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Compound ammonium fluoroborate, nonlinear optical crystal of ammonium fluoroborate, and preparation method and use thereof

a technology of ammonium fluoroborate and ammonium fluoroborate, which is applied in the direction of polycrystalline material growth, borates, instruments, etc., can solve the problems of limited application of cbo and clbo crystals, inability to achieve phase matching of lbo crystals, etc., to achieve long growth cycle of crystals, high growth rate, and easy growth

Active Publication Date: 2020-05-28
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0036]d. adding 10-100 mL of a solvent to the container in step c, then subjecting the mixture to ultrasonication to make the mixture mix and dissolve thoroughly, adjusting the pH value of the mixture to pH=1-11, performing filtration with a qualitative filter paper, then sealing the container with a polyvinyl chloride film in which several small holes are punched to adjust the volatilization rate of the solvent in the solution, and placing the container into a static environment without shaking, pollution and air convection, and leaving the mixture to stand at room temperature to allow the crystal to grow, so as to obtain the nonlinear optical crystal of NH4B4O6F with a size of 1-20 mm at the end of the crystal growth; wherein the solvent is deionized water, anhydrous ethanol, N,N-dimethylformamide, N,N-dimethylacetamide or hydrofluoric acid.
[0043]With the method for preparing the nonlinear optical crystal of ammonium fluoroborate of the present invention, the centimeter-sized nonlinear optical crystal of NH4B4O6F can be obtained and the crystal has no obvious layered growth habit. When a large-sized crucible or container is used and the growth cycle of the crystal is prolonged, the corresponding large-sized nonlinear optical crystal of NH4B4O6F can be obtained. During the growth of the nonlinear optical crystal of NH4B4O6F, the crystal is easy to grow up, transparent and with out inclusion, and has the advantages of high growth rate, low cost, and easy to obtain large-sized crystals and so on.
[0044]The large-sized nonlinear optical crystal of NH4B4O6F obtained by the method for preparing the nonlinear optical crystal of ammonium fluoroborate in the present invention can be used as a nonlinear optical device by orienting the raw crystal based on the crystallographic data of the crystal, cutting the crystal according to the desired angle, thickness and sectional size, and polishing the transmission surface of the crystal. The nonlinear optical crystal of NH4B4O6F has the advantages of a wide transmission region, stable physical and chemical properties, a high mechanical hardness, hard to break and deliquesce, easy to cut, polish and preserve and so on.

Problems solved by technology

However, LBO crystal is unable to achieve phase matching in the deep-ultraviolet region due to its relatively small birefringence (Δn=0.04-0.05) and the shortest second harmonic wavelength is 276 nm.
Similar to LBO crystal, CBO and CLBO crystals also have limited applications in the deep-ultraviolet region due to the relatively small birefringence.
Although BBO crystal has a large frequency-doubling coefficient and a large birefringence, its relatively high ultraviolet absorption cutoff edge (189 nm) and the shortest second harmonic wavelength of 204.8 nm limit its application in the deep-ultraviolet region.
KBBF can output a frequency-sextupled light from a 1064 nm fundamental wavelength directly; however, it is difficult to grow a large-sized crystal due to the layered growth habit of KBBF, which limits its application to some extent.

Method used

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  • Compound ammonium fluoroborate, nonlinear optical crystal of ammonium fluoroborate, and preparation method and use thereof
  • Compound ammonium fluoroborate, nonlinear optical crystal of ammonium fluoroborate, and preparation method and use thereof
  • Compound ammonium fluoroborate, nonlinear optical crystal of ammonium fluoroborate, and preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

Preparation

[0051]The compound NH4B4O6F was synthesized by the solid phase reaction process based on the reaction equation NH4F+2B2O3→NH4B4O6F.

[0052]NH4F and B2O3 were mixed uniformly at a molar ratio of 1:1.5 and placed into a Φ10 mm quartz tube. The quartz tube was vacuumized to reach a vacuum degree of 1×10−3 Pa and sealed with a flame gun, and then placed into a muffle furnace. The temperature was raised to 400° C. at a rate of 30° C. / h and kept for 24 h and then reduced to 30° C. at a rate of 6° C. / h, and the quartz tube was opened to obtain the compound NH4B4O6F.

example 2

Preparation

[0053]The compound NH4B4O6F was synthesized by the solid phase reaction process based on the reaction equation NH4F+4H3BO3→NH4B4O6F+6H2O↑.

[0054]NH4F and H3BO3 were mixed uniformly at a molar ratio of 1:3.5 and placed into a hydrothermal reactor having a volume of 23 mL and lined with polytetrafluoroethylene. The hydrothermal reactor was screwed tightly to be sealed and then was placed into a drying oven. The temperature was raised to 220° C. at a rate of 35° C. / h and kept for 24 h and then reduced to 30° C. at a rate of 6° C. / h, and the hydrothermal reactor was opened to obtain the compound NH4B4O6F.

Example 3: Synthesis of the Nonlinear Optical Crystal of NH4B4O6F by the Room Temperature Solution Method

[0055]The compound NH4B4O6F was synthesized according to the specific operation steps in Example 1 based on the reaction equation NH4F+2B2O3→NH4B4O6F.

[0056]The resultant compound NH4B4O6F was sealed in a hydrothermal reactor and then the hydrothermal reactor was placed into...

example 25

[0143]The NH4B4O6F crystal obtained in any one of Examples 1-24 was processed in the direction of phase matching, and placed in position 3 as shown in FIG. 5. A Q-switched Nd:YAG laser is used as a light source at room temperature, and the incident wavelength is 1064 nm. The Q-switched Nd:YAG laser 1 emits an infrared beam 2 with a wavelength of 1064 nm, which is then transmitted to an NH4B4O6F crystal 3, thus generating a green frequency-multiplied light with a wavelength of 532 nm, and the intensity of the output beam is about 3 times of that from KDP in the same condition.

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Abstract

A compound ammonium fluoroborate, a nonlinear optical crystal of ammonium fluoroborate, and a preparation method and use thereof; the compound has the chemical formula of NH4B4O6F with a molecular weight of 176.28, and is prepared by a solid phase reaction process; the crystal has the chemical formula of NH4B4O6F with a molecular weight of 176.28, belongs to the orthorhombic system, and has a space group of Pna21 and the following unit cell parameters: a=7.615(3) Å, b=11.207(4) Å, c=6.604(3) Å, Z=4, V=563.6 Å3. The nonlinear optical crystal can be obtained by the method of the present invention. The present invention provides uses of the nonlinear optical crystal in producing harmonic light and a deep-ultraviolet frequency-multiplied light below 200 nm; and in making a frequency multiplication generator, a frequency up or down converter or an optical parametric oscillator.

Description

CROSS REFERENCE TO RELATED APPLICATIONS[0001]This application is the national phase entry of International Application No. PCT / CN2017 / 074336, filed on Feb. 22, 2017, which is based upon and claims priority to Chinese Patent Application No. 201611128283.3, filed on Dec. 9, 2016, the entire contents of which are incorporated herein by reference.TECHNICAL FIELD[0002]The present invention relates to a compound ammonium fluoroborate NH4B4O6F, a nonlinear optical crystal of ammonium fluoroborate NH4B4O6F, and a preparation method and use thereof.BACKGROUND[0003]Recently, with the strong demand for the deep-ultraviolet laser source (generally refers to the laser source emitting a laser with a wavelength of shorter than 200 nm) of 193 nm lithography technology, micro-nano fine laser processing, and modern instruments such as ultra-high energy resolution photoelectron spectrometer and photoelectron emission microscopy, developing an all-solid-state deep-ultraviolet laser source has become a ...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C01B35/06C30B7/10C30B7/14C30B9/12C30B11/00C30B29/12G02F1/355G02F1/35G02F1/37G02F1/39
CPCC30B7/10C30B11/00C01P2002/78C01P2002/77C30B29/12G02F1/39G02F2001/354G02F1/37C01P2002/85G02F1/3551C01P2002/76C01B35/06C01P2002/74C30B9/12C01P2002/82C30B7/14G02F1/353C01B35/061C01P2002/72G02F1/392C01B35/12G02F1/35G02F1/354
Inventor PAN, SHILIESHI, GUOQIANGZHANG, FANGFANGHOU, XUELING
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI