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新型碱金属硼酸盐的熔盐合成与结构表征 本研究利用硼酸熔融法合成两种新型碱金属硼酸盐,并利用溶液法合成了一种有机化合物,其中重点介绍硼酸熔融法及其利用该法合成的硼酸盐化合物。与水热法相比,硼酸熔融法工艺简单,易于引进硼原子。所有化合物均以单晶衍射仪收集数据并进行结构解析,两种硼酸盐通过粉晶衍射、红外光谱、热重等对该化合物进行了表征。 本论文所合成的三种化合物如下: (1) NaZnB3P2O10(OH)2•1.17H2O (2) RbB5O7(OH)2•H2O (3) C16H10O8•H2O 硼磷酸盐NaZnB3P2O10(OH)2•1.17H2O属于六方晶系,P6(3)/m空间群,晶胞参数a=1.17272(3)nm,c=1.21317(6)nm, γ=120°, V=1.44491(10) nm3 , Z=6,R1=0.0679, wR2=0.1566 。该化合物是一种具有十二元环和六元环两种孔道的新型三维结构。 五硼酸盐RbB5O7(OH)2•H2O属于单斜晶系,P2/n空间群,晶胞参数a=0.7640(2)nm,b=0.9019(3)nm,c=1.0833(3)nm,β=103.681(5)°,V=0.7252(4) nm3,Z=2,Rl=0.0737,wR2=0.1588。结构中的硼氧聚阴离子[B5O7(OH)2]-单元通过氧原子与相临的[B5O7(OH)2]-单元相连接形成无限的链状结构,链状结构通过氧原子与Rb+离子相连接形成三维的手性结构。 晶体C16H10O8•H2O属于三斜晶系,P1空间群,晶胞参数a=0.71765(1)nm,b=0.94677 (2)nm,c=1.19301(2)nm,α=,106.013(1)°,β=100.098(1)°,γ=96.753(1)°,V=0.75518(2) nm3,Z=2。晶体结构中两个苯环的二面角为71.63(2)°。 本文的所用的硼酸熔融法工艺简单、易于引进硼原子,已经成功应用于合成锂电池阴极材料上,文中所得具有巨环结构、手性结构的硼酸盐化合物也为硼酸盐材料增添了新的血液,为开发更多具有特殊功能的新材料奠定坚实的基础。 关键词:硼酸熔融法;硼磷酸盐;巨环结构;五硼酸盐;手性结构; |
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2楼2012-03-24 15:17:47
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3楼2012-03-24 15:19:02
xiaohanhan2007
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【答案】应助回帖
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Mally89: 金币+1, 感谢应助!~ 2012-03-26 22:19:50
Mally89: 金币+1, 感谢应助!~ 2012-03-26 22:19:50
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Syntheses and structural characterizations of novel molten alkali metal borates In this study, two novel alkali metal borates were synthesized by the borate fusion method, and an organic compound was synthesized by the solution method, in which the borate fusion method and the resulting borate compounds were emphasized. Compared to the hydrothermal method, borate fusion method is simpler and is able to introduce boron atoms more easily. All the structural data of the compounds were collected by a single crystal diffractometer and then analyzed. Both of the two borates were characterized by X-ray powder diffraction, IR and TGA. The three compounds synthesized in this paper include: (1) NaZnB3P2O10(OH)2•1.17H2O (2) RbB5O7(OH)2•H2O (3) C16H10O8•H2O Borophosphate NaZnB3P2O10 (OH) 2 • 1.17H2O belongs to hexagonal crystal system and P6(3)/m space group. Its unit cell parameters include a = 1.17272 (3) nm, c = 1.21317 (6) nm, γ = 120 °, V = 1.44491 nm3, Z = 6, R1 = 0.0679 and wR2 = 0.1566. The compound is a novel three-dimensional structure consisting of both 12-membered-ring and six-membered-ring pores. Pentaborate RbB5O7 (OH) 2 • H2O belongs to the monoclinic crystal system and P2/n space group. Its unit cell parameters include a=0.7640(2)nm, b=0.9019(3)nm, c=1.0833(3)nm, β=103.681(5)°, V=0.7252(4) nm3, Z=2, R1=0.0737 and wR2=0.1588. Boron-oxygen polyanion unit [B5O7(OH)2]- is connected with the adjacent unit [B5O7(OH)2]- by O atoms that form infinite chains, which are further connected by O atoms and Rb+ ions that form a three-dimensional chiral structure. C16H10O8•H2O belongs to the triclinic crystal system and P1 space group. Its cell parameters include a=0.71765(1)nm, b=0.94677 (2)nm, c=1.19301(2)nm, α=,106.013(1)°, β=100.098(1)°, γ=96.753(1)°, V=0.75518(2) nm3, Z=2.Dihedral angle between the two benzene rings is 71.63(2)°. Borate fusion method used herein is easily handling and is able to introduce boron atoms readily, which has been successfully applied in the syntheses of lithium battery cathode materials. Borates that are of macro-ring and chiral structures prepared in this paper will facilitate the innovation of borate materials and lay a solid foundation for the development of more novel materials with special functions. |
4楼2012-03-24 15:55:54
budong0915
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5楼2012-03-24 16:10:06
xiaohanhan2007
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6楼2012-03-24 16:51:33













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