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Preparation method of disk hexagonal boron nitride polycrystalline fine powder

A hexagonal boron nitride and sheet-like technology is applied in the field of preparation of wafer-like hexagonal boron nitride polycrystalline micropowder, which can solve the problems of complex process, high reaction temperature and high resource consumption, and achieves simple process and lower reaction temperature. , the effect of uniform distribution

Inactive Publication Date: 2010-12-08
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned prior art has the disadvantages that the reaction temperature is higher, the process is complicated, and the resource consumption is higher.

Method used

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  • Preparation method of disk hexagonal boron nitride polycrystalline fine powder
  • Preparation method of disk hexagonal boron nitride polycrystalline fine powder
  • Preparation method of disk hexagonal boron nitride polycrystalline fine powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 5.64 grams of B 2 o 3 , 19.24 g NH 4 Cl, 3.92 grams of magnesium powder and 1.61 grams of Fe 2 o 3 (element molar ratio B: N: Mg: M = 1: 2.24: 1.02: 0.13, M = Fe) After fully mixing, add the stainless steel reaction tank, put the reaction tank into a nitrogen-protected heating furnace, and keep it at 750 ° C for 15 Minutes, cool down naturally. Open the tank and process the collected product, soak it in 0.5M dilute hydrochloric acid and stir for 30 minutes to dissolve impurities such as catalyst, then filter with suction and wash with water to remove water-soluble impurities such as magnesium chloride, and dry the filter cake at 80°C for 8 hours to obtain 3.89 gram off-white powder, the yield is 97.25%. After XRD, SEM and FTIR analysis, it is proved that the product is disc-shaped h-BN, the size and shape of the crystal grains are uniform, the particle diameter is 0.5-1.4 μm, the average diameter is about 0.9 μm, the thickness is 80-150 nm, and the average thi...

Embodiment 2

[0032] Take 2.81 grams of B 2 o 3 , 18.62 g NH 4 Cl, 2.94 g magnesium powder and 1.71 g Co 2 o 3 (Element molar ratio B: N: Mg: M=1: 4.29: 1.51: 0.26, M=Co) After fully mixing, add the stainless steel reaction tank, put the reaction tank into a heating furnace protected by nitrogen, and keep it warm at 800 ° C for 18 Minutes, cool down naturally. Open the tank and process the collected product, soak it in 2M dilute hydrochloric acid, and stir for 30 minutes to dissolve impurities such as catalyst, then filter with suction and wash with water to remove water-soluble impurities such as magnesium chloride, dry the filter cake at 80°C for 12 hours, and finally obtain 1.93 grams Off-white powder with a yield of 96.5%. After XRD, SEM and FTIR analysis, it is proved that the product is disc-shaped h-BN, the size and shape of the crystal grains are uniform, the particle diameter is 0.6-1.3μm, the average diameter is about 0.9μm, the thickness is 70-130nm, the average thickness A...

Embodiment 3

[0034] Take 4.94 g H 3 BO 3 , 12.93 g NH 4 NO 3 , 3.04 grams of magnesium powder and 3.82 grams of NiCl 2 (Element molar ratio B: N: Mg: M=1: 3.94: 1.54: 0.36, M=Ni) After fully mixing, add the stainless steel reaction tank, put the reaction tank into a heating furnace protected by nitrogen, and keep it at 800 ° C for 16 Minutes, cool down naturally. Open the tank and process the collected product, soak it in 5M dilute nitric acid, and stir for 30 minutes to dissolve impurities such as catalyst, then filter with suction and wash with water to remove water-soluble impurities such as magnesium chloride, dry the filter cake at 80°C for 8 hours, and finally obtain 1.87 grams Off-white powder with a yield of 93.51%. After XRD, SEM and FTIR analysis, it is proved that the product is disc-shaped h-BN, the grain size and shape are uniform, the particle diameter is 0.5-1.3μm, the average diameter is about 0.85μm, the thickness is 60-120nm, and the average thickness About 90nm.

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Abstract

The invention relates to a preparation method of disk hexagonal boron nitride polycrystalline fine powder, wherein B-N source reaction precursor reacts under the effect of transition metallic compound catalyst, the B-N source reaction precursor is composed of mixture of boric anhydride or boric acid, ammonium salt and magnesium metal powder, the mole ratio of reactive elements of B: N: Mg: M is 1: 1.5 to 5.0: 1.0 to 2.2: 0.1 to 1.0, M represents transition metal elements of the transition metal compound, the obtained crude product is separated and purified so that the disk hexagonal boron nitride polycrystalline micro-powder can be obtained. The preparation method has the following beneficial effects: the product h-BN fine powder has regular shape, micron-level granularity and uniform distribution. The preparation condition is gentle, the technology process is simple, the cost is low, and the preparation method is applied to industrial production.

Description

technical field [0001] The invention relates to the field of ceramic materials, in particular to a preparation method of disc-shaped hexagonal boron nitride polycrystalline micropowder. Background technique [0002] The structure of hexagonal boron nitride (h-BN) is similar to that of graphite, with a hexagonal layered structure, soft texture, strong machinability, and white color, commonly known as "white graphite". [1] . h-BN boron nitride has the characteristics of high temperature resistance, corrosion resistance, good thermal conductivity, low thermal expansion coefficient, thermal shock resistance, stable chemical properties, good lubricity, etc., and has excellent electrical properties. Widely used in cutting-edge technologies such as [2] . [0003] Previously, it was reported to use the borax-urea (ammonium chloride) method to prepare h-BN by mixing anhydrous borax and urea in an ammonia stream at 1100 °C [7] ; using H 3 BO 3 , white phosphorus and NaN 3 h-BN ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/064C30B29/38
Inventor 谷云乐王吉林潘新叶
Owner WUHAN INSTITUTE OF TECHNOLOGY
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