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Method for preparing potassium titanium oxide phosphate crystal by liquid phase coprecipitation sythesis of growth material

A co-precipitation method and co-precipitation technology, applied in the direction of single crystal growth, crystal growth, single crystal growth, etc., can solve the problem of crystals prone to scattering particles, and achieve the effect of improving crystal quality

Inactive Publication Date: 2009-07-01
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

Generally, solid-phase synthesis is used to grow raw materials, and crystal defects such as scattering particles are prone to appear in the grown crystals.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Molar ratio TiCl 4 :KH 2 PO 4 :K 2 CO 3 =0.1:1.26:0.27; 20ml, 5mol / L TiCl 4 Dilute to Ti in an ice-water bath 4+ 500ml solution A with an ion concentration of 0.1mol / L;

[0019] Weigh KH 2 PO 4 172.21g and K 2 CO 3 37.42 g, KH with deionized water 2 PO 4 and K 2 CO 3 Dissolve and prepare 1800ml clear solution B;

[0020] In an ice-water bath, slowly add solution A to clear solution B to obtain a white emulsion, and age the emulsion for 12 hours under continuous stirring with a magnetic stirrer, and then use a heating magnetic stirrer to evaporate the emulsion until it becomes a paste;

[0021] Put it in an oven, dry it at 140°C for 10 hours, take it out, grind it thoroughly in an agate grinder and mix it evenly, put it into a platinum crucible of φ60×70mm, and first sinter it in a muffle furnace at a constant temperature of 600°C for 6 hours to get Sintered body. After cooling, put it into a vertical resistance wire single crystal growth furnace, rapidly...

Embodiment 2

[0023] Mole ratio Ti(OC 4 h 9 ) 4 :KH 2 PO 4 :K 4 P 2 o 7 =0.18:0.93:0.07 Measure 62ml tetrabutyl titanate Ti(OC 4 h 9 ) 4 Mix it with 28.6ml of ethanol to prepare a tetrabutyl titanate-ethanol solution with a volume ratio of 5:2, and stir it magnetically at room temperature for 35 minutes. At this time, the solution is a uniform and transparent solution A. Weigh KH 2 PO 4 126.49g and K 4 P 2 o 7 23.12 g, KH with deionized water 2 PO 4 and K 4 P 2 o 7 Dissolve to make 1000ml clear solution B. Slowly add solution A to solution B to prepare a white emulsion. After aging for 12 hours under continuous stirring with a magnetic stirrer, use a heated magnetic stirrer to evaporate the emulsion to a paste state. Put it in an oven, dry it at 160°C for 10 hours, take it out, grind it thoroughly in an agate grinder and mix it evenly, put it into a platinum crucible with a diameter of 50×60mm, and first sinter it in a muffle furnace at a constant temperature of 600°C fo...

Embodiment 3

[0025] Molby H 2 TiO 3 :KH 2 PO 4 :K 2 HPO 4 =0.1:0.275:0.175. H 2 TiO 3 Ti 4+ 500ml solution A with an ion concentration of 0.1mol / L. Weigh KH 2 PO 4 37.41g and K 2 HPO 4 30.46 g, KH with deionized water 2 PO 4 and K 2 HPO 4Dissolved to make 500ml clear solution B. In an ice-water bath, slowly add the diluent A to the clear solution B to obtain a white emulsion, and age the emulsion for 12 hours under continuous stirring with a magnetic stirrer, and then evaporate the emulsion to dryness with a heated magnetic stirrer until it becomes a paste. Put it in an oven, dry it at 150°C for 10 hours, take it out, grind it thoroughly in an agate grinder and mix it evenly, put it into a platinum crucible of φ50×50mm, and first sinter it in a muffle furnace at a constant temperature of 600°C for 6 hours to get Sintered body. After cooling, put it into a vertical resistance wire single crystal growth furnace, rapidly raise the temperature to 1000°C and keep the temperat...

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Abstract

The invention discloses a method for preparing KTP crystals by synthesizing a growth material through liquid phase coprecipitation, which comprises the following steps: 1) a TiCl4 solution is added into a clear solution consisting of KH2PO4, K2CO3 and deionized water in an ice-water bath to form a milky coprecipitation compound, the mol ratio of TiCl4 to KH2PO4 to K2CO3 is 0.1-0.303: 0.86-1.36: 0.125-0.31, and the milky coprecipitation compound is dried, ground into powder, and placed into a platinum crucible to be sintered to obtain a sintered body; and 2) the sintered body obtained in step 1) is melted at the temperature of 1,000 DEG C, keeps the constant temperature, and is cooled to be between 10 and 20 DEG C above a saturation temperature to obtain a melt, and seed crystals enter the melt for remelting and then are subjected to crystal growth to obtain the KTP crystals. The method adopts a liquid phase to synthesize a growth raw material of the KTP crystals and then performs the sintering, and the obtained crystals have good optical homogeneity and no crystal defects such as scattering particles and so on.

Description

technical field [0001] The invention belongs to the preparation method of nonlinear optical crystal potassium titanyl phosphate (KTP), in particular to a method for preparing nonlinear optical crystal KTP by synthesizing growth material with liquid phase co-precipitation Background technique [0002] Potassium titanyl phosphate (KTP) crystal is a kind of nonlinear optical crystal with excellent performance. It not only has high nonlinear optical coefficient, high thermal conductivity, high laser damage threshold, small mismatch degree and Good walk-off angle, stable chemical and mechanical properties, not easy to deliquescence, and the crystal surface is easy to polish. The frequency doubling efficiency of the crystal from 1064nm to 532nm can reach 80%. It can be widely used in the production of components such as frequency doubling, frequency mixing, electro-optical modulation, optical parametric oscillation and optical waveguide. [0003] KTP crystals melt at about 1170°...

Claims

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Application Information

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IPC IPC(8): C30B29/22C30B29/14C30B11/00
Inventor 胡章贵胡静
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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