Method and device for near stoichiometric lithium niobate single crystal growth

A near-stoichiometric ratio and growth method technology, which is applied in the field of preparing near-stoichiometric lithium niobate single crystals, can solve problems such as uneven melting in the melting zone, low melting efficiency, and affecting crystal quality, achieving easy cleaning, Extend the service life and avoid the effect of low efficiency

Inactive Publication Date: 2012-06-06
UNIONLIGHT TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the high melting point of LN crystals (generally at 1200-1300°C), if the reaction pre-synthesis is not performed in advance, at this temperature, it is easy to cause volatilization of oxides and carbonates, which makes the melt composition deviate; moreover, the raw materials Middle Li 2 CO 3 Excessive amount, cannot be completely decomposed during the melting process of raw materials, so a large amount of gas will be generated during the crystal growth process, and bubbles will be formed inside the crystal, affecting the quality of the crystal
[0011] Another Chinese patent application No. 200410024543.3 discloses a technology that improves the double crucible method. During the crystal growth process, the crucible is divided into two regions by a movable upper closed noble metal cylinder, It solves the problems of low melting efficiency of the double-crucible device in the prior art, uneven melting in the melting zone during continuous feeding, easy generation of floating crystals and volatilization of lithium oxide, etc.
However, in the growth process of this kind of high-temperature volatile crystals, it is found that the volatilized components in the high-temperature melt are quickly deposited on the heat preservation cover, rather than existing in the sealed system in the form of gas, so the sealed system cannot It has the effect of inhibiting the volatilization of components after reaching the saturated vapor pressure

Method used

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  • Method and device for near stoichiometric lithium niobate single crystal growth
  • Method and device for near stoichiometric lithium niobate single crystal growth

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Embodiment 1

[0029]Use commercial high-purity raw materials, prepare LN polycrystalline raw materials A and B (A: Li 2 O:Nb 2 o 5 =1:1.05, B: Li 2 O:Nb 2 o 5 =1:1.15), material B is used as raw material, and material A is used as supplementary material. A suspended three-crucible automatic continuous feeding system is adopted. First, material B is put into an iridium gold crucible to melt. After the material is completely melted, slowly lower the iridium gold double-layer partition to a place 1-2mm away from the liquid surface for preheating. After the temperature of the two is close, the partition plate is lowered so that it extends vertically into the molten iridium crucible, and the LN crystal is grown by the process of seeding, necking, shouldering, equal diameter, and finishing by the pulling method. The supplementary material A is put into the transition chamber first, after vacuuming and N filling 2 +CO 2 (N 2 :CO 2 =2:1 (volume ratio)) mixed gas, slowly added to the supply...

Embodiment 2

[0031] Use commercial high-purity raw materials, prepare LN polycrystalline raw materials A and B (A: Li 2 O:Nb 2 o 5 =1:1.15, B:Li 2 O:Nb 2 o 5 =1:1.30), material B is used as raw material, and material A is used as supplementary material. A suspended three-crucible automatic continuous feeding system is adopted. First, material B is put into an iridium gold crucible to melt. After the material is completely melted, slowly lower the iridium gold double-layer partition to a place 1-2mm away from the liquid surface for preheating. After the temperature of the two is close, the partition plate is lowered so that it extends vertically into the molten iridium crucible, and the LN crystal is grown by the process of seeding, necking, shouldering, equal diameter, and finishing by the pulling method. The supplementary material A is put into the transition chamber first, after vacuuming and N filling 2 +CO 2 (N 2 :CO 2 =1:1 (volume ratio)) mixed gas, slowly added to the supply...

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Abstract

The invention provides a method and a device for near stoichiometric lithium niobate single crystal growth. The method and the device are main suitable for Czochralski method-based growth of near stoichiometric lithium niobate single crystals having uniform components and relate to the field of crystal growth. The method is characterized in that liquid synthetic polycrystalline raw materials are prepared into near stoichiometric lithium niobate single crystals having large sizes and high quality in a N2-CO2 weak-oxidizing protective atmosphere through a suspension-type three-crucible automatic continuous charging system. The method and the device have the advantages that polycrystalline raw material components are uniform; a Li2O volatilization amount is low; automatic continuous charging is realized; melting efficiency is high; and a temperature fluctuation of a crystal growth zone is small.

Description

technical field [0001] The invention relates to the field of crystal growth, in particular to a method for preparing a near-stoichiometric lithium niobate single crystal and a device used therefor. Background technique [0002] Lithium niobate (LiNbO 3 , LN) crystal is an excellent multifunctional crystal, which has excellent piezoelectric properties, nonlinear optical properties, electro-optic and photorefractive properties, etc. Large-sized LN crystals can be grown by pulling method, and LN crystals have good thermal stability, chemical stability and mechanical stability. Based on the above advantages, LN crystals are widely used in nonlinear optics, optoelectronics, communications and optical storage. The usual lithium niobate crystals are grown by the pulling method from the homogeneous eutectic composition, and the Li / Nb molar ratio is 48.4 / 51.6 instead of the stoichiometric ratio. The absence of Li ions causes a large number of vacancy defects in the crystal, which ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/30C30B15/00
Inventor 柳祝平黄小卫王有明
Owner UNIONLIGHT TECH
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