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Fluxing medium growing method for fluoroboric acid calcium non-linear optical crystal

A nonlinear optics and growth method technology, applied in the field of flux growth of calcium fluoroborate nonlinear optical crystals, can solve problems such as the growth and other properties of Ca5B3O9F crystals that have not yet been seen, achieve easy processing and storage, reduce growth temperature, fast growth effect

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

However, there have been no reports on the crystal growth and other properties of Ca5B3O9F

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Ca 5 B 3 o 9 Synthesis of F compound:

[0023] 1) Sintering is carried out at a high temperature of 1000°C by a solid-state synthesis method, and its chemical formula is: 9CaCO 3 +6H 3 BO 3 +CaF 2 →2Ca 5 B 3 o 9 F+9CO 2 ↑+9H 2 O↑[(2) reaction formula]

[0024] 150 g (1.5 mol) CaCO 3 , 61.8 grams (1mol) H 3 BO 3 , 13.26 grams (0.17mol) CaF 2Put 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 50°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, then put it in the crucible, keep the temperature in the muffle furnace at 1000°C for 24-72 hours, then the sample shrinks. At this point, take it out, put it in a mortar, mash and grind it to get Ca 5 B 3 o 9 F compound. X-ray analysis...

Embodiment 2

[0031] The synthetic Ca of embodiment 1 [(2) reaction formula] 5 B 3 o 9 Compound F is mixed with flux, and its mixing mass ratio is: Ca 5 B 3 o 9 F: Flux (LiF—CaO—B 2 o 3 ) system flux=1:0.1, wherein the molar ratio of the three substances in the flux system is LiF:CaO:B 2 o 3 = 1:0:0, namely Ca 5 B 3 o 9 F: LiF=1:0.1; Put the prepared raw materials into a platinum crucible with a Φ40mm×40mm opening, put the crucible into a single crystal growth furnace, seal the opening at the top of the furnace with insulating material, and connect the top of the furnace with the crucible Leave a small hole at the corresponding position of the center for the access of the seed rod, raise the temperature to 1170°C at a rate of 100°C / hour, and quickly cool down to 1135°C (10°C above the saturation temperature) after constant temperature for 24 hours to obtain fluorine-containing Mixed melt of calcium borate and flux;

[0032] Ca 5 B 3 o 9 The F seed crystal is fixed on the lowe...

Embodiment 3

[0034] The synthetic Ca of embodiment 1 [(2) reaction formula] 5 B 3 o 9 Compound F is mixed with flux, and its mixing mass ratio is: Ca 5 B 3 o 9 F: flux system (LiF—CaO—B 2 o 3 )=1:0.1, wherein the molar ratio of the three substances in the flux system is LiF: CaO: B 2 o 3 =0.7:0.2:0.1, put the prepared raw materials into a platinum crucible with an opening of Φ40mm×40mm, put the crucible into a single crystal growth furnace, seal the opening at the top of the furnace with insulating material, and place a gap between the top of the furnace and the center of the crucible Leave a small hole at the corresponding position for the seed rod to enter and exit, heat up to 1200°C at a heating rate of 70°C / hour, and quickly cool down to 1150°C (5°C above the saturation temperature) after constant temperature for 10 hours to obtain fluorine-containing boric acid Mixed melt of calcium and flux;

[0035] Ca 5 B 3 o 9 The F seed crystal is fixed on the lower end of the seed ro...

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Abstract

The invention relates to a preparation method of a calcium fluoborate nonlinear optic crystal; calcium fluoborate and a flux are mixed, and heated to 900 - 1170 DEG C at a heating rate of 20- 100 DEG C / hour, and kept in constant temperature for 5- 50 hours, and then cooled to a temperature 2- 10 DEG C higher than saturate temperature, and a mixing melt of calcium fluoborate and the flux is obtained; the mass ratio between calcium fluoborate and the flux is 1: 0.1-1, and the flux is a LiF-CaO-B2O3 system, wherein the molar ratio of LiF: CaO: B2O3 is 1-0.5 : 0-0.37 : 0-0.2; a crystallon arranged on a crystallon rod is dropped to the mixing melt prepared through the steps and cooled to saturate temperature at the same time, the crystallon rod is rotated at a rotating rate of 5-50 revolutions / minute, then the temperature is slowly reduced at a rate of 0.2-3 DEG C / day, the obtained crystal is lifted from the liquid surface and cooled to room temperature at a cooling rate of 5- 100 DEG C / hour, and the obtained calcium fluoborate is a nonlinear optic crystal. The method has the advantages of simple operation, fast growing speed, easy growing and low cost.

Description

technical field [0001] The invention belongs to a flux growth method for nonlinear optical crystals, in particular to a flux growth method for calcium fluoroborate nonlinear optical crystals. Background technique [0002] Nonlinear optical crystals are a class of crystal materials with nonlinear optical effects such as frequency doubling, frequency mixing, and optical parametric oscillation. Using the frequency doubling effect of the crystal, the frequency of the laser can be changed, and the wavelength range of the laser light source can be broadened, thereby obtaining a new laser light source and making the laser widely used. The all-solid-state blue-green laser system is made of nonlinear optical crystals. It has the advantages of small size, stable light source, and low cost, and has broad application prospects. [0003] At present, the nonlinear optical crystals used to make blue-green laser systems are mainly borates and phosphates. The boronoxy group and phosphorus ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B15/00C30B29/22
Inventor 吴以成陈国军傅佩珍
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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