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Growth method for fluxing medium of boron phosphate single crystal

A growth method, boron phosphate technology, applied in the direction of single crystal growth, single crystal growth, crystal growth, etc., can solve the problems of difficult to grow large-sized transparent crystals, unable to obtain satisfactory optical properties, easy to form inclusions, etc., to achieve UV cut-off The effect of short wavelength, moderate hardness, and not easy to break

Inactive Publication Date: 2009-05-20
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 viscosity of this system is high, and it is impossible to obtain BPO that meets the optical performance test 4 the crystal
In 2004, Li Zhihua et al reported the use of Li 4 P 2 o 7 -Li 2 O-Compound Flux Growth of BPO 4 Crystal method ("Journal of Crystal Growth", 2004, Vol.270, 486-490), but this system still has the disadvantages of high viscosity, easy formation of inclusions, and difficulty in growing large-sized transparent crystals.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Solid phase synthesis of boron phosphate compounds:

[0028] It is synthesized by high-temperature solid-state reaction method, and its chemical reaction equation is:

[0029] NH 4 h 2 PO 4 +H 3 BO 3 =BPO 4 +NH 3 +3H 2 O [reaction formula (1) above]

[0030]Weigh 115.03g (1.0mol) of NH 4 h 2 PO 4 and 61.833g (1.0mol) of H 3 BO 3 Put it into a mortar, mix and grind it thoroughly, then put it into a corundum crucible, slowly raise the temperature to 550°C in a muffle furnace, the heating rate is lower than 30°C / hour, keep the temperature constant for 24 hours, then cool down and take out the crucible, at this time, The sample is loose, take out the sample and re-grind it evenly, then raise the temperature to 800°C-900°C again, and keep the temperature constant for 24-48 hours. Then the temperature is lowered to room temperature, the crucible is taken out, the sample is put into a mortar, crushed and ground to obtain boron phosphate compound powder.

[0031]...

Embodiment 2

[0038] Boron Phosphate Crystal Growth:

[0039] According to boron phosphate: Li 2 O:MoO 3 =1.0:0.2:1.5, adopt the synthetic boron phosphate compound of embodiment 1, select analytically pure Li for use 2 CO 3 、MoO 3 As a flux, weigh 211.56g BPO 4 , 29.56g Li 2 CO 3 , 431.82g MoO 3 , melt the above mixture in batches in φ60×60mm platinum crucibles, then put the crucibles into the crystal growth furnace, cover the opening on the top of the furnace with the furnace cover, and leave a space at the corresponding position between the furnace cover and the center of the crucible for The small hole for the seed rod to enter and exit, while leaving a light hole and an observation hole on both sides of the center of the furnace cover, heat up to complete melting, keep the temperature at a constant temperature for 24 hours to fully homogenize the high-temperature solution, and then cool down to 2°C above the saturation temperature ;Fix the cut boron phosphate seed crystal on the...

Embodiment 3

[0041] Boron Phosphate Crystal Growth:

[0042] According to boron phosphate: Li 2 O:MoO 3 =1.0:1.0:0.2, adopt the synthetic boron phosphate compound of embodiment 1, select analytically pure Li for use 2 CO 3 、MoO 3 As a flux, weigh 211.56g BPO 4 , 147.78g Li 2 CO 3 , 56.56g MoO 3 , melt the above mixture in batches in φ60×60mm platinum crucibles, then put the crucibles into the crystal growth furnace, cover the opening on the top of the furnace with the furnace cover, and leave a space at the corresponding position between the furnace cover and the center of the crucible for The small hole for the seed rod to enter and exit, while leaving a light hole and an observation hole on both sides of the center of the furnace cover, heat up to 800°C, keep the temperature for 24 hours and then drop it to 15°C above the saturation temperature, and place the cut boron phosphate seeds The crystal is fixed on the lower end of the seed rod with a platinum wire, and slowly descends ...

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PUM

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Abstract

The invention relates to a growth method of a fluxing agent of boron phosphate monocrystal, which comprises the steps of: 1) proportionally mixing a boron phosphate compound and the fluxing agent, putting the mixture into platinum crucible, and heating till completely fusing in a crystal growing furnace; and then cooling to the temperature being 2 to 15 DEG C above a saturation temperature, thus obtaining a high temperature melt containing boron phosphate and the fluxing agent; and 2) putting seed crystal loaded on a seed rod into the high temperature melt, keeping constant temperature for 10 to 180 minutes, reducing the temperature to saturation temperature, and rotating the seed rod at the speed of 10 to 50 revolution / minute; and reducing the temperature at the speed of 0.1 to 2 DEG C / day, lifting the crystal from the liquid surface after the crystal grows up, and cooling to room temperature at the speed of 20 to 50 DEG C / hour to obtain the boron phosphate monocrystal. The fluxing agent used by the method can reduce the viscosity of the high temperature melt, is beneficial to melt mass transportation in the process of crystal growth, avoids the formation of inclusions in the crystal, and can stably grow the transparent boron phosphate monocrystal which has cm-level size, short ultraviolet cutoff wavelength and good mechanical processing performance, is not easy to crack, does not absorb moisture, and is easy to be stored.

Description

technical field [0001] The invention belongs to the field of single crystal growth methods, in particular to a flux growth method for boron phosphate single crystals. Background technique [0002] In modern laser technology, the laser wavelengths that can be directly obtained by using laser crystals are limited. Nonlinear optical crystals have attracted much attention because they can effectively broaden the wavelength range of lasers. The use of nonlinear optical crystals to make second harmonic generators, up and down frequency converters, optical parametric oscillators and other nonlinear optical devices is an important means of obtaining new laser light sources. [0003] At present, borate and phosphate nonlinear optical crystals such as BBO, LBO, KTP, and DKDP crystals have attracted much attention due to their excellent nonlinear optical properties. The nonlinear optical properties of the crystal play an important role. In 1934, the German magazine "Zeitschrift fuer...

Claims

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Application Information

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IPC IPC(8): C30B29/14C30B9/00
Inventor 吴以成张书峰张尔攀傅佩珍陈创天
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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