后的薄膜的光致发光特性,初步研究了杂质的特征发光谱、杂质能级以及发光淬灭中心对薄膜发光特性的影响。为以后的研究工作积累必要的资料。本工作利用溶胶凝胶法、丝网印刷法制备Li_2B_4O_7薄膜,通过X射线衍射测试对薄膜进行定性分析,用可见-紫外分光光度计以及光致发光法测量薄膜的光学性质;并利用金属元素(Cu、In)掺杂对Li_2B_4O_7薄膜进行了光学性质的改性。XRD分析结果表明溶胶凝胶法制备的薄膜杂相较多,这不利于薄膜在辐射剂量学中的应用,因此还需要对溶胶凝胶法进行进一步的改善;丝网印刷法制备的Li_2B_4O_7薄膜,没有杂相,并能够很好的控制膜厚,由于Li_2B_4O_7熔点较高,在高温下不易分解和被氧化,因此在干燥或烧结之后也没有其它相的产生。用Cu、In元素掺杂的方法观察Li_2B_4O_7薄膜的光学性质的变化,实验结果表明,掺杂之后的Li_2B_4O_7:Cu,In薄膜与Li_2B_4O_7:Cu薄膜均存在2种吸收机制、光学禁带宽度均比未掺杂时的窄,这将有利于改善Li_2B_4O_7材料的热释光及光释光性质。光致发光实验结果表明,轻度Cu掺杂能够增大Li_2B_4O_7薄膜的发光强度,但当Cu重度掺杂的时候出现了发光淬灭;Cu、In共掺杂时,发现原先Li_2B_4O_7:Cu薄膜的发光强度随Cu浓度的增加而逐渐减弱。
Li_2B_4O_7 materials could store radiation information after being radiated. The energy is released by thermo-luminescence (TL) and optical stimulated luminescence (OSL) manners. The quantity of the energy is according to the tensity of the TL or the OSL. Moreover, the effective atomic number of the Li_2B_4O_7 material (Ze=7.26) is close to the body organizational tissue (Ze=7.13).Therefore, the material has application prospects in the intensity and the species of ray detection. Before the study of the TL and the OSL properties, it is necessary to study the luminescence properties of the Li_2B_4O_7 material. The methods of films’preparation in this work are the sol-gel method and the silk screen painting method. And the structural information of the films was obtained by the X-ray diffraction (XRD) analysis; we also studied the optical properties through optical absorption and photo- luminescence analysis. Furthermore we improved the film’s optical properties by Cu and In elements doping .The experimental results showed that there were lots of impurity phase in films prepared by sol-gel method, therefore we have to improve the experimental technique in our later works. Because the melt point of the Li_2B_4O_7 material is very high , and it is not easy to decompose and oxidize under the high temperature. The films prepared by the silk screen painting method almost have no impurity phase even after the annealing under the high temperature and the thickness of the films could be controlled better.The Cu and In elements doping experimental results showed that the optical properties changed with the different doping concentration. The results also showed there were two absorption manners for Li_2B_4O_7:Cu ,In and Li_2B_4O_7:Cu films; the forbidden band gap of Li_2B_4O_7 thin films got smaller when they were doped with Cu and In element .These results would be favorable to the TL and OSL properties. The photo- luminescence results showed that slight doping could increase the luminescence intensity, but when the doping concentration is high there was center of luminescence quenching. When doped the Li_2B_4O_7: Cu films with In element at the same time, the luminescence intensity of the Li_2B_4O_7: Cu films reduced as the Cu concentration increased.
Li_2B_4O_7 materials could store radiation information after being radiated. The energy is released by thermo-luminescence (TL) and optical stimulated luminescence (OSL) manners. The quantity of the energy is according to the tensity of the TL or the OSL. Moreover, the effective atomic number of the Li_2B_4O_7 material (Ze=7.26) is close to the body organizational tissue (Ze=7.13).Therefore, the material has application prospects in the intensity and the species of ray detection. Before the study of the TL and the OSL properties, it is necessary to study the luminescence properties of the Li_2B_4O_7 material. The methods of films’preparation in this work are the sol-gel method and the silk screen painting method. And the structural information of the films was obtained by the X-ray diffraction (XRD) analysis; we also studied the optical properties through optical absorption and photo- luminescence analysis. Furthermore we improved the film’s optical properties by Cu and In elements doping .The experimental results showed that there were lots of impurity phase in films prepared by sol-gel method, therefore we have to improve the experimental technique in our later works. Because the melt point of the Li_2B_4O_7 material is very high , and it is not easy to decompose and oxidize under the high temperature. The films prepared by the silk screen painting method almost have no impurity phase even after the annealing under the high temperature and the thickness of the films could be controlled better.The Cu and In elements doping experimental results showed that the optical properties changed with the different doping concentration. The results also showed there were two absorption manners for Li_2B_4O_7:Cu ,In and Li_2B_4O_7:Cu films; the forbidden band gap of Li_2B_4O_7 thin films got smaller when they were doped with Cu and In element .These results would be favorable to the TL and OSL properties. The photo- luminescence results showed that slight doping could increase the luminescence intensity, but when the doping concentration is high there was center of luminescence quenching. When doped the Li_2B_4O_7: Cu films with In element at the same time, the luminescence intensity of the Li_2B_4O_7: Cu films reduced as the Cu concentration increased.
引文
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[4]陈超敏,周凌宏,吕庆文.我国立体定向放射治疗设备的现状与发展.医疗卫生装备[J],2003;
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[7]张进冉均国苟立苏葆辉王兵廖晓明,新型金刚石膜辐射剂量计的研究进展,材料导报[J],2004,18(8):15;
[8]林敏崔莹李华芝陈克胜肖振红陈云东,丙氨酸/ESR剂量体系比对总结,中国原子能科学研究院年报[J],2002,36(1):116;
[9] G Gambarini, M Carrara, V Colli,Further developments and applications of layer gel dosimetry,Journal of Physics: Conference Series 3 2004:213;
[10]唐强,张纯祥热释光和光释光发光光谱的测量发光学报2006,27(3);
[11]王寿山热释光剂量学的研究、现状及发展;
[12] Ya.V.Burak Radiation-induced centers in the Li2B4O7 single crystals Nuclear Instrument and Methods in Physics Research B 191(2002) 633-637;
[13] Ya.V.Burak Optical absorption of isotopically enriched Li2B4O7 single crystals irradiated by themal neutrons Radiation Measurement 38 (2004) 681-684;
[14] Magdalyna Ignatovych Luminescence characteristics of Cu-and Eu-doped Li2B4O7 Radiation Measurement 38 (2004) 567-570;
[15] Magdalyna Ignatovych UV and electron Radiation-induced luminescence of Cu-and Eu-doped lithium tetraborates Radiation Physics Chemistry 67 (2003) 587-591;
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[18]Chen R, McKeever S W S. Theory of thermo-luminescence and related phenomena.(Singapore: World Scientific) 1997;
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[20] Chen R, Glow curves with general order kinetics, J. Electrochem. Sco: Solid Atite Sci,1969,16: 1254-1257;
[21] Randall J T, Wilkins M H F. Proc. Royl, Soc.,1945,184:366;
[22] Garlick G F, Gibson A F.Proc. , Phys. , Soc. , 1948,60:574;
[23]唐强,张纯祥等, SrSO4:Eu磷光体的光释光特性。物理学报,2005,54(1):64-69;
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[26]黄昆,韩汝琦,《固体物理学》高等教育出版社(1988)第一版,P44;
[27]王华馥,吴自勤,《固体物理实验方法》高等教育出版社(1990)第一版,P83、214;
[28]西格著,徐乐,钱建业译,《半导体物理学》人民教育出版社(1980);
[29]叶良修,《半导体物理学》下册,高等教育出版社(1987)第一版,P905;
[30]徐叙瑢,苏勉曾,《发光学与发光材料》化学工业出版社(2004)第一版,P3;
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[33].马礼敦,物理学进展, 1996, 16(2):251.
[34] Sun L., Yao J., Liu C. J. Lumin. 2000, 447, 87-89.
[1] Wen wei Ge, Huai jin Zhang , Yan ting Lin, Xiao peng Hao, Xian gang Xu, Ji yang Wang, Hong xia Li, Hong yan Xu, Min hua Jiang. Preparation of Li2B4O7 thin films by chemical solution decomposition method, Materials Letters ,61(2007) ,736-740;
[2] HIROYA YAMASHITA, TOSHINOBU YOKO AND SUMIO SAKKA. Sol-gel preparation of amorphous Li2B407 coating films, Thin Solid Films, 189 (1990) L5 LIO;
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[6] Yoldas B E, Monolithic g1ass formation by chemical polymerization, J Mat Sci·,1979( 14):1843～1849;
[7]罗伍文.用于溶胶-凝胶法的主要原料——金属醇盐.硅酸盐通报,1993(4):6O～67;
[8]李建利,董相廷,张洪波,刘景和,雷亚贵,杨魁胜.溶胶凝胶法制备Li2B4O7薄膜的研究,长春光学精密机械学院学报, 1995年6月,第18卷第2期,55-58;
[9] H.YAM ASHITA,T.YOKO,S.SAKKA,J.Mater.Sci.Lctt.1900(9):796~ 800
[10] Hiroya Yamashlta,Toshinobu Yoko, and Sumio Sakka. J.Am.Ceram.Soc,1991,74 (7):1668～1674.
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[2]胡逸民.肿瘤放射治疗物理的进展.中国医学物理学杂志[J],2002,19(4):195;
[3]蒋国梁.三维适形放疗和调强放疗.肿瘤[J],2003,(4):261;
[4]陈超敏,周凌宏,吕庆文.我国立体定向放射治疗设备的现状与发展.医疗卫生装备[J],2003;
[5]张文仲,郭勇,微剂量学的发展及其应用,辐射防护[J],2004,24(6):388;
[6]邢桂平,王树华,实用医学放射剂量学,黄河出版社,1995, P67-78页;
[7]张进冉均国苟立苏葆辉王兵廖晓明,新型金刚石膜辐射剂量计的研究进展,材料导报[J],2004,18(8):15;
[8]林敏崔莹李华芝陈克胜肖振红陈云东,丙氨酸/ESR剂量体系比对总结,中国原子能科学研究院年报[J],2002,36(1):116;
[9] G Gambarini, M Carrara, V Colli,Further developments and applications of layer gel dosimetry,Journal of Physics: Conference Series 3 2004:213;
[10]唐强,张纯祥热释光和光释光发光光谱的测量发光学报2006,27(3);
[11]王寿山热释光剂量学的研究、现状及发展;
[12] Ya.V.Burak Radiation-induced centers in the Li2B4O7 single crystals Nuclear Instrument and Methods in Physics Research B 191(2002) 633-637;
[13] Ya.V.Burak Optical absorption of isotopically enriched Li2B4O7 single crystals irradiated by themal neutrons Radiation Measurement 38 (2004) 681-684;
[14] Magdalyna Ignatovych Luminescence characteristics of Cu-and Eu-doped Li2B4O7 Radiation Measurement 38 (2004) 567-570;
[15] Magdalyna Ignatovych UV and electron Radiation-induced luminescence of Cu-and Eu-doped lithium tetraborates Radiation Physics Chemistry 67 (2003) 587-591;
[16] McKeever S W S, Moscovitch M and Townsend P D. Thermoluminesence Dosimetry Materials: Properties and Uses (Ashford, UK : Nuclear Technology Publishing).1995;
[17]田志恒,辐射剂量学,原子能出版社(北京), 1992;
[18]Chen R, McKeever S W S. Theory of thermo-luminescence and related phenomena.(Singapore: World Scientific) 1997;
[19]McKeever S W S, Chen R. Luminescence models. Radiation Measurement, 1997,27:625-611;
[20] Chen R, Glow curves with general order kinetics, J. Electrochem. Sco: Solid Atite Sci,1969,16: 1254-1257;
[21] Randall J T, Wilkins M H F. Proc. Royl, Soc.,1945,184:366;
[22] Garlick G F, Gibson A F.Proc. , Phys. , Soc. , 1948,60:574;
[23]唐强,张纯祥等, SrSO4:Eu磷光体的光释光特性。物理学报,2005,54(1):64-69;
[24] Botter Jensen L etal. Optical stimulated luminescence Dosimetry Using Nature and Synthetic Materials. Radiat Prot Dosim, 1996,65:273;
[25]马礼敦,《高等结构分析》复旦大学出版社(2002)第一版,P369、426、199;
[26]黄昆,韩汝琦,《固体物理学》高等教育出版社(1988)第一版,P44;
[27]王华馥,吴自勤,《固体物理实验方法》高等教育出版社(1990)第一版,P83、214;
[28]西格著,徐乐,钱建业译,《半导体物理学》人民教育出版社(1980);
[29]叶良修,《半导体物理学》下册,高等教育出版社(1987)第一版,P905;
[30]徐叙瑢,苏勉曾,《发光学与发光材料》化学工业出版社(2004)第一版,P3;
[31] [英]D.A.朗著《喇曼光谱学》科学出版社(1983);
[32].宋庆梅,陈暨耀,吴中亚.复旦学报, 1995, 34(1):103-106.
[33].马礼敦,物理学进展, 1996, 16(2):251.
[34] Sun L., Yao J., Liu C. J. Lumin. 2000, 447, 87-89.
[1] Wen wei Ge, Huai jin Zhang , Yan ting Lin, Xiao peng Hao, Xian gang Xu, Ji yang Wang, Hong xia Li, Hong yan Xu, Min hua Jiang. Preparation of Li2B4O7 thin films by chemical solution decomposition method, Materials Letters ,61(2007) ,736-740;
[2] HIROYA YAMASHITA, TOSHINOBU YOKO AND SUMIO SAKKA. Sol-gel preparation of amorphous Li2B407 coating films, Thin Solid Films, 189 (1990) L5 LIO;
[3]吴立军,周亚栋.Sol—Gel法制备Li2BO4薄膜,压电与声光, 1997(8),第19卷第4期,273-276;
[4]丁燕怀,苏光耀,高德淑,刘黎,王承位.溶胶凝胶法合成正极材料LiFePO4,电池, 2006年2月,第36卷第1期:52-53;
[5] Hiroga Yamashita.Preparation of Li2B4O7 thin film by sol-gel method.Joural of Material Science Letter,1990(9):96～800;
[6] Yoldas B E, Monolithic g1ass formation by chemical polymerization, J Mat Sci·,1979( 14):1843～1849;
[7]罗伍文.用于溶胶-凝胶法的主要原料——金属醇盐.硅酸盐通报,1993(4):6O～67;
[8]李建利,董相廷,张洪波,刘景和,雷亚贵,杨魁胜.溶胶凝胶法制备Li2B4O7薄膜的研究,长春光学精密机械学院学报, 1995年6月,第18卷第2期,55-58;
[9] H.YAM ASHITA,T.YOKO,S.SAKKA,J.Mater.Sci.Lctt.1900(9):796~ 800
[10] Hiroya Yamashlta,Toshinobu Yoko, and Sumio Sakka. J.Am.Ceram.Soc,1991,74 (7):1668～1674.
[1]宋强。使用印刷技术丛书——丝网印刷[M].化学工业出版社2002年12月第一版;
[2]宣大荣,韦文兰。表面组装技术[M].王德贵编著电子工业出版社,1994年8月第一版;
[3]张忠文,陈庭金,刘祖明。晶体硅太阳电池的串联电阻及其测量[Z];
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