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Production method of high temperature covering agent grade boron oxide

A production method and technology of boron oxide, applied in boron oxides, boron oxide compounds, etc., can solve problems such as high vacuum degree is not easy to obtain, small output, unfavorable stable production and product quality control

Active Publication Date: 2018-10-09
广东先导微电子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has the following disadvantages: directly dehydrating boric acid under a vacuum of 0.01-100 Pa will cause boric acid splashing and volatilization of boric acid powder, and the splashed boron oxide will be adsorbed on the inner wall of the glass tube. , Boron oxide will cause crystallization or reaction with the inner wall of the quartz glass tube, resulting in product loss; and for the entire dehydration system, a high vacuum degree of less than 1 Pa is not easy to obtain, and it is difficult to maintain for a long time, which is not conducive to stable production and product quality control
The boron oxide production process adopted by the above methods has technical defects such as high calcination temperature, prone to burning of the crucible, severe boric acid or boron oxide splashing, high vacuum degree requirements, small output, and unstable dehydration effect.

Method used

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  • Production method of high temperature covering agent grade boron oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Dry 400g of boric acid powder with a purity of 5N at 100°C for 24 hours or more in advance, then divide it into two batches and put them into platinum crucibles, adjust the heating power of the intermediate frequency furnace, heat the boric acid to 600°C, and feed the two batches at an interval of 10 minutes . When the boric acid powder in the crucible is all in a transparent molten state and no longer bubbles, put 100g of anhydrous boron oxide with a purity of 5N into it. Adjust the heating power of the intermediate frequency furnace, heat the boron oxide to 900 °C, and calcine for 15 min. Connect the vacuum system, turn on the vacuum switch, turn the valve to 1 / 3, and adjust the induction heating power to the set value. Observe the boiling of the melt, and control the splashing of the melt by controlling the tightness of the bottom valve. Pump the vacuum of the intermediate frequency furnace to below 50 Pa within 40 min, tighten the bottom valve, and continue vacuum...

Embodiment 2

[0029] Dry 500 g of boric acid powder with a purity of 5N at 100°C for 24 hours or more in advance, divide it into two batches and put it into a platinum crucible, adjust the heating power of the intermediate frequency furnace, heat the boric acid to 700°C, and feed the two batches at an interval of 20 minutes . When the boric acid powder in the crucible is all in a transparent molten state and no longer bubbles, put 200g of anhydrous boron oxide with a purity of 5N into it. Adjust the heating power of the intermediate frequency furnace, heat the boron oxide to 950 °C, and calcine for 30 min. Connect the vacuum system, turn on the vacuum switch, turn the valve to 1 / 4, and adjust the induction heating power to the set value. Observe the boiling of the melt, and control the splashing of the melt by controlling the tightness of the bottom valve. Pump the vacuum of the intermediate frequency furnace to below 50 Pa within 50 minutes, tighten the bottom valve, and continue vacuum ...

Embodiment 3

[0031] Dry 600 g of boric acid powder with a purity of 5N at 100°C for 24 hours or more in advance, and then divide it into two batches and put them into platinum crucibles. Adjust the heating power of the intermediate frequency furnace to heat the boric acid to 800°C. 30min. When the boric acid powder in the crucible is all in a transparent molten state and no longer bubbles, drop 300g of anhydrous boron oxide with a purity of 5N into it. Adjust the heating power of the intermediate frequency furnace to heat boron oxide to 1000 °C for 20 min. Connect the vacuum system, turn on the vacuum switch, turn the valve to 1 / 2, and adjust the induction heating power to the set value. Observe the boiling of the melt, and control the splashing of the melt by controlling the tightness of the bottom valve. Pump the vacuum of the intermediate frequency furnace to below 50 Pa within 40 min, tighten the bottom valve, and continue vacuum dehydration for 150 min. Keep the heating power const...

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Abstract

The invention relates to a production method of high temperature covering agent grade boron oxide. The production method comprises following steps: S1, boric acid heating is carried out; S2, anhydrousboron oxide is added; S3, calcining and dehydration are carried out; and S4, casting moulding is carried out. According to the production method, comprehensive consideration of production cost, production period, and product quality stability is adopted, the lowest vacuum degree and the highest dehydration temperature are not adopted, the boron oxide capable of satisfying high temperature covering grade requirements is obtained, and product yield is 95% or higher.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to a production method of high-temperature covering agent grade boron oxide. Background technique [0002] Liquid-enclosed crystal growth method (LEC) is a main method for preparing III-V compound semiconductors (such as gallium arsenide, gallium phosphide, and indium arsenide). Covered with a liquid phase layer to prevent the loss of volatile components of compound semiconductors. The liquid phase layer usually adopts boron oxide with purity ≥ 99.999% and water content ≤ 200ppm. [0003] The preparation method of existing anhydrous boron oxide mainly is following several. [0004] 1. Prepared by two-stage dehydration. Chinese patent application CN200810155689.X proposes a method for preparing high-temperature covering agent-grade boron oxide. In this method, boron oxide is first heated to 400-500°C in air and kept for half an hour; then boron oxide is heated to 1000°C in air ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/10
CPCC01B35/1027C01P2002/82C01P2006/80
Inventor 蔡新志朱刘刘留胡智向黄宇彬
Owner 广东先导微电子科技有限公司
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