新型紫外、深紫外非线光学晶体氯硼酸钾、氟硼酸钡的合成、生长及性能研究
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摘要
本论文主要在K_2O-KCl-B_2O_3和BaO-BaF_2-B_2O_3体系中合成出两种具有应用前景的新型紫外非线性光学晶体材料卤素硼酸盐K_3B_6O_(10)Cl (KBOC)和Ba_4B_(11)O_(20)F(BBOF)，KBOC和BBOF的紫外截止边都达到了深紫外区，BBOF粉末倍频效应达10倍KDP。采用顶部籽晶法生长出了大尺寸的晶体对其性能进行了测试；在探索新型紫外非线性光学晶体材料过程中，发现了四种结构新颖的硼酸盐化合物；另外，使用室温溶液法得到了两种新型有机-无机杂化的硼酸盐化合物。主要工作及结果如下：
1.新型紫外非线性光学晶体KBOC的研究
在硼氧框架中引入碱金属阳离子和卤素离子以提高其性能的设计思想指导下，首次获得一种新型的碱金属卤素硼酸盐（KBOC）。其中，选择硼氧功能基元为阴离子，其带隙较大，双光子吸收概率小，激光损伤阈值较高；B-O键利于宽波段光透过；阳离子选择无d~0电子跃迁的碱金属离子，有利于紫外光透过；同时卤素离子的引入也将拓宽其透光范围；在结构上，选择类钙钛矿结构，有助于产生大的非线性光学效应。
非线性光学性能测试表明，KBOC粉末倍频效应约为3倍KDP，可实现相位匹配。分析发现，KBOC化合物的非线性光学效应主要来源于畸变的ClK_6多面体及B_6O_(10)基团。
通过TG-DSC测试表明KBOC为非同成分熔融化合物。通过助熔剂探索，生长出25mm×11mm×7mm高质量单晶。测量了KBOC晶体的透光范围，采用最小偏向角法对KBOC晶体折射率进行了测量，计算出KBOC晶体的相位匹配区间，证实了在1064nm基频光下，可以实现I类、II类相位匹配。KBOC晶体的I类相匹配最短倍频波长为255nm。
KBOC晶体的激光损伤阈值实验表明：其激光损伤阈值大于9.2GW/cm~2。晶体的热膨胀系数沿a和c方向分别为3.08×10~(-6)和28.4×10~(-6)K~(-1)。硬度测试表明，KBOC晶体的莫氏硬度约为4-5Mohs，物化性能稳定。
2.新型紫外非线性光学晶体BBOF的研究
将无d-d电子跃迁的金属阳离子基元和利于紫外光透过的氟离子与硼氧功能基元结合，首次设计、合成出新型紫外非线性光学晶体BBOF。
利用高温熔液法获得小尺寸BBOF晶体。单晶结构解析表明，BBOF晶体属正交晶系，空间群为Cmc21，晶胞参数为：a=18.8112(15)，b=10.7151(6)，c=8.6031(5)，Z=4，V=1734.1(2)3。BBOF晶体结构是由新的硼氧功能基元B11O24通过氧原子连接形成一个沿c方向的孔道，Ba(1)-F(1)-Ba(2)链填充于孔道中，Ba(3)原子位于孔道周围对称的位置上。
非线性光学性能测试表明，BBOF粉末倍频效应约为10倍KDP，可实现相位匹配。采用顶部籽晶法生长出BBOF晶体，BBOF晶体透过光谱测试表明其紫外截止边约为190nm。硬度测试表明，BBOF晶体的硬度约5Mohs。潮解性能实验表明，BBOF晶体不吸潮，在水中和空气中都很稳定。
3.四种新型硼酸盐化合物的研究
发现了四种新型硼酸盐化合物：K_3ZnB_5O_(10)、Pb_xBa_(9-x)B_(18)O_(36)、K_3B_3O_3F_6和CsB_5O_8，解析其单晶结构，测试其光学和热学性能。其中，K3ZnB5O10为同成分熔融化合物。Pb_xBa_(9-x)B_(18)O_(36)晶体结构中含有B_3O_6功能基元，与β-BaB_2O_4结构比较：B_3O_6功能基元的排列方式对材料的倍频效应有较大影响。在K_3B_3O_3F_6化合物中，B和F的成键在常压下比较少。CsB_5O_8晶体属正交晶系，空间群为Pccn，基本功能基元为B_(10)O_(22)，它与文献报道的α-CsB_5O_8、β-CsB_5O_8和γ-CsB_5O_8结构不同，其差异主要是由基本功能基元不同引起的。
4.两种新型有机-无机杂化硼酸盐的研究
通过室温溶液法合成了两种有机-无机杂化硼酸盐晶体Sr[B(C_6H_5O_7)_2](H_2O)_43H_2O和Ca[B(C_6H_6O_7)_2](H_2O)_4HCl，反应原料的初始摩尔比和溶液的pH值对生长这两种晶体起着重要的作用。解析了晶体结构，测试了红外、透过光谱，分析了其热性能及元素组成。
Two new halogen complex borates, K_3B_6O_(10)Cl (KBOC) and Ba_4B_(11)O_(20)F (BBOF)have been found in the K_2O-KCl-B_2O_3and BaO-BaF_2-B_2O_3systems. The large singlecrystals have been grown by the top-seeded solution growth method and some propertieshave been characterized. In addition, other four novel borates and two organic-inorganichybrid borates have been synthesized by the high-temperature solution method and theslow evaporation of water solution at room temperature, respectively. The dissertationmainly consists of the discussions about their solid-state synthesis, crystal structuredetermination, crystal growth and measurement of properties.
1. Research on UV nonlinear optical KBOC crystal
Pure phase of KBOC compound was synthesized by the solid-state reaction for thefirst time. The crystal structure of KBOC was determined by the single crystal X-raydiffraction. KBOC crystallizes in the rhombohedral system, space group R3m with unit-cellparameters a=10.0624(14), c=8.8361(18), Z=4, V=774.8(2)3. The structureexhibits an intricate3-dimensional (3D) network composed of [B_6O_(10)] units and [ClK_6]octahedra and can also be described as two networks (a [B_6O_(10)]∞and a ReO_3-type ClK_6network) that are interweaved.
As-prepared KBOC has a powder second harmonic generation (SHG) effect aboutthree times that of KDP and is phase matchable as supported by powder SHGmeasurements. The large SHG response arises from the distortions of [B_6O_(10)] and ClK_6groups.
The TG-DSC analysis proves that KBOC is an incongruently melting compound. Ahigh quality single crystal of KBOC with dimensions up to25mm×11mm×7mm wassuccessfully grown by the top-seeded solution growth method for the first time. By theminimum deviation technique, the refractive indices of the crystal were measured andfitted to the Sellmeier equations. The limit of type-I phase matching SHG wavelength wascalculated to be255nm. The transmittance spectrum shows that the as-grown crystal is transparent in the wavelength range of180-3460nm. The thermal properties and laserdamage threshold have been investigated. The two principal coefficients of thermalexpansion along a and c axes were measured to be3.08×10~(-6)and28.4×10~(-6)K~(-1),respectively. The optical damage threshold was estimated, which is more than9.2GW/cm~2.
The measured hardness of the KBOC crystal is approximately4-5Mohs.Experiments demonstrate that the KBOC crystal is nonhygroscopic, very stable in water orair.
2. Research on UV nonlinear optical BBOF crystal
Pure phase of BBOF was synthesized by the solid-state reaction for the first time. Thecrystal structure of BBOF was investigated. It crystallizes in the orthorhombic system,space group Cmc21with unit-cell parameters a=18.8112(15), b=10.7151(6), c=8.6031(5), Z=4, V=1734.1(2)3. BBOF has a3D network structure, in which a newFunction Building Block (FBB) B11O24was observed. The FBBs are connected with eachother by sharing O atoms to form3D network with tunnels viewing along c axis, whereBa(1)-F(1)-Ba(2) chains are filled, and the Ba(3) atoms are located at symmetrical site inthe periphery of the tunnel.
The SHG measurement suggests that BBOF has a powder SHG effect about10timesthat of KDP and is phase matchable.
The TG-DSC experiment proves that BBOF melts incongruently. BBOF single crystalhas been grown by the high temperature solution method. The UV-vis-NIR transmittancespectrum of the BBOF crystal was measured, and the UV cutoff edge is about190nm. Themeasured hardness of the BBOF crystal is approximately5Mohs.
3. Research on four new borate compounds
Four compounds, K_3ZnB_5O_(10), Pb_xBa_(9-x)B_(18)O_(36), K_3B_3O_3F_6and CsB_5O_8, have beenfound to crystallize in new structure types. Some properties of the compounds are reported.The DSC experiments prove that K_3ZnB_5O_(10)melts congruently. In Pb_xBa_(9-x)B_(18)O_(36), the FBB is B_3O_6group. By comparing the structures of Pb_xBa_(9-x)B_(18)O_(36)with that of β-BaB_2O_4,it is found that the arrangement of B_3O_6groups in the compounds leads to different SHGeffect. In K_3B_3O_3F_6, the FBB is B_3O_3F_6, but scarcely see the linkage of B-F under ambientpressure. CsB_5O_8crystallizes in the orthorhombic space group Pccn. By comparing thestructures of CsB_5O_8with that of α-CsB_5O_8, β-CsB_5O_8andγ-CsB_5O_8, it is found that thedifference of FBB among the compounds leads to crystallize in different space groups.
4. Research on two organic-inorganic hybrid borate compounds
Sr[B(C_6H_5O_7)_2](H_2O)_43H_2O and Ca[B(C_6H_6O_7)_2](H_2O)_4HCl have been synthesizedby the slow evaporation of water solution at room temperature. Their crystal structureswere established by single-crystal X-ray diffraction and optical properties were measured.
1.新型紫外非线性光学晶体KBOC的研究
在硼氧框架中引入碱金属阳离子和卤素离子以提高其性能的设计思想指导下，首次获得一种新型的碱金属卤素硼酸盐（KBOC）。其中，选择硼氧功能基元为阴离子，其带隙较大，双光子吸收概率小，激光损伤阈值较高；B-O键利于宽波段光透过；阳离子选择无d~0电子跃迁的碱金属离子，有利于紫外光透过；同时卤素离子的引入也将拓宽其透光范围；在结构上，选择类钙钛矿结构，有助于产生大的非线性光学效应。
非线性光学性能测试表明，KBOC粉末倍频效应约为3倍KDP，可实现相位匹配。分析发现，KBOC化合物的非线性光学效应主要来源于畸变的ClK_6多面体及B_6O_(10)基团。
通过TG-DSC测试表明KBOC为非同成分熔融化合物。通过助熔剂探索，生长出25mm×11mm×7mm高质量单晶。测量了KBOC晶体的透光范围，采用最小偏向角法对KBOC晶体折射率进行了测量，计算出KBOC晶体的相位匹配区间，证实了在1064nm基频光下，可以实现I类、II类相位匹配。KBOC晶体的I类相匹配最短倍频波长为255nm。
KBOC晶体的激光损伤阈值实验表明：其激光损伤阈值大于9.2GW/cm~2。晶体的热膨胀系数沿a和c方向分别为3.08×10~(-6)和28.4×10~(-6)K~(-1)。硬度测试表明，KBOC晶体的莫氏硬度约为4-5Mohs，物化性能稳定。
2.新型紫外非线性光学晶体BBOF的研究
将无d-d电子跃迁的金属阳离子基元和利于紫外光透过的氟离子与硼氧功能基元结合，首次设计、合成出新型紫外非线性光学晶体BBOF。
利用高温熔液法获得小尺寸BBOF晶体。单晶结构解析表明，BBOF晶体属正交晶系，空间群为Cmc21，晶胞参数为：a=18.8112(15)，b=10.7151(6)，c=8.6031(5)，Z=4，V=1734.1(2)3。BBOF晶体结构是由新的硼氧功能基元B11O24通过氧原子连接形成一个沿c方向的孔道，Ba(1)-F(1)-Ba(2)链填充于孔道中，Ba(3)原子位于孔道周围对称的位置上。
非线性光学性能测试表明，BBOF粉末倍频效应约为10倍KDP，可实现相位匹配。采用顶部籽晶法生长出BBOF晶体，BBOF晶体透过光谱测试表明其紫外截止边约为190nm。硬度测试表明，BBOF晶体的硬度约5Mohs。潮解性能实验表明，BBOF晶体不吸潮，在水中和空气中都很稳定。
3.四种新型硼酸盐化合物的研究
发现了四种新型硼酸盐化合物：K_3ZnB_5O_(10)、Pb_xBa_(9-x)B_(18)O_(36)、K_3B_3O_3F_6和CsB_5O_8，解析其单晶结构，测试其光学和热学性能。其中，K3ZnB5O10为同成分熔融化合物。Pb_xBa_(9-x)B_(18)O_(36)晶体结构中含有B_3O_6功能基元，与β-BaB_2O_4结构比较：B_3O_6功能基元的排列方式对材料的倍频效应有较大影响。在K_3B_3O_3F_6化合物中，B和F的成键在常压下比较少。CsB_5O_8晶体属正交晶系，空间群为Pccn，基本功能基元为B_(10)O_(22)，它与文献报道的α-CsB_5O_8、β-CsB_5O_8和γ-CsB_5O_8结构不同，其差异主要是由基本功能基元不同引起的。
4.两种新型有机-无机杂化硼酸盐的研究
通过室温溶液法合成了两种有机-无机杂化硼酸盐晶体Sr[B(C_6H_5O_7)_2](H_2O)_43H_2O和Ca[B(C_6H_6O_7)_2](H_2O)_4HCl，反应原料的初始摩尔比和溶液的pH值对生长这两种晶体起着重要的作用。解析了晶体结构，测试了红外、透过光谱，分析了其热性能及元素组成。
Two new halogen complex borates, K_3B_6O_(10)Cl (KBOC) and Ba_4B_(11)O_(20)F (BBOF)have been found in the K_2O-KCl-B_2O_3and BaO-BaF_2-B_2O_3systems. The large singlecrystals have been grown by the top-seeded solution growth method and some propertieshave been characterized. In addition, other four novel borates and two organic-inorganichybrid borates have been synthesized by the high-temperature solution method and theslow evaporation of water solution at room temperature, respectively. The dissertationmainly consists of the discussions about their solid-state synthesis, crystal structuredetermination, crystal growth and measurement of properties.
1. Research on UV nonlinear optical KBOC crystal
Pure phase of KBOC compound was synthesized by the solid-state reaction for thefirst time. The crystal structure of KBOC was determined by the single crystal X-raydiffraction. KBOC crystallizes in the rhombohedral system, space group R3m with unit-cellparameters a=10.0624(14), c=8.8361(18), Z=4, V=774.8(2)3. The structureexhibits an intricate3-dimensional (3D) network composed of [B_6O_(10)] units and [ClK_6]octahedra and can also be described as two networks (a [B_6O_(10)]∞and a ReO_3-type ClK_6network) that are interweaved.
As-prepared KBOC has a powder second harmonic generation (SHG) effect aboutthree times that of KDP and is phase matchable as supported by powder SHGmeasurements. The large SHG response arises from the distortions of [B_6O_(10)] and ClK_6groups.
The TG-DSC analysis proves that KBOC is an incongruently melting compound. Ahigh quality single crystal of KBOC with dimensions up to25mm×11mm×7mm wassuccessfully grown by the top-seeded solution growth method for the first time. By theminimum deviation technique, the refractive indices of the crystal were measured andfitted to the Sellmeier equations. The limit of type-I phase matching SHG wavelength wascalculated to be255nm. The transmittance spectrum shows that the as-grown crystal is transparent in the wavelength range of180-3460nm. The thermal properties and laserdamage threshold have been investigated. The two principal coefficients of thermalexpansion along a and c axes were measured to be3.08×10~(-6)and28.4×10~(-6)K~(-1),respectively. The optical damage threshold was estimated, which is more than9.2GW/cm~2.
The measured hardness of the KBOC crystal is approximately4-5Mohs.Experiments demonstrate that the KBOC crystal is nonhygroscopic, very stable in water orair.
2. Research on UV nonlinear optical BBOF crystal
Pure phase of BBOF was synthesized by the solid-state reaction for the first time. Thecrystal structure of BBOF was investigated. It crystallizes in the orthorhombic system,space group Cmc21with unit-cell parameters a=18.8112(15), b=10.7151(6), c=8.6031(5), Z=4, V=1734.1(2)3. BBOF has a3D network structure, in which a newFunction Building Block (FBB) B11O24was observed. The FBBs are connected with eachother by sharing O atoms to form3D network with tunnels viewing along c axis, whereBa(1)-F(1)-Ba(2) chains are filled, and the Ba(3) atoms are located at symmetrical site inthe periphery of the tunnel.
The SHG measurement suggests that BBOF has a powder SHG effect about10timesthat of KDP and is phase matchable.
The TG-DSC experiment proves that BBOF melts incongruently. BBOF single crystalhas been grown by the high temperature solution method. The UV-vis-NIR transmittancespectrum of the BBOF crystal was measured, and the UV cutoff edge is about190nm. Themeasured hardness of the BBOF crystal is approximately5Mohs.
3. Research on four new borate compounds
Four compounds, K_3ZnB_5O_(10), Pb_xBa_(9-x)B_(18)O_(36), K_3B_3O_3F_6and CsB_5O_8, have beenfound to crystallize in new structure types. Some properties of the compounds are reported.The DSC experiments prove that K_3ZnB_5O_(10)melts congruently. In Pb_xBa_(9-x)B_(18)O_(36), the FBB is B_3O_6group. By comparing the structures of Pb_xBa_(9-x)B_(18)O_(36)with that of β-BaB_2O_4,it is found that the arrangement of B_3O_6groups in the compounds leads to different SHGeffect. In K_3B_3O_3F_6, the FBB is B_3O_3F_6, but scarcely see the linkage of B-F under ambientpressure. CsB_5O_8crystallizes in the orthorhombic space group Pccn. By comparing thestructures of CsB_5O_8with that of α-CsB_5O_8, β-CsB_5O_8andγ-CsB_5O_8, it is found that thedifference of FBB among the compounds leads to crystallize in different space groups.
4. Research on two organic-inorganic hybrid borate compounds
Sr[B(C_6H_5O_7)_2](H_2O)_43H_2O and Ca[B(C_6H_6O_7)_2](H_2O)_4HCl have been synthesizedby the slow evaporation of water solution at room temperature. Their crystal structureswere established by single-crystal X-ray diffraction and optical properties were measured.
引文
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