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Preparation method of high-purity superfine hafnium boride powder and hafnium boride powder

A technology of hafnium boride and powder, which is applied in the field of hafnium boride preparation, can solve the problems affecting the purity of grain boundaries and the uniform distribution of ceramic structures, and achieve the effects of lowering temperature, avoiding uneven structure and high purity

Inactive Publication Date: 2021-06-08
BEIJING MINING & METALLURGICAL TECH GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the addition of sintering aids may affect the HfB 2 The purity of grain boundaries affects HfB 2 The structure of the ceramic is evenly distributed

Method used

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  • Preparation method of high-purity superfine hafnium boride powder and hafnium boride powder
  • Preparation method of high-purity superfine hafnium boride powder and hafnium boride powder
  • Preparation method of high-purity superfine hafnium boride powder and hafnium boride powder

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preparation example Construction

[0035] A preparation method of high-purity ultrafine hafnium boride powder, comprising the following steps:

[0036] S1: mixing hafnium oxide, a boron source and a carbon source as raw materials, drying and pressing into a block; the boron source is boric anhydride and / or boric acid;

[0037] S2: The block is subjected to primary heat treatment, hot water treatment, and secondary heat treatment in sequence to obtain high-purity ultrafine hafnium boride powder; The temperature is higher than the primary heat treatment temperature.

[0038] Here, "high-purity and ultra-fine" means that the purity of the hafnium boride powder reaches ≥99%, and the particle size reaches 0.1-2 μm.

[0039] The raw materials of the present invention include hafnium oxide (HfO 2 ), boron source and carbon source, wherein boron source is boron anhydride (B 2 o 3 ) and / or boric acid (H 3 BO 3 ), that is, the boron source is B 2 o 3 , or, the boron source is H 3 BO 3 , or, the boron source is ...

Embodiment 1

[0075] A method for preparing high-purity ultrafine hafnium boride powder, comprising the following steps:

[0076] (1) Hafnium oxide powder with a purity of 99.9% and an average particle size of 1 μm, boric anhydride with a purity of 99.9% and an average particle size of 1 μm, and carbon black with a purity of 99.8% are put into a polyethylene bottle according to a mass ratio of 56:28:16, Use ethanol and grinding balls to mix, the mixing time is 15h, the amount of ethanol added is 15ml / g of the total feeding amount, after mixing, dry and press into blocks;

[0077] (2) Heat the block in a high-temperature furnace at 1300°C for 60 minutes once, place the block after heat treatment in hot water at 80°C for 30 minutes to remove boron oxide, heat it twice at 1600°C for 60 minutes, and finally crush it to obtain High-purity ultra-fine hafnium boride powder.

[0078] Gained product is carried out purity, particle size analysis and XRD characterization, specifically see table 1 and...

Embodiment 2

[0080] A method for preparing high-purity ultrafine hafnium boride powder, comprising the following steps:

[0081] (1) Put hafnium oxide powder with a purity of 99.5% and an average particle size of 1 μm, boric acid with a purity of 99.5% and an average particle size of 1 μm, and carbon black with a purity of 99.5% in a polyethylene bottle according to a mass ratio of 46:41:13, and use Mix ethanol and grinding balls, the mixing time is 18h, the amount of ethanol added is 20ml / g of the total feeding amount, after mixing, dry and press into blocks;

[0082] (2) Heat the block in a high-temperature furnace at 1150°C for 120 minutes once, place the heat-treated block in hot water at 60°C for 90 minutes to remove boron oxide, heat it twice at 1400°C for 180 minutes, and finally crush it to obtain High-purity ultra-fine hafnium boride powder.

[0083] The obtained product was analyzed for purity and particle size, see Table 1 for details, and the product purity reached 99.03wt%. ...

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Abstract

The invention provides a preparation method of high-purity superfine hafnium boride powder and the hafnium boride powder, and relates to the technical field of hafnium boride preparation. The preparation method comprises the following steps: mixing, drying and pressing hafnium oxide, a boron source and a carbon source into blocks, wherein the boron source comprises boric anhydride and / or boric acid; and sequentially carrying out primary heat treatment, hot water treatment and secondary heat treatment on the block to obtain the high-purity superfine hafnium boride powder. The temperature of the primary heat treatment is 1150-1500 DEG C, and the temperature of the secondary heat treatment is 1400-1900 DEG C. According to the method, abnormal growth of crystal grains can be avoided, the hafnium boride powder with high purity and ultrafine granularity is obtained, and the method is easy to operate and suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of hafnium boride preparation, in particular to a preparation method of high-purity ultrafine hafnium boride powder and the hafnium boride powder. Background technique [0002] Hafnium boride (HfB 2 ) has a series of unique and excellent properties such as high melting point (3250°C), high hardness (39GPa), high conductivity (15Ω·cm), low oxidation rate and high chemical stability. The key raw materials of thermal protection structural materials that can still maintain chemical and physical stability under high temperature and aerobic environment can be widely used in industries such as engines, advanced aircraft, plasma discharge bodies, cutting tools, furnace components, etc., so it has attracted many in recent years focus on. Purity and particle size are key factors affecting hafnium boride applications. [0003] At present, there are direct synthesis method and self-propagating method commonly used in...

Claims

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Application Information

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IPC IPC(8): C04B35/58C04B35/626
CPCC04B35/58078C04B35/62675C04B2235/3244C04B2235/3409C04B2235/424C04B2235/425C04B2235/48C04B2235/5288C04B2235/96
Inventor 张鑫贾坤乐王彦军张思源章德铭胡晓蕾孟玲
Owner BEIJING MINING & METALLURGICAL TECH GRP CO LTD
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