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新型碱金属、镉/铅硼酸盐化合物的合成、结构和性能研究
周琳
学位类型硕士
导师周忠祥、潘世烈
2013-05-28
学位授予单位中国科学院大学
学位授予地点北京
学位专业材料工程
关键词非线性光学晶体 硼酸盐 碱金属 二阶姜-泰勒畸变
其他摘要

本文以新型碱金属镉硼酸盐化合物Na2Cd7B8O20 和β-LiCdBO3 以及新型碱金属铅硼酸盐LiPb2B5O10KPbB5O9 K3PbB5O10 为主要内容,开展了对其合成、结构测定以及性能测试等的研究。

1. 将具有d10 过渡金属阳离子Cd2+与硼氧功能基团相结合,合成出了一种新的化合物Na2Cd7B8O20,并解析了其晶体结构。Na2Cd7B8O20 属正交晶系,空间群为Fdd2,晶胞参数为:a = 51.5597(7) Åb = 58.6920(8) Åc = 3.381 ÅZ = 24V = 10231.4(2) Å3Na2Cd7B8O20 晶体结构是由CdOn (n = 6, 7)多面体、Na/CdOn (n = 5, 6)多面体、NaOn (n = 4, 6)多面体,以及B3O7 BO3 基团组成。测试了其红外光谱、紫外-可见-近红外漫反射光谱等物化性能。

2. 用高温固相法合成了β-LiCdBO3。β-LiCdBO3 属于单斜晶系,空间群为P21/c其晶胞参数为:a = 10.500(4) Åb = 9.073(4) Åc = 10.887(5) Å,β = 92.74(2)°,Z = 16。该晶体结构由BO3 基团、LiO4 以及CdO5 多面体组成。

3. 将具有孤对电子的金属阳离子Pb2+与硼氧基团相结合,在Li2O-PbO-B2O3 元体系中生长出了一种铅硼酸盐晶体LiPb2B5O10,用高温固相烧结法得到了该化合物的纯相。该晶体属于单斜晶系,空间群为P21/m,晶胞参数为:a =4.4023(10) Åb = 14.037(3) Åc = 6.8846(16) Å,β = 107.408(2)°,Z = 2。该晶体结构是由B5O10 基团、LiO4 以及PbO7 多面体组成的。PbO7 多面体通过共边和共顶点形成三维网络结构,B5O10 基团通过共顶点与该三维网络结构相连接,Li 离子填充在这个网络结构中。测试了其红外光谱、紫外-可见-红外漫反射光谱等物化性能。

4. KPbB5O9 晶体属单斜晶系,空间群为P21/c,晶胞参数为:a = 6.717(3) Åb =8.389(3) Åc = 13.686(5) Å,β = 94.679(4)°,Z = 4。该晶体结构由B5O9 基团、KO8 以及PbO6 多面体组成。PbO6 多面体通过共顶点O 原子形成沿b 方向上的∞[PbO6]长链,而长链之间通过二聚物[K2O14]相连接。测试并分析了化合物KPbB5O9 的红外光谱、紫外-可见-近红外漫反射光谱以及热学性质。

5. K3PbB5O10 属于正交晶系,空间群为Cmca,晶胞参数为:a = 9.444(10) Åb= 13.380(14) Åc = 17.530(19) ÅZ = 8K3PbB5O10 晶体结构是由B5O10 基团、PbO4 以及KO8 多面体组成。B5O10 基团与PbO4 四面体形成∞[PbB5O10]层,层与层之间通过K 原子连接。

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In this thesis alkali metal cadmium borate compounds, Na2Cd7B8O20 and β-LiCdBO3, and novel alkali lead borate compounds, LiPb2B5O10, KPbB5O9 and K3PbB5O10, were studied. The major work consist of their synthesis, crystal structure determination and measurements of properties. Combined d10 cation Cd2+ with borate, a new noncentrosymmetric compound, Na2Cd7B8O20, has been synthesized by solid-state reaction.The compound crystallizes in the orthorhombic space group Fdd2 with a = 51.5597(7) ?, b = 58.6920(8) ? and c = 3.381 ?. The crystal structure is composed of CdOn (n = 6, 7), Na/CdOn (n = 5, 6) and NaOn (n = 4, 6) polyhedra, B3O7 and BO3 units. The IR spectrum, the UV-vis-NIR diffuse reflectance spectrum and other properties have been measured. β-LiCdBO3 has been obtained by the high solid-state reaction method. The compound crystallizes in the monoclinic space group P21/c with a = 10.500(4) ?, b = 9.073(4) ?, c = 10.887(5) ?, β = 92.74(2)°, and Z = 16. The structure consists of BO3 units, LiO4 and CdO5 polyhedra. Mixing lead atom and borate systems, a new compound LiPb2B5O10 has been obtained by the high temperature solution method in the Li2O-PbO-B2O3 ternary system. It crystallizes in the monoclinic space group P21/m with lattice constants a = 4.4023(10) ?, b = 14.037(3) ?, c = 6.8846(16) ?, β = 107.408(2)° and Z = 2. The structure consists of B5O10 units, LiO4 and PbO7 polyhedra. The PbO7 polyhedra are interconnected by shared corners or edges to form the three-dimensional framework, and the B5O10 units connected with PbO7 polyhedra via corner O atoms. The Li atoms are located between the B5O10 and PbO7 groups to hold the groups through coordination with oxygen atoms. The IR spectrum, the UV-vis-NIR diffuse reflectance spectrum and other properties have been measured. KPbB5O9 crystallizes in the monoclinic space group P21/c with lattice constants a = 6.717(3) ?, b = 8.389(3) ?, c = 13.686(5) ?, β = 94.679(4)° and Z = 4. The structure consists of B5O9 units, KO8 and PbO6 polyhedra. The PbO6 polyhedra linked together via corner-sharing O atom forming novel infinite ∞[PbO6] chains along the b axis, the [K2O14] dimers distributed between the ∞[PbO6] chains and interconnected by sharing edges. The IR spectrum, the optical diffuse reflectance spectrum and other properties of KPbB5O9 have been studied. K3PbB5O10 crystallizes in the space group Cmca of the orthorhombic system with a = 9.444(10) ?, b = 13.380(14) ?, c = 17.530(19) ?, and Z = 8. The structure consists of B5O10 units, PbO4 and KO8 polyhedra. The B5O10 groups and PbO4 polyhedra are connected to form ∞[PbB5O10] layer, and K atoms are located between these layers to balance charge and also to hold the layer together through coordination with oxygen atoms.

文献类型学位论文
条目标识符http://ir.xjipc.cas.cn/handle/365002/2464
专题材料物理与化学研究室
作者单位中国科学院新疆理化技术研究所
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周琳. 新型碱金属、镉/铅硼酸盐化合物的合成、结构和性能研究[D]. 北京. 中国科学院大学,2013.
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