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Flux growing method of R2CaB10O19 monocrystal

A r2cab10o19, growth method technology, applied in the direction of single crystal growth, single crystal growth, crystal growth, etc., can solve the problems of high melt viscosity and volatility, easy to produce inclusions, high growth temperature, avoid cleavage phenomenon, The effect of avoiding inclusions and reducing growth temperature

Inactive Publication Date: 2007-06-13
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 object of the invention is to overcome prior art growth R 2 CaB 10 o 19 Single crystals have relatively high growth temperature, high melt viscosity and volatility, high equipment requirements, complicated operation, and defects that are easy to generate inclusions, thus providing a method that can grow and melt at lower growth temperatures. R with less bulk viscosity and volatility, and less prone to inclusions 2 CaB 10 o 19 Single Crystal Flux Growth Method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1, preparation La 2 CaB 10 o 19 single crystal

[0018] According to La 2 o 3 :CaO:Li 2 O: B 2 o 3 1:2:1.55:11.65 molar ratio ingredients, weigh La 2 o 3 74.93 g, Ca 2 CO 3 46.00 grams, Li 2 CO 3 26.34 grams, B 2 o 3 186.54 grams, ground and mixed evenly, placed in a corundum crucible, heated slowly to 200°C in a muffle furnace for 10 hours, cooled, transferred to a small dish, and heated to 500°C in a muffle furnace for more than 24 hours. The product was crushed and ground and melted in batches in a Ф60mm×60mm platinum crucible. Put the platinum crucible containing the above-mentioned molten material into the crystal growth furnace, raise the temperature to 1040°C at a rate of 300°C / h to completely melt the above-mentioned molten material, and keep it at this temperature for 48 hours to fully homogenize the high-temperature solution. Use the seed crystal trial method to find that the saturation temperature for crystal growth is 980°C, cool t...

Embodiment 2

[0019] Embodiment 2, preparation (La 0.95 Nd 0.05 ) 2 CaB 10 o 19 single crystal

[0020] Follow R 2 o 3 :CaO:Li 2 O: B 2 o 3 It is a molar ratio of 1:2:2.3:13.97, where R represents two elements, La and Nd, and Nd 2 o 3 The number of moles of R 2 o 3 5% of La 2 o 3 61.91 g, Nd 2 o 3 3.364 g, CaCO 3 40.00 grams, Li 2 CO 3 33.98 grams, H 3 BO 3 345.5 grams, ground and mixed evenly, melted in batches in a platinum crucible of Ф60mm×60mm. Put the platinum crucible containing the above melting material into the crystal growth furnace, raise the temperature at 350 °C / h to 1000 °C to completely melt the above melting material, and keep it at this temperature for 24 hours to fully homogenize the high temperature solution. Use the seed crystal trial method to find that the saturation temperature of crystal growth is 942°C, cool the above high temperature solution to 952°C (10°C above the saturation temperature) at a rate of 30°C / h, and fix the seed crystal c...

Embodiment 3

[0021] Embodiment 3, preparation (La 0.85 Yb 0.15 ) 2 CaB 10 o 19 single crystal

[0022] Follow R 2 o 3 :CaO:Li 2 O: B 2 o 3 It is a molar ratio of 1:2:3.87:18.60, where R represents two elements, La and Yb, and Yb 2 o 3 The number of moles of R 2 o 3 15% of La 2 o 3 44.312 grams, Yb 2 o 3 9.458 g, CaCO 3 32.00 grams, Li 2 CO 3 45.76 grams, B 2 o 3 207.19 grams, ground and mixed evenly, put into a corundum crucible, placed in a muffle furnace and slowly raised to 500°C, and kept at a constant temperature for more than 24 hours, the product was melted in batches in a platinum crucible of Ф60mm×60mm, and after the crucible was cooled, put It is placed in a crystal growth furnace, heated to melting at a rate of 300°C / h, kept at this temperature for 24 hours to fully homogenize the high-temperature solution, cooled to near the saturation temperature at a rate of 50°C / h, and used as a seed crystal Find the exact saturation temperature by trial and error. Aft...

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Abstract

The invention relates to an R2CaB10O19 single crystal fluxing agent growth method. It includes the following steps: preparing in mol ratio R2O3: CaO: Li2O: B 2 O 3 1:1.5-4:1-10:9-32; doing pretreatment; fully melting in growth furnace; leading in seed crystal; keeping temperature for 10-200min; quickly cooling to saturation temperature; controlling each parameter according to the crystal growth; lifting crystal; gaining the purpose cooling the room temperature at rate of under 50 centigrade degree per hour. The method is used new fluxing agent to greatly reduce growth temperature, high temperature solution viscosity and volatility. Thus, it can stably growth out the single crystal.

Description

technical field [0001] The present invention relates to a kind of growth method of single crystal, relate in particular to R 2 CaB 10 o 19 Flux growth method for single crystal, wherein, R represents one or more elements; when R represents only one element, it is La; when R represents multiple elements, one of them is La, and the remaining elements are selected from rare earth elements Element or Y. Background technique [0002] R 2 CaB 10 o 19 Single crystals can be used as nonlinear optical crystals, and are widely used in the manufacture of nonlinear optical devices and laser nonlinear optical composite functional devices. The existing technology prepares the crystal, usually in the melt by the pulling method or the Kyroplasty method, and can also use R as disclosed in Chinese patent ZL98108570.9. 2 o 3 -CaO-B 2 o 3 The system is used as a flux, and the flux method is used for growth. Using the above method, R 2 CaB 10 o 19 single crystal. However, the grow...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/22
Inventor 吴以成景芳丽傅佩珍陈创天
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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