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Preparation method and application of lithium metaborate crystal

A technology of lithium metaborate and crystal, which is applied in the field of preparation of lithium metaborate crystal, and achieves the effects of excellent deep ultraviolet transmittance, easy growth and processing, and easy processing.

Active Publication Date: 2019-10-15
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there have been studies on this crystal since then, there are few reports on the growth of high-quality large-size single crystal and the use of this crystal as an optical crystal.

Method used

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  • Preparation method and application of lithium metaborate crystal
  • Preparation method and application of lithium metaborate crystal
  • Preparation method and application of lithium metaborate crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1 Melt pulling method grows lithium metaborate crystal:

[0042] According to the chemical formula: Li 2 O+2H 3 BO 3 →LiBO 2 +H 2 O↑preparation of lithium metaborate crystals, the raw material used Li 2 O and H 3 BO 3 For analytical pure (≥99%):

[0043] Li directly 2 O and H 3 BO 3 According to the molar ratio of lithium: boron = 1:1, mix evenly and fully grind it, put it into a platinum crucible, slowly heat up to a temperature of 900°C, and keep the temperature at a constant temperature for 24 hours to obtain a mixed melt;

[0044] Preparation of lithium metaborate seed crystals: quickly cool down the obtained mixed melt by 5°C each time, and keep it at the corresponding temperature for 2 hours. Slowly lower the temperature at a rate of / d until the crystallization is complete, then lower the temperature to room temperature at a rate of 10°C / h, and spontaneously crystallize to obtain lithium metaborate seed crystals;

[0045] Put the prepared c...

Embodiment 2

[0048] Embodiment 2 melt pulling method grows lithium metaborate crystal:

[0049] Directly weigh the analytically pure (≥99%) lithium metaborate reagent and put it into a platinum crucible, slowly heat up to a temperature of 900° C., and keep the temperature at a constant temperature for 5 hours to obtain a mixed melt;

[0050] Preparation of lithium metaborate seed crystal: Lower the platinum wire fixed at the lower end of the seed rod into the obtained mixed melt, slowly cool down at a rate of 5°C / h until crystals appear on the platinum wire, and then rotate at a rate of 5r / min Slowly lower the temperature of the seed rod at a rate of 2°C / d. After the crystal grows to the desired size, lift it out of the liquid surface and drop it to room temperature at a rate of 30°C / h to obtain a lithium metaborate seed crystal ;

[0051] Put the prepared crucible containing the mixed melt into the crystal growth furnace, fix the obtained seed crystal on the seed crystal rod, lower the t...

Embodiment 3

[0053] Embodiment 3 melt top seed method grows lithium metaborate crystal:

[0054] According to the chemical formula: Li 2 CO 3 +2H 3 BO 3 →LiBO 2 +CO 2 ↑+H 2 O↑preparation of lithium metaborate crystals, the raw material used Li 2 CO 3 and H 3 BO 3 Analytical pure (≥99%);

[0055] Will Li 2 CO 3 and H 3 BO 3 According to the molar ratio of lithium: boron = 1:1, mix well and grind thoroughly, then put it into a corundum crucible and pre-fire at 300°C for 8 hours, then raise the temperature by 100°C each time and keep it at the corresponding temperature for 8 hours, take it out and grind it and compact it, Repeat this process until the temperature rises to 800°C, and finally keep the temperature at 800°C for 5 days to obtain polycrystalline powder of lithium metaborate compound, which is analyzed by X-ray, and the obtained X-ray spectrum is ground into powder with lithium metaborate single crystal The subsequent X-ray spectra are consistent;

[0056] Put the sy...

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Abstract

The invention relates to a lithium metaborate crystal and a preparation method and use thereof. The crystal has a chemical formula of LiBO2, a molecular weight of 49.75, and is a member of the monoclinic crystal system. The crystal has a P21 / c space group and lattice constants of a=5.85(8) Å, b=4.35(7) Å, c=6.46(6) Å, β=115(5) I°, and Z=4. The crystal can be applied in wavelengths of infrared-visible-deep ultraviolet, and is grown by utilizing a melt crystallization method or a flux method. The crystal obtained using the method described in the invention is easily grown and processed, and can be used in the manufacture of a polarizing beam splitting prism such as a Glan prism, a Wollaston prism, a Rochon prism or a beam-splitting polarizer, and other optical components, enabling crucial applications in the fields of optics and communication.

Description

technical field [0001] 本发明涉及一种用于红外-可见-深紫外波段的分子式为LiBO 2 的偏硼酸锂晶体的制备方法和用途,属于人工晶体生长技术领域和光学技术领域。 Background technique [0002] 双折射是光束入射到各向异性的晶体,分解为两束光而沿不同方向折射的现象。具有双折射现象的晶体称为双折射晶体。产生双折射现象的晶体可分为单轴晶体和双轴晶体,三方、四方或六方晶系的晶体是单轴晶体,正交、单斜和三斜晶系的晶体称为双轴晶体。晶体的双折射是电光功能材料的重要光学性能参数,伴随着近年来光通讯技术的迅猛发展,双折射晶体成为制作格兰棱镜、渥拉斯顿棱镜等偏振分束棱镜以及光隔离器、光束位移器、环形器等光通讯元件的关键材料。 [0003] 常用的双折射晶体材料主要有YVO 4 晶体、金红石晶体、LiNbO 3 晶体、方解石晶体、MgF 2 晶体以及α-BaB 2 o 4 晶体等。YVO 4 是一种性能良好的人工双折射晶体,而且容易用提拉法生长出大尺寸高光学品质的晶体,但是它的透过范围是400-5000nm,不能用于紫外区。 金红石虽然双折射大但由于硬度大加工器件难度较大。 LiNbO 3 晶体易于得到大尺寸晶体,但双折射率太小。 主要以天然形式存在的方解石晶体杂质含量比较高,人工合成比较困难,一般尺寸都比较小,无法满足大尺寸光学偏光元件的要求,普通方解石晶体只能使用于350nm以上波段,紫外光学级方解石晶体获得困难,其使用波段也无法达到深紫外区(<200nm)。 MgF 2 晶体是一种应用于深紫外很好的材料,它的透过范围宽(110-8500nm),但是它的双折射率太小,不适合用作制造格兰棱镜,只能用于洛匈棱镜,且光束分离角小,器件尺寸大,使用不便。α-BaB 2 o 4 由于存在固态相变,很容易在晶体生长过程中开裂。因此,急需探索新的能够克服现有双折射晶体缺点的新型双折射晶体材料从而满足光通讯技术等领域发展的迫切需求。 [0004] 含有碱金属或者碱土金属阳离子的硼酸盐具有宽的透过范围和优异的紫外透过能力,因此在光学领域尤其是在深紫外光谱区具有重要的应用价值。本发明提供的偏硼酸锂晶体分子式为LiBO 2 属于单斜晶系,是一个中心对称的化合物,1964年由W.H.Zacha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/10C30B9/12C30B11/00C30B15/00C30B17/00G02B1/08
CPCC30B9/12C30B11/00C30B15/00C30B17/00C30B29/10G02B1/08C01B35/121C30B11/003C30B19/02C30B29/22G02B5/04G02B5/3083C01P2002/76C01P2002/77C01P2006/60C01P2006/80C30B15/14
Inventor 潘世烈陈幸龙张方方侯雪玲
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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