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Top seed solution growth reentrance technology in fluxing agent growth method

A technology of flux and seed crystal, applied in the field of functional crystal materials, can solve problems such as difficulty in directly obtaining high-quality seed crystals

Active Publication Date: 2009-02-11
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Seed crystals are easy to introduce local stress during orientation and cutting, so it is difficult to directly obtain high-quality seed crystals without macroscopic defects and uniform transparency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: RE 1-x :KLu x (WO 4 ) 2 Crystal preparation. RE=Nd, Yb, Ho or Tm and other activated rare earth ions.

[0013] Use WO 3 、KCO 3 、Lu 2 o 3 and RE 2 o 3 As the initial raw material, according to the chemical equation:

[0014] K 2 CO 3 +2WO 3 →K 2 W 2 o 7 +CO 2 ↑

[0015] K 2 CO 3 +4WO 3 +xLu 2 o 3 +(1-x)RE 2 o 3 →2RE 1-x :KLu x (WO 4 ) 2 +CO 2

[0016] Wherein RE=Nd, Yb, Ho or Tm, X=90at%-99.95at%.

[0017] Place the raw materials configured in molar ratios into a platinum crucible, melt them at a temperature of 1060°C for 10 hours, and keep them warm for two days to fully melt the raw materials. In order to fully melt and mix the melt, stir for 12 hours. Use the seed crystal test method to measure the saturation point temperature of the melt. When the temperature is 3°C higher than the saturation point, the seed crystal is lowered 3mm below the liquid surface, and the c-direction seed crystal is used to grow KLuW series crystal...

Embodiment 2

[0018] Example 2: GaPO 4 Crystal preparation

[0019] Use Ga 2 o 3 , 2NH 4 h 2 PO 4 , Li 2 CO 3 , and MoO 3 As the initial raw material, according to the chemical equation:

[0020] Ga 2 o 3 +2NH 4 h 2 PO 4 =2GaPO 4 +2NH 3 ↑+3H 2 O↑

[0021] Li 2 CO 3 +3MoO 3 = Li 2 Mo 3 o 10 +CO 2

[0022] Place the raw materials configured in molar ratios into a platinum crucible, melt them at a temperature of 1020°C for 10 hours, and keep them warm for two days to fully melt the raw materials. In order to fully melt and mix the melt, stir for 12 hours. The saturation point temperature of the melt is measured by the seed crystal test method, and the seed crystal is lowered 3mm below the liquid surface when the temperature is 3°C higher than the saturation point temperature, and the c-direction seed crystal is used to grow GaPO 4 Crystal, after 7 days, lift the seed crystal up 2-4 mm, but do not lift it from the liquid surface, continue to grow the crystal, lift the...

Embodiment 3

[0023] Example 3: Ga 3 PO 7 Crystal preparation.

[0024] Use Ga 2 o 3 , 2NH 4 h 2 PO 4 , Li 2 CO 3 , and MoO 3 As the initial raw material, according to the chemical equation:

[0025] 3Ga 2 o 3 +2NH 4 h 2 PO 4 = 2Ga 3 PO 7 +2NH 3 ↑+3H 2 O↑

[0026] Li 2 CO 3 +3MoO 3 = Li 2 Mo 3 o 10 +CO 2

[0027] Place the raw materials configured in molar ratios into a platinum crucible, melt them at a temperature of 1020°C for 10 hours, and keep them warm for two days to fully melt the raw materials. In order to fully melt and mix the melt, stir for 12 hours. The temperature of the saturation point of the melt is measured by the seed crystal test method. When the temperature is 5°C higher than the saturation point, the seed crystal is lowered 3mm below the liquid surface, and the c-direction seed crystal is used to grow Ga 3 PO 7 Crystal, after 7 days, lift the seed crystal up 2-4 mm, but do not lift it from the liquid surface, continue to grow the crystal, l...

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Abstract

The invention provides a top seed reentry technique in flux growth, which belongs to the technical field of functional crystal materials. The top seed reentry technique is characterized in that: (1) a well processed seed crystal is immerged into the solution for crystal growth at a temperature of 3 to 5 DEG C above the saturation temperature of the solution for crystal growth; (2) the temperature of the solution for crystal growth is reduced to the saturation point, afterwards, the crystal grows for 5 to 7 days with a cooling rate of 0.5 DEC C each day, and a little crystal with regular shape is fabricated, then the little crystal is up-lifted for 2 to 4 millimeters without leaving the surface of the solution for crystal growth; (3) the little crystal with regular shape obtained in step (2) is immerged into the solution for crystal growth again as a seed crystal for a new growth until a crystal accorded with the requirement is fabricated; (4) the crystal is lifted off the surface of the solution after the fabrication is finished, the temperature is reduced at the rate of 4 DEG C each hour. When the temperature reaches 200 DEG C, the crystal is cooled to room temperature by natural. The top seed reentry technique has the advantages of simple preparation process, short fabrication cycle, and good stability, and the crystal grown has small seed crystal recovery area and high optical quality.

Description

technical field [0001] The invention relates to a top seed crystal reentrant technology in a flux growth method, and belongs to the technical field of functional crystal materials. Background technique [0002] The top seed rotation pulling technology in the flux growth crystal combines the flux seed rotation method with the melt pulling method, which not only grows the crystal faster, but also avoids the thermal stress and the stress added to the crystal by the solidification of the flux. It is a method that is often used at present. However, the top seed crystal method generally has relatively high requirements on the seed crystal. Firstly, the size should not be too small, and secondly, the quality requirement is very high. The seed crystal is easy to introduce local stress during the process of orientation and cutting, so it is difficult to directly obtain a high-quality seed crystal with no macroscopic defects and uniform transparency. Contents of the invention [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B15/00C30B9/00
Inventor 王继扬李静张建秀
Owner SHANDONG UNIV
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