CaLa_2B_（10）O_（19）晶体的生长
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摘要
本论文围绕非线性光学晶体CaLa_2B_(10)O_(19)(LCB)的生长,从以下几个方面展开工作:CaO-La_2O_3-B_2O_3 三元体系中各组分含量的分析,LaB_3O_6-CaB_4O_7 赝二元体系相图的研究,以CaB_4O_7 为助溶剂生长LCB 晶体过程中动力学因素的初步研究,LCB 晶体生长的研究。
(1)用化学分析的方法对CaO-La_2O_3-B_2O_3 三元体系中CaO、La_2O_3、B_2O_3的含量进行测定。用pH=10 的NH_3·H_2O-NH_4Cl 缓冲溶液分离Ca~(2+)、La~(3+),用络合滴定方法测定CaO、La_2O_3的含量,并计算B2O3的含量。CaO、La_2O_3的回收率分别大98%和98.5%。确定了CaLa_2B_(10)O_(19)晶体的组成。
(2)通过X-射线粉末衍射和差热分析等方法研究了LaB_3O_6-CaB_4O_7赝二元体系相图。LaB_3O_6-CaB_4O_7 赝二元体系中除了LaB_3O6 和CaB_4O_7 外只存在化合物CaLa_2B_(10)O_(19),它是一种非同成分熔融的化合物,转熔温度约1047℃,在此温度下液相、LaB_3O_6和CaLa_2B_(10)O_(19)之间发生包晶反应。在温度967℃左右,存在CaB_4O_7、CaLa_2B_(10)O_(19) 和液相之间的共晶反应,共晶点的成分约87mol% CaB_4O_7。根据所得到的结果,采用高温溶液生长法,选择摩尔比CaB_4O_7:CaLa_2B_(10)O_(19)分别为1:1、1.5:1 和2:1 三种不同浓度的高温溶液体系来生长CaLa_2B_(10)O_(19),结果都可以长出CaLa_2B_(10)O_(19) 晶体。
(3)在我们实验室已在CaO-La_2O_3-B_2O_3 三元高温溶液体系中发现的新晶体基础上,用化学分析的方法确定了它的组成是CaLa_2B_8O_(16)。进一步研究了高温溶液的动力学特性,阐述并用实验证明了CaLa_2B_8O_(16)晶体相的析出和B_2O_3挥发的关系,通过在溶液中添加适量的B_2O_3可以增加溶液的稳定性。采用助熔剂法,选用B_2O_3、CaB_4O_7 和Ca_2B_6O_(11) 等不同的化合物做助熔剂来生长CaLa_2B_8O_(16) 晶体。在以一定量Ca_2B_6O_(11)做助溶剂时,可以长出了24×14×6mm~3较为透明的CaLa_2B_8O_(16)晶体。该晶体的粉末倍频效应接近KDP 的粉末倍频效应,并且它的物理化学性能较为稳定,不易潮解。
In this dissertation, the growth of nonlinear optical crystal, CaLa_2B_(10)O_(19) (LCB) was focused. The major work consisted of: Measurement of the content of CaO、La_2O_3、B2O3 in the CaO-La_2O_3-B_2O_3 system., Investigation of the phase relation of the pseudo-binary LaB_3O_6-CaB_4O_7 system, Study on the kinetics in the CaLa_2B_(10)O_(19)-CaB_4O_7 system and the growth of LCB crystal.
(1) The content of CaO、La_2O_3、B_2O_3 in the CaO-La_2O_3-B_2O_3 system were measured by chemical analysis. Ca~(2+)、La~(3+) were separated by the pH=10 puffer solution and measured by the means of complexometric titration, the content of B_2O_3 was calculated. The recoveries of CaO、La_2O_3 were more than 98% and 98.5% respectively. The composition of CaLa_2B_(10)O_(19) was determined.
(2) Phase relationship of the LaB_3O_6-CaB_4O_7 pseudo-binary system was investigated by means of X-ray powder diffraction analysis and differential thermal analysis. In the system, there exists a compound of CaLa_2B_(10)O_(19) except for LaB_3O_6 and CaB_4O_7. A peritectic reaction occurs at 1047℃,the compound of CaLa_2B_(10)O_(19) melts incongruently to LaB_3O_6 and liquid. A eutectic reaction, among CaLa_2B_(10)O_(19), CaB_4O_7 and liquid phase, occurs at 967℃and the composition of eutectic point is about 87mol% CaB_4O_7. According to the result, we successfully obtained the CaLa_2B_(10)O_(19) single crystal from three high-temperature solutions with the compositions (molar ratio) of CaB_4O_7: CaLa_2B_(10)O_(19)=1:1, CaB_4O_7: CaLa_2B_(10)O_(19)=1.5:1 and CaB_4O_7: CaLa_2B_(10)O_(19)=2:1.
(3) On the base of the find of a new calcium-lanthanunm borate crystal in the preceding experiment, when attempting to grow the CaLa_2B_(10)O_(19) single crystal from the high-temperature solution with the composition of CaLa_2B_(10)O_(19):CaB_4O_7 =1:1, the crystal was subject to wet chemical analysis and the result showed the chemical composition of the crystal is CaLa_2B_8O_(16). Furthermore, We found the B_2O_3 was the
volatile component in the solution and elucidated the relationship between the CaLa2B8O16 crystal formation and the volatility. Further supporting experiment was carried to directly obtain the CaLa2B8O16 crystal from the high-temperature solution with the composition of CaO:La2O3:B2O3=2:1:4. On contract, by adding more B2O3 to the solution with the composition of CaLa2B10O19:CaB4O7 =1:1, the stability of the solution was improved in the process to grow CaLa2B10O19. Among these solvents of B2O3 CaB4O7 and CaLa2B8O16, we chose suitable weight CaLa2B8O16 as solvent and obtained a transparent crystal with dimensions of 24 14 6mm3. Second harmonic generation effect of the crystal powder is nearly that of KDP. The crystal is chemical stable and not hygroscopic. (4) LCB single crystal were grown by the top seeded solution growth (TSSG) method using self-flux, The effect of the growth conditions, such as solutions composition, temperature gradient, cooling rate, rotation rate, seed direction, were investigated. An even temperature gradient in the axial direction over surface of solutions was required to avoid the erosion of the seed crystal. Low rotation and seeding in c direction were helpful to grow relative large LCB crystal, With careful control of the above parameters, clear crystals with relatively large were grown from the solution with the composition of CaLa2B10O19:CaB4O7 =1:1.5, and large crystal with relative clear were obtained from the solution with the composition of CaLa2B10O19:CaB4O7 :B2O3=1:1:0.7.
(1)用化学分析的方法对CaO-La_2O_3-B_2O_3 三元体系中CaO、La_2O_3、B_2O_3的含量进行测定。用pH=10 的NH_3·H_2O-NH_4Cl 缓冲溶液分离Ca~(2+)、La~(3+),用络合滴定方法测定CaO、La_2O_3的含量,并计算B2O3的含量。CaO、La_2O_3的回收率分别大98%和98.5%。确定了CaLa_2B_(10)O_(19)晶体的组成。
(2)通过X-射线粉末衍射和差热分析等方法研究了LaB_3O_6-CaB_4O_7赝二元体系相图。LaB_3O_6-CaB_4O_7 赝二元体系中除了LaB_3O6 和CaB_4O_7 外只存在化合物CaLa_2B_(10)O_(19),它是一种非同成分熔融的化合物,转熔温度约1047℃,在此温度下液相、LaB_3O_6和CaLa_2B_(10)O_(19)之间发生包晶反应。在温度967℃左右,存在CaB_4O_7、CaLa_2B_(10)O_(19) 和液相之间的共晶反应,共晶点的成分约87mol% CaB_4O_7。根据所得到的结果,采用高温溶液生长法,选择摩尔比CaB_4O_7:CaLa_2B_(10)O_(19)分别为1:1、1.5:1 和2:1 三种不同浓度的高温溶液体系来生长CaLa_2B_(10)O_(19),结果都可以长出CaLa_2B_(10)O_(19) 晶体。
(3)在我们实验室已在CaO-La_2O_3-B_2O_3 三元高温溶液体系中发现的新晶体基础上,用化学分析的方法确定了它的组成是CaLa_2B_8O_(16)。进一步研究了高温溶液的动力学特性,阐述并用实验证明了CaLa_2B_8O_(16)晶体相的析出和B_2O_3挥发的关系,通过在溶液中添加适量的B_2O_3可以增加溶液的稳定性。采用助熔剂法,选用B_2O_3、CaB_4O_7 和Ca_2B_6O_(11) 等不同的化合物做助熔剂来生长CaLa_2B_8O_(16) 晶体。在以一定量Ca_2B_6O_(11)做助溶剂时,可以长出了24×14×6mm~3较为透明的CaLa_2B_8O_(16)晶体。该晶体的粉末倍频效应接近KDP 的粉末倍频效应,并且它的物理化学性能较为稳定,不易潮解。
In this dissertation, the growth of nonlinear optical crystal, CaLa_2B_(10)O_(19) (LCB) was focused. The major work consisted of: Measurement of the content of CaO、La_2O_3、B2O3 in the CaO-La_2O_3-B_2O_3 system., Investigation of the phase relation of the pseudo-binary LaB_3O_6-CaB_4O_7 system, Study on the kinetics in the CaLa_2B_(10)O_(19)-CaB_4O_7 system and the growth of LCB crystal.
(1) The content of CaO、La_2O_3、B_2O_3 in the CaO-La_2O_3-B_2O_3 system were measured by chemical analysis. Ca~(2+)、La~(3+) were separated by the pH=10 puffer solution and measured by the means of complexometric titration, the content of B_2O_3 was calculated. The recoveries of CaO、La_2O_3 were more than 98% and 98.5% respectively. The composition of CaLa_2B_(10)O_(19) was determined.
(2) Phase relationship of the LaB_3O_6-CaB_4O_7 pseudo-binary system was investigated by means of X-ray powder diffraction analysis and differential thermal analysis. In the system, there exists a compound of CaLa_2B_(10)O_(19) except for LaB_3O_6 and CaB_4O_7. A peritectic reaction occurs at 1047℃,the compound of CaLa_2B_(10)O_(19) melts incongruently to LaB_3O_6 and liquid. A eutectic reaction, among CaLa_2B_(10)O_(19), CaB_4O_7 and liquid phase, occurs at 967℃and the composition of eutectic point is about 87mol% CaB_4O_7. According to the result, we successfully obtained the CaLa_2B_(10)O_(19) single crystal from three high-temperature solutions with the compositions (molar ratio) of CaB_4O_7: CaLa_2B_(10)O_(19)=1:1, CaB_4O_7: CaLa_2B_(10)O_(19)=1.5:1 and CaB_4O_7: CaLa_2B_(10)O_(19)=2:1.
(3) On the base of the find of a new calcium-lanthanunm borate crystal in the preceding experiment, when attempting to grow the CaLa_2B_(10)O_(19) single crystal from the high-temperature solution with the composition of CaLa_2B_(10)O_(19):CaB_4O_7 =1:1, the crystal was subject to wet chemical analysis and the result showed the chemical composition of the crystal is CaLa_2B_8O_(16). Furthermore, We found the B_2O_3 was the
volatile component in the solution and elucidated the relationship between the CaLa2B8O16 crystal formation and the volatility. Further supporting experiment was carried to directly obtain the CaLa2B8O16 crystal from the high-temperature solution with the composition of CaO:La2O3:B2O3=2:1:4. On contract, by adding more B2O3 to the solution with the composition of CaLa2B10O19:CaB4O7 =1:1, the stability of the solution was improved in the process to grow CaLa2B10O19. Among these solvents of B2O3 CaB4O7 and CaLa2B8O16, we chose suitable weight CaLa2B8O16 as solvent and obtained a transparent crystal with dimensions of 24 14 6mm3. Second harmonic generation effect of the crystal powder is nearly that of KDP. The crystal is chemical stable and not hygroscopic. (4) LCB single crystal were grown by the top seeded solution growth (TSSG) method using self-flux, The effect of the growth conditions, such as solutions composition, temperature gradient, cooling rate, rotation rate, seed direction, were investigated. An even temperature gradient in the axial direction over surface of solutions was required to avoid the erosion of the seed crystal. Low rotation and seeding in c direction were helpful to grow relative large LCB crystal, With careful control of the above parameters, clear crystals with relatively large were grown from the solution with the composition of CaLa2B10O19:CaB4O7 =1:1.5, and large crystal with relative clear were obtained from the solution with the composition of CaLa2B10O19:CaB4O7 :B2O3=1:1:0.7.
引文
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