Al-doped CsLiB6O10 crystal growth fluxing agent and crystal growth method

A technology of crystal growth and flux, which is applied in the field of optical materials, can solve the problems of poor crystal growth stability and repeatability, poor solute transport and heat transfer, and difficulty in accurately measuring the saturation point temperature, so as to achieve easy crystal growth and anti-corrosion. Increased deliquescence ability and reduced growth difficulty

Pending Publication Date: 2017-08-18
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

However, the self-flux system has the following disadvantages: the viscosity of the system is extremely high (>1000cp), the solute transport and heat transfer are not smooth, the crystals are prone to defects such as inclusions during growth, and it is difficult to obtain high-quality crystals; , the saturation point temperature is relatively high, between 840 and 860 ° C, the system volatilizes seriously, and it is easy to cause component deviation. Floating crystals are often formed on the surface of the high-temperature solution, and the floating crystals are easy to collide with the crystals, and volatiles can corrode the seed crystals. Crystals are easy to fall off during growth; in addition, the saturation point temperature in this system fluctuates greatly, it is difficult to accurately measure the saturation point temperature, it is difficult to control the initial growth rate of crystals, and the stability and repeatability of crystal growth are poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1: adopt Cs 2 O–Li 2 O–MoO 3 Preparation of Al-doped CLBO Crystals by Flux System

[0039] to CsLiB 6 o 10 Powder and analytically pure Cs 2 CO 3 , Li 2 CO 3 、MoO 3 、Al 2 o 3 As raw material, in molar ratio CsLiB 6 o 10 : Cs 2 CO 3 : Li 2 CO 3 :MoO 3 :Al 2 o 3 = 2:1:1:2:0.05 ingredients, weigh 820.58 grams of CsLiB 6 o 10 Powder, 366.54 g Cs 2 CO 3 , 83.13 g Li 2 CO 3 , 323.87 g MoO 3 , 5.88 g Al 2 o 3 , that is, the molar ratio of CsLiB in the growth system 6 o 10 : Cs 2 O: Li 2 O: MoO 3 :Al 2 o 3 =2:1:1:2:0.05.

[0040] Grind and mix the weighed raw materials evenly, then add Φ100×70mm in batches 3 In a platinum crucible, it is first melted in a muffle furnace at 920 ° C, and after cooling to room temperature, it is the raw material for crystal growth. The crucible for crystal growth is 10 cm high, and the liquid level (liquid level) is about 8 cm high from the bottom of the crucible.

[0041] Put the crystal growth raw...

Embodiment 2

[0045] Embodiment 2: Adopt Cs 2 O–Li 2 O–MoO 3 Preparation of Al-doped CLBO Crystals by Flux System

[0046] to CsLiB 6 o 10 Powder and analytically pure Cs 2 CO 3 , Li 2 CO 3 、MoO 3 、Al 2 o 3 As raw material, in molar ratio CsLiB 6 o 10 : Cs 2 CO 3 : Li 2 CO 3 :MoO 3 :Al 2 o 3 = 2:1:1:2:0.10 ingredients, weigh 820.58 grams of CsLiB 6 o 10 Powder, 366.54 g Cs 2 CO 3 , 83.13 g Li 2 CO 3 , 323.87 g MoO 3 , 11.47 g Al 2 o 3 , that is, the molar ratio of CsLiB in the growth system 6 o 10 : Cs 2 O: Li 2 O: MoO 3 :Al 2 o 3 =2:1:1:2:0.10. After grinding and mixing the weighed raw materials evenly, add Φ100×70mm 3 In a platinum crucible, it is first melted in batches in a muffle furnace at 940 ° C, and after cooling to room temperature, it becomes the raw material for crystal growth.

[0047] Put the crystal growth raw material into the single crystal growth furnace heated by resistance wire, seal the opening on the top of the furnace with a cover ...

Embodiment 3

[0050] Embodiment 3: Adopt Cs 2 O–Li 2 O–MoO 3 Preparation of Al-doped CLBO Crystals by Flux System

[0051] to CsLiB 6 o 10 Powder and analytically pure Cs 2 CO 3 , Li 2 CO 3 、MoO 3 、Al 2 o 3 As raw material, in molar ratio CsLiB 6 o 10 : Cs 2 CO 3 : Li 2 CO 3 :MoO 3 :Al 2 o 3 = 2:1:1:2:0.25 ingredients, weigh 820.58 grams of CsLiB 6 o 10 Powder, 366.54 g Cs 2 CO 3 , 83.13 g Li 2 CO 3 , 323.87 g MoO 3 , 28.68 grams of Al 2 o 3 , that is, the molar ratio of CsLiB in the growth system 6 o 10 : Cs 2 O: Li 2 O: MoO 3 :Al 2 o 3 =2:1:1:2:0.25. After grinding and mixing the weighed raw materials evenly, add Φ100×70mm 3 In a platinum crucible, it is first melted in batches in a muffle furnace at 950 ° C, and after cooling to room temperature, it becomes the raw material for crystal growth.

[0052]Put the crystal growth raw material into the single crystal growth furnace heated by resistance wire, seal the opening on the top of the furnace with a ...

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Abstract

The invention belongs to the field of optical materials and provides an Al-doped CsLiB6O10 crystal growth fluxing agent. The Al-doped CsLiB6O10 crystal growth fluxing agent is characterized in that the Al-doped CsLiB6O10 crystal growth fluxing agent is a fluxing agent of a Cs2O-Li2O-MoO3 system; the mol ratio of Cs2O to Li2O to MoO3 in the system is 1 to (0.8 to 1.2) to (1.6 to 2.0). The invention further provides an Al-doped CsLiB6O10 crystal growth method utilizing the fluxing agent. According to a novel fluxing agent system provided by the invention, the growth temperature of a crystal can be effectively reduced and a temperature range is 800 DEG C to 820 DEG C; a growth solution is clear and transparent and a crystal growth condition is easy to observe in real time. The volatility of the system can be remarkably reduced and the stability of a growth system is improved; a floating crystal is prevented from forming and the crystal growth success rate is improved. The viscosity of the solution is remarkably reduced and solute transportation is facilitated; the crystal is easy to grow and almost no inclusions are generated.

Description

technical field [0001] The invention belongs to the field of optical materials, and in particular relates to a method for growing nonlinear optical crystals. Background technique [0002] Cesium lithium borate (CsLiB 6 o 10 , referred to as CLBO) crystal is a nonlinear optical crystal material with excellent comprehensive performance discovered in the 1990s. The crystal has the advantages of large nonlinear optical coefficient and phase matching allowable angle, small walk-off angle, large temperature bandwidth and spectral bandwidth, high laser damage threshold, and wide light transmission range. CLBO can realize the double frequency, triple frequency, quadruple frequency and quintuple frequency output of Nd:YAG laser 1064nm laser, especially in the quadruple frequency and quintuple frequency output, so the crystal is used in the field of solid-state laser frequency conversion with broadly application foreground. CLBO belongs to the tetragonal crystal system, a molten c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B9/12C30B29/10G02F1/355
CPCC30B9/12C30B29/10G02F1/3551
Inventor 胡章贵朱显超涂衡
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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