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A high-temperature and high-pressure hydrothermal kettle containing foamed metal crystal parts

A technology of high-temperature, high-pressure water and metal foam, which is applied in the direction of pressure vessels used in chemical processes, can solve the problems of crystal grains blocking the growth of baffle holes, difficult growth of crystal nuclei, and slowing down the convection of the solution in the kettle, so as to promote the growth of crystal grains. Effects of further growth, increase in crystal yield, and increase in crystallization efficiency

Active Publication Date: 2016-07-27
CHINA NONFERROUS METAL (GUILIN) GEOLOGY & MINING CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 2. In hydrothermal crystallization, there is a violent transport process of nutrient salts inside the autoclave. The transport is from the hot end to the cold end of the autoclave, and the nutrient salts are cooled at the cold end and flow back to the hot end. It happens in the condensation process of nutrient salts (some crystals have a reverse temperature coefficient and may crystallize during the heating process). Although today's high-performance autoclaves can accurately control the temperature and widen the temperature difference, it is difficult to achieve amplified condensation (heating ) in the crystallization process section to slow down the convection of the solution in the kettle
[0006] 3. In order to solve the problem of severe convection in the hydrothermal crystallization process, internal baffle equipment has been installed between the dissolution zone and the crystallization zone at home and abroad. The internal baffle slows down the transportation of nutrient salts in a certain sense and enlarges the condensation The crystallization process increases the crystallization amount and the crystal nucleus. However, after the formation of the crystal nucleus, it will migrate to the dissolution zone or the position of the baffle with the force of gravity and transportation, and the utilization rate of the crystal nucleus is not high.
In the actual growth process, it often occurs that the crystal nuclei are difficult to grow (repeatedly dissolving crystals in the kettle), and the crystal grains block the baffle holes and cause growth stagnation.
[0007] 4. It has been reported in the literature to use wound or folded metal sheets, wires, etc. to produce crystallization regions and increase the area of ​​bonding sites. Although it plays the role of accepting crystal grains and slowing down the convection of the solution, the metal sheets and wires are not stable. The density is high, but the unit specific surface area is small, and the utilization rate of the index surface matching the crystal unit cell is still not high; on the other hand, if a large-area metal sheet or wire is used, it will hinder the transportation of nutrients

Method used

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  • A high-temperature and high-pressure hydrothermal kettle containing foamed metal crystal parts
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  • A high-temperature and high-pressure hydrothermal kettle containing foamed metal crystal parts

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Effect test

Embodiment 1

[0031] Embodiment 1: High-temperature and high-pressure hydrothermal kettle containing foamed metal crystallization parts for hydrothermal growth of crystals

[0032] Such as figure 1As shown, the high-temperature and high-pressure hydrothermal kettle containing foamed metal crystal parts according to the present invention includes a kettle body 4 and a kettle cover 3, and the kettle cover 3 is provided with a self-tightening sealed kettle that cooperates with the opening of the inner cavity of the kettle body 4 Plug 1, the kettle body 4 and the kettle cover 3 are connected by fastening bolts 2; a bushing pipe 5 is placed in the inner cavity of the autoclave body 4, and a middle and lower part of the bushing pipe 5 is placed in the center and the edge A perforated baffle 6 (with a porosity of 7-10%), the baffle 6 divides the space inside the liner pipe 5 into a lower dissolution zone 9 and an upper crystallization zone 7 . In the crystallization zone 7, the crystallization pa...

Embodiment 2

[0034] Example 2: Using the device of the present invention to grow scandium-doped zinc oxide single crystal by hydrothermal method

[0035] The crystalline parts are made of nickel foam with the following structural parameters: the pore diameter is 0.1-0.5mm, the porosity is >90%, the through-porosity is 95%, and the volume density is 0.85g / cm 3 .

[0036] In this embodiment, the crystalline part 8 made of nickel foam with the above structural parameters has a continuous tooth-like structure, and the crystalline part 8 is cleaned with absolute ethanol for 5 minutes under ultrasonic conditions, and then washed with 0.1 mol / L hydrochloric acid The solution was washed for 20s, and then washed in 4mol / L KOH solution for 20s, and then vacuum-dried. then press figure 1 The structure of the device shown is to construct the autoclave used in this embodiment, wherein the liner tube 5 adopts the gold liner tube 5 of Φ22 (the inner diameter of the liner tube 5 is 22mm), the precious m...

Embodiment 3

[0039] Embodiment 3: Adopt the device hydrothermal method of the present invention to grow KTP (potassium titanyl phosphate) single crystal

[0040] The crystalline parts are made of silver foam with the following structural parameters: porosity ≥ 85%, number of pores: 80-110PPI, thickness: (0.2-2.5) ± 0.05mm, specific surface area ≥ 10㎡ / g.

[0041] In the present embodiment, the crystalline part 8 made of foamed silver with the above structural parameters is in a disc-shaped structure, specifically, it is arranged in a disc shape from the center of the circle to the outer spiral disk, and the crystalline part 8 made under ultrasonic conditions is used without Wash with water and ethanol for 5 minutes, then wash with 0.1mol / L hydrochloric acid solution for 20s, then wash with 4mol / L KOH solution for 20s, and then vacuum dry. then press figure 1 The structure of the device shown is to construct the autoclave used in this embodiment, wherein the liner tube 5 adopts the gold lin...

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Abstract

The invention discloses a high-temperature and high-pressure hydrothermal kettle containing foamed metal crystallization parts, which includes a hydrothermal reaction vessel placed in the autoclave body. There is a dissolution zone and a crystallization zone in the hydrothermal reaction vessel, and the setting in the crystallization zone is beneficial to A crystalline part for crystal growth, the crystalline part being made of metal foam. By setting crystallization parts made of metal foam in the crystallization area, using the structural characteristics of metal foam such as high specific surface area, a large number of nucleation sites suitable for crystal attachment are generated, and the fine mesh inside the metal foam can play a role Grasp the role of the crystal grains to prevent them from slipping into the dissolution zone. While absorbing the advantages of using metal wires and metal sheets as the crystallization carrier in the traditional temperature difference hydrothermal kettle, it solves the problem that the effective nucleation area is small and the grains that have grown into Defects such as falling, strong convection, and hindered transport greatly increase the crystallization efficiency, promote the further growth of crystal grains, and further increase the crystal yield.

Description

technical field [0001] The invention relates to a device for artificially growing crystals, in particular to a high-temperature and high-pressure hydrothermal kettle containing foamed metal crystal parts. Background technique [0002] The research on the method of artificially growing crystals began as early as the end of the nineteenth century, and has a history of more than one hundred years. The methods for growing single crystals mainly include flux method, hydrothermal method, gas phase method, zone melting method, etc. Among them, water The crystals grown by the thermal method have the characteristics of small thermal stress, small macroscopic defects, good crystal uniformity, and high transmittance. The hydrothermal crystal growth method specifically dissolves the raw material (solute) in the solvent, and takes appropriate measures to cause the supersaturated state of the solution (the saturated vapor pressure of the dilute phase increases), so that the solid phase pa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J3/04
Inventor 任孟德周海涛何小玲张昌龙王金亮曾志平左艳彬李东平吴文渊林峰秦建新
Owner CHINA NONFERROUS METAL (GUILIN) GEOLOGY & MINING CO LTD