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Fluxing agent growing method of K2Al2B2O7 crystal

A k2al2b2o7, growth method technology, applied in the direction of crystal growth, single crystal growth, single crystal growth, etc., can solve problems such as unfavorable KABO growth, affecting solute transport, slow melt flow, etc., to avoid composition shift and improve stability. properties and, the effect of reducing viscosity

Inactive Publication Date: 2010-07-28
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

Other fluxes (such as MoO 3 ), the viscosity of the system increases, the melt flows slowly, which affects the transmission of the solute, and the flux is easily brought into the crystal during growth, resulting in the formation of inclusions, which seriously affects the quality of the crystal
In addition, due to the high temperature, the saturation point temperature is 950-1000°C, so the volatilization is serious, and there are white needles around the seed rod and the furnace mouth, which is not conducive to the growth of KABO

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: adopt flux method to prepare K 2 Al 2 B 2 o 7 the crystal

[0028] with K 2 Al 2 B 2 o 7 Powder and analytically pure NaF are used as raw materials, according to the molar ratio K 2 Al 2 B 2 o 7 : NaF = 1: 1.5 ingredients, weighed 265.62g K 2 Al 2 B 2 o 7 Powder, 63gNaF, that is, the molar ratio K in the growth system 2 Al 2 B 2 O7:NaF=1:1.5; After grinding and mixing the weighed raw materials evenly, put them into an open platinum crucible of Φ70mm×85mm, melt them in a muffle furnace at 1050°C, and after cooling to room temperature, put the above-mentioned Put the crucible of molten material into the vertical electric furnace wire heating single crystal growth furnace, seal the opening on the top of the furnace with insulating material, and leave a hole at the position corresponding to the top of the furnace and the center of the crucible for the seed rod to enter and exit. Small hole, heat up to 950°C to completely melt the above-mentio...

Embodiment 2

[0031] Embodiment 2: adopt flux method to prepare K 2 Al 2 B 2 o 7 the crystal

[0032] with K 2 Al 2 B 2 o 7 powder analytically pure BaF 2 as raw material, according to the molar ratio K 2 Al 2 B 2 o 7 :BaF 2 = 1:1.4 ingredients, weighing 265.62g K 2 Al 2 B 2 o 7 Powder, 245.44g BaF 2 , that is, the molar ratio K in the growth system 2 Al 2 B 2 o 7 :BaF 2 =1:1.4. Grind and mix the weighed raw materials evenly, put them into a Φ70mm×85mm open platinum crucible, first melt them in a muffle furnace at 950°C, and after cooling to room temperature, put the crucible containing the molten material into a vertical In the vertical single crystal growth furnace, seal the opening at the top of the furnace with insulating material, leave a small hole at the position corresponding to the center of the crucible on the top of the furnace for the seed rod to enter and exit, and raise the temperature to 960°C to make the above melting The material is completely melted...

Embodiment 3

[0035] Embodiment 3: adopt flux method to prepare K 2 Al 2 B 2 o 7 the crystal

[0036] with K 2 CO 3 、Al 2 o 3 、H 3 BO 3 and analytically pure NaF, BaF 2 as raw material, according to the molar ratio K 2 CO 3 : Al 2 o 3 :H 3 BO 3 :NaF:BaF 2 = 1:1:2:1.3:0.6 ingredients, weigh 138.22g K 2 CO 3 Powder, 102gAl 2 o 3 Powder, 123.66g H 3 BO 3 , 54.6gNaF, 105.19gBaF 2 , that is, the molar ratio K in the growth system 2 Al 2 B 2 o 7 :NaF:BaF 2 =1:1.3:0.6. Grind and mix the weighed raw materials evenly, put them into an open platinum crucible of Φ70mm×85mm, melt them in a muffle furnace at 1000°C, and put the crucible containing the molten material into a vertical crucible after cooling to room temperature. In the vertical single crystal growth furnace, seal the opening at the top of the furnace with insulating material, leave a small hole at the position corresponding to the center of the crucible on the top of the furnace for the seed rod to enter and ex...

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Abstract

The invention relates to a fluxing agent growing method of K2Al2B2O7 crystal. The method comprises the following steps: mixing K2Al2B2O7 with fluxing agent in a molar ratio of 1:1.4-2.2, placing the mixture in a 950-1050 DEG C of muffle furnace to melt, cooling at room temperature to obtain growing raw material; then placing in an electric stove wire heating crystal growing furnace to heat and obtain a high temperature solution; introducing seed crystal under 2-10 DEG C above saturation temperature; cooling by using the saturation point temperature as the cooling starting point while rotating the crystal, wherein the vertical temperature gradient of the high temperature solution is 0.05-1 DEG C / cm; lifting the crystal, which grows to the required size, from the level surface to cool to the room temperature and obtain K2Al2B2O7 crystal, wherein the fluxing agent is M'F, M''F or M'F+M''F, M' is Li, Na or K, and M'' is Ca or Ba. The method of the invention has low growing temperature and the growing system has low volatility and viscosity so that solute can be conveniently transported and high optical quality K2Al2B2O7 crystal without inclusion and optical path can be grown.

Description

technical field [0001] The present invention relates to a kind of growth method of single crystal, specifically make and relate to K 2 Al 2 B 2 o 7 Flux growth method for nonlinear optical crystals. Background technique [0002] K 2 Al 2 B 2 o 7 The compound was first synthesized by Kaduk [Power Diffraction File Set.46-582], and its single phase was proved by X-ray diffraction method, but no detailed structure was given, and its properties were not clear. In 1998, Chinese and Japanese scientists [Ye Ning, Zeng wenrong, Wu baichang, Chen Chuangtian, "Two new nonlinear optical crystals: BaAl 2 B 2 o 7 and K 2 Al 2 B 2 o 7 ", SPIE Vol.3556, 21-23; Zhanggui Hu, Y. Mori, T. Higashiyama, et al., "K 2 Al 2 B 2 o 7 -A Newnonlinear optical crystal”, SPIE Vol.3556, 156-161] also reported K 2 Al 2 B 2 o 7 (KABO for short) is an excellent nonlinear optical material, and its structure was analyzed by growing KABO single crystal. The space group of KABO is P321, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B11/00C30B29/22
Inventor 胡章贵岳银超吴振雄
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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