TSB溶液的回流热处理与晶体生长
|
摘要
首先对反式二苯乙烯(TSB)的环己酮溶液进行回流热处理,考察不同回流加热时间对TSB溶液饱和点的影响,以高效液相色谱(HPLC)及气质联用技术(GC-MS)检测与分析回流加热过程中溶液的成分,随后采用降温法在该溶液中进行晶体生长,并观测了所生长TSB晶体的完整性。结果表明:环己酮是适合生长TSB晶体的溶剂,对溶液进行适当的回流热处理虽然会产生少量杂质,但在一定程度上能够加快溶剂合反应平衡并提高溶液稳定性,同时,晶体的完整性和闪烁性能也有所改善。
Trans-stilbene(TSB) solutions were treated via reflux heating with cyclohexanone as a solvent. The effect of reflux heating time on the saturation temperature of the solution was investigated, and the compositions of the heated solutions were analyzed by high-performance liquid chromatography(HPLC) and gas chromatography-mass spectrometry(GC-MS). The crystals were grown in the solutions by a slow-cooling method. The results show that cyclohexanone is an effective solvent for the growth of TSB crystals, and the proper heat treatment of reflux to the solution can accelerate the equilibrium of solvating reaction and improve the stability of the solution in a certain degree. Also, the perfection and scintillation property of the crystals improve although a small amount of impurities appear in the reflux period.
Trans-stilbene(TSB) solutions were treated via reflux heating with cyclohexanone as a solvent. The effect of reflux heating time on the saturation temperature of the solution was investigated, and the compositions of the heated solutions were analyzed by high-performance liquid chromatography(HPLC) and gas chromatography-mass spectrometry(GC-MS). The crystals were grown in the solutions by a slow-cooling method. The results show that cyclohexanone is an effective solvent for the growth of TSB crystals, and the proper heat treatment of reflux to the solution can accelerate the equilibrium of solvating reaction and improve the stability of the solution in a certain degree. Also, the perfection and scintillation property of the crystals improve although a small amount of impurities appear in the reflux period.
引文
[1]张明荣,葛云程.无机闪烁晶体及其产业化开发[J].新材料产业,2002(3):15?19.ZHANG Mingrong, GE Yuncheng. Adv Mater Ind(in Chinese),2002(3):15?19.
[2]张杰.中国散裂中子源(CSNS)——多学科应用的大科学平台[J].中国科学院院刊, 2006, 21(5):415?417.ZHANG Jie. Bull Chin Acad Sci(in Chinese), 2006, 21(5):415?417.
[3]杨帆,任国浩.中子探测用闪烁体的研究进展[J].核电子学与探测技术, 2009, 29(4):895?901.YANG Fan, REN Guohao. Nucl Electron Detect. Technol(in Chinese),2009, 29(4):895?901.
[4]刘波,施朝淑.医用闪烁体进展[J].科学通报, 2002(1):1?9.LIU Bo, SHI Chaoshu. Chin Sci Bull(in Chinese), 2002(1):1?9.
[5]汲长松.中子探测[M].北京:中国原子能出版, 2014:126?151.
[6]丁大钊,叶春堂,赵志祥.中子物理学原理,方法与应用(上册)[M].北京:原子能出版社, 2005:92?118..
[7]杨帆,任国浩.中子探测用闪烁体的研究进展[J].核电子学与探测技术, 2009, 29(4):895?901.YANG Fan, REN Guohao. Nucl Electron Detect. Technol(in Chinese),2009, 29(4):895?901.
[8] HOEKSTRA A, MEERTENS P, VOS A. Refinement of the crystal structure of trans-stilbene(TSB). The molecular structure in the crystalline and gaseous phases[J]. Acta Crystallogr B:Struct Crystallography Cryst Chem, 1975, 31(12):2813?2817.
[9] LEININGER R F. On the preparation of stilbene crystals[J]. Rev Sci Instrum, 1952, 23(3):127?128.
[10] ZAITSEVA N, GLENN A, CARMAN L, et al. Scintillation properties of solution-grown trans-stilbene single crystals[J]. Nucl Instrum Methods Phys Res A, 2015, 789:8?15.
[11]俞嗣皎,申敬廉,唐祖梅.有机闪烁体—芪晶体制备[J].核电子学与探测技术, 1984(1):25?29+34.YU Sihao, SHEN Jinglian, TANG Zumei. Nucl Electron Detect.Technol(in Chinese), 1984(1):25?29+34.
[12] ARULCHAKKARAVARTHI A, SANTHANARAGHAVAN P,RAMASAMY P. Crystal growth of trans-stilbene by vertical bridgman technique with modified growth vessels and its characterization[J]. J Cryst Growth, 2001, 224(1/2):89?94.
[13] ARULCHAKKARAVARTHI A, SANTHANARAGHAVAN P,RAMASAMY P. Studies on microhardness and slip systems of Bridgman grown trans-stilbene crystals[J]. Mater Lett, 2001, 51(2):151?155.
[14] ZENG FANBO, LUO DONGMEI, ZHANG ZHAO, et al. Study on the behavior of sulfur in hydrolysis process of titanyl sulfate solution[J]. J Alloy Compd, 2016, 670:249?257.
[15] ZAITSEVA N P, NEWBY J, HAMEL S, et al. Neutron detection with single crystal organic scintillators[J]. Int Soc Opt Photonics, 2009,7449:744911?744920.
[16] ARULCHAKKARAVARTHI A, JAYAVEL P, SANTHANARAGHAVAN P,et al. Growth of organic molecular single crystal trans-stilbene by selective self seeding from vertical bridgman technique[J]. J Cryst Growth, 2002, 234(1):159?163.
[17] ZAITSEVA N, GLENN A, CARMAN L, et al. Scintillation properties of solution-grown Trans-stilbene single crystals[J]. Nucl Instrum Methods Phys Res Sect A, 2015, 789:8?15.
[18]任继齐,常新安,陈学安,等.反式二苯乙烯(TSB)的溶液法晶体生长[J].人工晶体学报, 2017, 46(3):404?409.REN Jiqi, CHANG Xinan, CHEN Xuean, et al. J Synth Cryst(in Chinese), 2017, 46(3):404?409.
[19]王淑君,常新安,陈学安,等.不同溶剂中TSB晶体的生长与形貌分析[J].硅酸盐学报, 2018, 46(7):957?963.WANG Shujun, CHANG Xinan, CHEN Xuean, et al. J Chin Ceram Soc, 2018, 46(7):957?963.
[2]张杰.中国散裂中子源(CSNS)——多学科应用的大科学平台[J].中国科学院院刊, 2006, 21(5):415?417.ZHANG Jie. Bull Chin Acad Sci(in Chinese), 2006, 21(5):415?417.
[3]杨帆,任国浩.中子探测用闪烁体的研究进展[J].核电子学与探测技术, 2009, 29(4):895?901.YANG Fan, REN Guohao. Nucl Electron Detect. Technol(in Chinese),2009, 29(4):895?901.
[4]刘波,施朝淑.医用闪烁体进展[J].科学通报, 2002(1):1?9.LIU Bo, SHI Chaoshu. Chin Sci Bull(in Chinese), 2002(1):1?9.
[5]汲长松.中子探测[M].北京:中国原子能出版, 2014:126?151.
[6]丁大钊,叶春堂,赵志祥.中子物理学原理,方法与应用(上册)[M].北京:原子能出版社, 2005:92?118..
[7]杨帆,任国浩.中子探测用闪烁体的研究进展[J].核电子学与探测技术, 2009, 29(4):895?901.YANG Fan, REN Guohao. Nucl Electron Detect. Technol(in Chinese),2009, 29(4):895?901.
[8] HOEKSTRA A, MEERTENS P, VOS A. Refinement of the crystal structure of trans-stilbene(TSB). The molecular structure in the crystalline and gaseous phases[J]. Acta Crystallogr B:Struct Crystallography Cryst Chem, 1975, 31(12):2813?2817.
[9] LEININGER R F. On the preparation of stilbene crystals[J]. Rev Sci Instrum, 1952, 23(3):127?128.
[10] ZAITSEVA N, GLENN A, CARMAN L, et al. Scintillation properties of solution-grown trans-stilbene single crystals[J]. Nucl Instrum Methods Phys Res A, 2015, 789:8?15.
[11]俞嗣皎,申敬廉,唐祖梅.有机闪烁体—芪晶体制备[J].核电子学与探测技术, 1984(1):25?29+34.YU Sihao, SHEN Jinglian, TANG Zumei. Nucl Electron Detect.Technol(in Chinese), 1984(1):25?29+34.
[12] ARULCHAKKARAVARTHI A, SANTHANARAGHAVAN P,RAMASAMY P. Crystal growth of trans-stilbene by vertical bridgman technique with modified growth vessels and its characterization[J]. J Cryst Growth, 2001, 224(1/2):89?94.
[13] ARULCHAKKARAVARTHI A, SANTHANARAGHAVAN P,RAMASAMY P. Studies on microhardness and slip systems of Bridgman grown trans-stilbene crystals[J]. Mater Lett, 2001, 51(2):151?155.
[14] ZENG FANBO, LUO DONGMEI, ZHANG ZHAO, et al. Study on the behavior of sulfur in hydrolysis process of titanyl sulfate solution[J]. J Alloy Compd, 2016, 670:249?257.
[15] ZAITSEVA N P, NEWBY J, HAMEL S, et al. Neutron detection with single crystal organic scintillators[J]. Int Soc Opt Photonics, 2009,7449:744911?744920.
[16] ARULCHAKKARAVARTHI A, JAYAVEL P, SANTHANARAGHAVAN P,et al. Growth of organic molecular single crystal trans-stilbene by selective self seeding from vertical bridgman technique[J]. J Cryst Growth, 2002, 234(1):159?163.
[17] ZAITSEVA N, GLENN A, CARMAN L, et al. Scintillation properties of solution-grown Trans-stilbene single crystals[J]. Nucl Instrum Methods Phys Res Sect A, 2015, 789:8?15.
[18]任继齐,常新安,陈学安,等.反式二苯乙烯(TSB)的溶液法晶体生长[J].人工晶体学报, 2017, 46(3):404?409.REN Jiqi, CHANG Xinan, CHEN Xuean, et al. J Synth Cryst(in Chinese), 2017, 46(3):404?409.
[19]王淑君,常新安,陈学安,等.不同溶剂中TSB晶体的生长与形貌分析[J].硅酸盐学报, 2018, 46(7):957?963.WANG Shujun, CHANG Xinan, CHEN Xuean, et al. J Chin Ceram Soc, 2018, 46(7):957?963.