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Molten salt growth method of barium borophosphate monocrystal

A technology of barium borophosphate and growth method, applied in the directions of single crystal growth, single crystal growth, crystal growth, etc., can solve the problem of single crystal preparation that has not yet been reported, and achieves easy processing and storage, good for mass transfer, and high hardness. Effect

Inactive Publication Date: 2003-02-05
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

But so far, BaBPO 5 The preparation of single crystal has not been reported yet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Barium borophosphate (BaBPO 5 ) compound synthesis:

[0032] Sintering is carried out at a high temperature of 900°C by a solid-state synthesis method, and its chemical equation is: [(7) reaction formula]

[0033] 59.19 g (0.3 mol) BaCO 3 , 18.55 grams (0.3mol) H 3 BO 3 , 34.51 grams (0.3mol) NH 4 h 2 PO 4 Put it into a mortar, mix and carefully grind it, then put it into an open platinum crucible of Φ60mm×60mm, press it tightly, put it into a muffle furnace, and slowly raise it to 500°C with a heating rate of 2°C / hour and a constant temperature of 24 Hours, take out the crucible after cooling, the sample is relatively loose at this time, then take out the sample and grind it evenly again, then put it in the crucible, keep the temperature in the muffle furnace at 900°C for 24-48 hours, at this time the sample is agglomerated. At this time, take it out, put it into a mortar, mash and grind it to get barium borophosphate (BaBPO5 ) compounds. Carry out X-ray ...

Embodiment 2

[0042] Preparation of BPO 4 -LiF flux: use analytically pure H 3 BO 3 , NH 4 h 2 PO 4 and LiF according to the following proportioning and the synthetic BaBPO of embodiment 1 [(7) reaction formula] 5 Mixing, its mixing molar ratio is: BaBPO 5 :H 3 BO 3 : NH 4 h 2 PO 4 : LiF=1:0.8:0.8:0.3, put it into a platinum crucible with an opening of Φ80mm×60mm, put the crucible into a single crystal growth furnace, seal the opening at the top of the furnace with insulating material, and place the top of the furnace and the center of the crucible Leave a small hole in the corresponding place for the seed rod to enter and exit, heat up to 1050°C at a heating rate of 2°C / hour, and quickly cool down to 920°C (5°C above the saturation temperature) after constant temperature for 24 hours, and cut along the c-axis BaBPO 5 The seed crystal is fixed on the lower end of the seed rod with a platinum wire, and the seed crystal is introduced into the crucible from the small hole on the to...

Embodiment 3

[0044] Homemade Li 4 P 2 o 7 Flux: use analytically pure NH 4 h 2 PO 4 and Li 2 CO 3 Mix according to molar ratio, and its molar ratio is: NH 4 h 2 PO 4 : Li 2 CO 3 = 1:1, after mixing and grinding, sintering at a temperature of 650-700°C for 24 hours to make Li 4 P 2 o 7 flux;

[0045] Will homemade Li 4 P 2 o 7 Flux and the BaBPO synthesized by the (6) reaction formula of embodiment 1 5 Mix according to the following molar ratio, BaBPO 5 : Li 4 P 2 o 7 = 1:1, after mixing evenly, put it into a platinum crucible with an opening of Φ80mm×60mm, put the crucible into a vertical heating furnace, seal the opening at the top of the furnace with insulating material, and place it between the top of the furnace and the center of the crucible Leave a small hole in the corresponding place for the seed rod to enter and exit, heat up to 1000°C at a heating rate of 8°C / hour, and quickly cool down to 825°C (3°C above the saturation temperature) after constant temperatu...

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Abstract

The molten salt growing method of barium borophosphate meonocrystal includes the following steps: 1). uniformly mixing barium borophosphate and flux according to a certain ratio, heating to 900 deg.C-1100 deg.C, after thermostatic process cooling to 2-10 deg.C above saturation temp. to obtain mixed melt containing barium borophosphate and flux, the flux is BPO4-R system or Li4P2O7 flux, their mole ratio: barium borphosphate: BPO4-R system flux=1:0.2-1.5:0.1-0.6; and barium borophosphate: Li4P2O7 flux=1:0.2-1.6; and 2). placing the inoculating crystal mounted on the inoculating crystal bar in 0-100 rpm, cooling to saturation temp., slowly temp.-lowering to obtain required crystal, lifting said crystal body from level, reducing to room temp. so as to obtain the invented barium borophosphate monocrystal.

Description

technical field [0001] The present invention relates to the growth method of single crystal, especially barium borophosphate (BaBPO 5 ) single crystal molten salt growth method. Background technique [0002] Borates such as BaB 2 o 4 , LiB 3 o 5 , phosphates such as KTiOPO 4 It has been widely used in the field of electro-optic. Having both boroxy and phosphooxy groups in one crystal may lead to functional materials with new properties. Until now, there have been few reports on functional materials with both boron-oxygen and phosphorus-oxygen groups. [0003] German Z.Anorg.Allg.Chem. magazine (Vol345,225-229,1966) reported barium borophosphate BaBPO 5 The presence of a compound indicates that the compound is a non-isotropic melting compound. J.SolidState Chem. Magazine (Vol135, 43-51, 1998) of the United States reported the determination of BaBPO by powder X-ray diffraction 5 Crystal structure, the crystal belongs to the hexagonal system, P3 1 21 space group, its...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B15/00C30B29/14
Inventor 吴以成潘世烈傅佩珍陈创天
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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