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Method for flux growth of Na3La9B8027

A growth method and crystal growth technology, applied in crystal growth, single crystal growth, single crystal growth, etc., can solve the problems of high volatility of the growth system, high equipment requirements, complicated operation, etc., and achieve low equipment requirements, low cost, Simple operation effect

Inactive Publication Date: 2008-03-26
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome prior art growth Na 3 La 9 B 8 o 27 Crystals have the defects of high growth temperature, high volatility of the growth system, high equipment requirements, and complicated operation, so as to provide a method that can grow at a lower growth temperature, the growth system is less volatile, and the crystal is layered. phenomenon significantly reduced Na 3 La 9 B 8 o 27 Crystal Flux Growth Method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: adopt Na 2 O-B 2 o 3 -NaF flux to prepare Na 3 La 9 B 8 o 27 the crystal

[0021] Take Na 3 La 9 B 8 o 27 Powder (synthesized according to the method disclosed in Chinese patent application 01134393.1) and analytically pure Na 2 CO 3 、H 3 BO 3 , NaF as raw material, molar ratio Na 3 La 9 B 8 o 27 :Na 2 CO 3 :H 3 BO 3 : NaF = 1: 5: 4.6: 13.13 ingredients, weigh 110 grams of Na 3 La 9 B 8 o 27 Powder, 31.723 g Na 2 CO 3 , 17.026 g H 3 BO 3 , 33 grams of NaF, that is, the molar ratio of Na in the growth system 3 La 9 B 8 o 27 :Na 2 O: B 2 o 3:NaF=1:5:2.3:13.13. Sodium carbonate in the raw material can be replaced by a corresponding amount of sodium nitrate, sodium oxalate, and sodium hydroxide; boric acid can be replaced by a corresponding amount of boron oxide. Grind and mix the weighed raw materials evenly, place them in a corundum crucible, put them in a muffle furnace and raise the temperature to 500°C, and keep the te...

Embodiment 2

[0022] Embodiment 2: adopt Na 2 O-B 2 o 3 -NaF flux to prepare Na 3 La 9 B 8 o 27 the crystal

[0023] Take Na 3 La 9 B 8 o 27 Powder (synthesized according to the method disclosed in Chinese patent application 01134393.1) and analytically pure Na 2 CO 3 、H 3 BO 3 , NaF as raw material, molar ratio Na 3 La 9 B 8 o 27 :Na 2 CO 3 :H 3 BO 3 : NaF = 1: 6: 6: 13.13 ingredients, weigh 110 grams of Na 3 La 9 B 8 o 27 Powder, 38.067 g Na 2 CO 3 , 22.207 g H 3 BO 3 , 33 grams of NaF, that is, the molar ratio of Na in the growth system 3 La 9 B 8 o 27 :Na 2 O: B 2 o 3 :NaF=1:6:3:13.13. Sodium carbonate in the raw material can be replaced by a corresponding amount of sodium nitrate, sodium oxalate, and sodium hydroxide; boric acid can be replaced by a corresponding amount of boron oxide. Grind and mix the weighed raw materials evenly, place them in a corundum crucible, put them in a muffle furnace and raise the temperature to 500°C, and keep the tempe...

Embodiment 3

[0024] Embodiment 3: adopt Na 2 O-B 2 o 3 -NaF flux to prepare Na 3 La 9 B 8 o 27 the crystal

[0025] Take Na 3 La 9 B 8 o 27 Powder (synthesized according to the method disclosed in Chinese patent application 01134393.1) and analytically pure Na 2 CO 3 、H 3 BO 3 , NaF as raw material, molar ratio Na 3 La 9 B 8 o 27 :Na 2 CO 3 :H 3 BO 3 : NaF=1: 7.54: 6.46: 8.75 ingredients, weigh 100 grams of Na 3 La 9 B 8 o 27 Powder, 43.480 g Na 2 CO 3 , 21.741 g H 3 BO 3 , 20 grams of NaF, that is, the molar ratio of Na in the growth system 3 La 9 B 8 o 27 :Na 2 O: B 2 o 3 :NaF=1:7.54:3.23:8.75. Sodium carbonate in the raw material can be replaced by a corresponding amount of sodium nitrate, sodium oxalate, and sodium hydroxide; boric acid can be replaced by a corresponding amount of boron oxide. Grind and mix the weighed raw materials evenly, place them in a corundum crucible, put them in a muffle furnace and raise the temperature to 500°C, and keep t...

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Abstract

This invention relates to a growing method for a flux of a non-linearity optical crystal including preparing materials according to the mol ration of 1;5-7.54 : 2.3-3.5: 8.75-35 of Na3La9B8027:Na20:B203 :NaF pre-processing, then rising the temperature in a crystal growing furnace till the complete melt, in which, the constant temperature uniforms the solution fully then introducing inoculating crystals above the saturation temperature of 5-20deg.C and keeping constant for 10-30mitutes then reducing the temperature quickly to the saturated, controlling the parameters to grow crystals, then the crystals break away from the surface to reduce the temperature to the room in the rate not greater than 50deg.C / h to get the crystal.

Description

technical field [0001] The present invention relates to a kind of growth method of single crystal, relate to Na in particular 3 La 9 B 8 o 27 Flux growth method for nonlinear optical crystals. Background technique [0002] In nonlinear optical crystal materials, the chemical formula is Na 3 La 9 B 8 o 27 Rare earth nonlinear optical crystals are widely used in the manufacture of nonlinear optical devices. In the Chinese patent application with application number 01134393.1, it is disclosed that the chemical formula is Na 3 La 9 B 8 o 27 The compound, its nonlinear optical crystal, the preparation method of the crystal and the nonlinear optical device made of the crystal. which is based on Na 2 O and B 2 o 3 For flux growth Na 3 La 9 B 8 o 27 Crystal, the growth temperature of this method is relatively high, and the growth system is highly volatile, which requires high equipment, which is not conducive to the operation during the crystal growth process, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B9/04C30B9/06C30B17/00C30B29/22
Inventor 傅佩珍李云阁张国春吴以成陈创天
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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