Synthesis method for selenium germanium gallium barium polycrystal and growth method for selenium germanium gallium barium monocrystal

A technology of synthesis method and growth method, which is applied in the field of high-performance nonlinear optical crystals, can solve the problems of invalid crystal nuclei and uncertain growth direction of single crystal, non-stoichiometric ratio and low yield, so as to improve yield and avoid Volatile, avoid explosion effect

Active Publication Date: 2019-08-20
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

[0005] The present invention aims to solve the technical problems of low non-stoichiometric ratio and low yield of the existing selenium-germanium-gallium-barium polycrystal synthesis and the technical problems that invalid crystal nuclei are easily f

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0025] Example 1, Polycrystalline synthesis experiment one of selenium germanium gallium barium

[0026] The raw materials used are barium (Ba), gallium (Ga), germanium (Ge), and selenium (Se) all of 6N grade. When compounding, the molar ratio of each raw material is barium: gallium: germanium: selenium = 1:2:1: 6. According to the above ratio, appropriately enrich selenium (excess 0.5%-1.5%) for ingredients: barium 35.082g, gallium 35.626g, germanium 18.553g selenium 122.501g.

[0027] The synthesis process steps are as follows:

[0028] 1. Reaction vessel cleaning and drying

[0029] Soak and rinse the quartz tube and PBN boat with tap water, soak it in aqua regia for 24 hours, then rinse with tap water to neutrality, place it in an ultrasonic cleaning tank, shake for 30 minutes, rinse with deionized water repeatedly, and then use high purity Rinse with alcohol and put it in a 100℃ oven to dry for later use.

[0030] 2. Loading

[0031] First put the weighed barium, gallium and germa...

Example Embodiment

[0035] Example 2, Polycrystalline synthesis experiment two of selenium germanium gallium barium

[0036] The raw materials used are barium (Ba), gallium (Ga), germanium (Ge), and selenium (Se) all of 6N grade. When compounding, the molar ratio of each raw material is barium: gallium: germanium: selenium = 1:2:1: 6. According to the above ratio, appropriately enrich selenium (excess 0.5%-1.5%) for ingredients: barium 17.541g, gallium 17.813g, germanium 9.277g selenium 60.823g.

[0037] The synthesis process steps are as follows:

[0038] 1. Reaction vessel cleaning and drying

[0039] Soak and rinse the quartz tube and PBN boat with tap water, soak it in aqua regia for 24 hours, then rinse with tap water to neutrality, place it in an ultrasonic cleaning tank, shake for 30 minutes, rinse with deionized water repeatedly, and then use high purity Rinse with alcohol, dry it in an oven at 100℃ for later use.

[0040] 2. Loading

[0041] First put the weighed barium, gallium and germanium int...

Example Embodiment

[0045] Example 3, single crystal growth experiment of selenium germanium gallium barium

[0046] The single crystal growth method of selenium germanium gallium barium of this embodiment includes the following steps:

[0047] 1. Soak the PBN crucible and quartz tube for crystal growth with aqua regia, then clean and dry with ultrapure water; the PBN crucible for single crystal growth is cylindrical with a seed crystal trap, the length of the PBN crucible is 200mm, the inner diameter is 30mm, and the front end The inner diameter of the seed crystal well is 2mm and the length is 30mm;

[0048] 2. Add 300 grams of polycrystalline selenium, germanium, gallium, and barium to the crucible, then place the crucible vertically in the quartz tube, and vacuum the quartz tube to 10 -4 Pa, and finally seal the quartz tube with a hydrogen-oxygen flame;

[0049] 3. Put the fused quartz tube into a vertical dual-temperature zone tubular resistance furnace. The growth furnace consists of high temperatu...

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Abstract

The invention discloses a synthesis method for a selenium germanium gallium barium polycrystal and a growth method for a selenium germanium gallium barium monocrystal. The growth of the polycrystal comprises the following steps: putting elemental Ga, elemental Ba and elemental Ge into a PBN boat; then placing the PBN boat at one end of a quartz tube and placing elemental Se at the other end of thequartz tube; conducting vacuumizing, and then carrying out heat sealing; and then putting the quartz tube into a horizontal double-temperature-region resistor furnace for synthesizing, so as to obtain a high-purity single-phase selenium germanium gallium barium polycrystal raw material, wherein the yield of the raw material is greater than 99%. The growth of the selenium germanium gallium bariummonocrystal comprises the following steps: adding the selenium germanium gallium barium polycrystal into a crystal growth crucible and vertically placing the crystal growth crucible into a quartz tube; conducting vacuumizing, and then carrying out heat sealing; and then putting the quartz tube into a vertical double-temperature-region resistor furnace, so as to obtain the selenium germanium gallium barium monocrystal after the growth of the monocrystal is finished. The selenium germanium gallium barium monocrystal obtained by the method disclosed by the invention has the advantages of few defects, high infrared band transmission rate and the like and can be used as a far infrared laser frequency conversion material.

Description

technical field [0001] The invention belongs to the technical field of high-performance nonlinear optical crystals, in particular, the invention relates to polycrystal synthesis and single crystal growth methods of mid- and far-infrared nonlinear optical materials. Background technique [0002] The all-solid-state laser with infrared nonlinear optical crystal as the key core component can generate mid-to-far infrared laser in the 3-17μm band through frequency conversion under the near-infrared laser pump. fields have a wide range of applications. Selenium germanium gallium barium, the molecular formula is BaGa 2 GeSe 6。 , is a new type of infrared nonlinear optical crystal with excellent performance, and its nonlinear optical effect is large (d 11 =49pm / V), high transmittance in the middle and far infrared range, large birefringence, high laser damage threshold, and has important application value. [0003] At present, the method for synthesizing selenium-germanium-galli...

Claims

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Application Information

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IPC IPC(8): C30B29/46C30B28/02C30B11/00
CPCC30B11/00C30B28/02C30B29/46
Inventor 姚吉勇郭扬武李壮罗晓宇
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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