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Low-reactivity inorganic boron nitride powder and preparation method thereof

A reactive, boron nitride powder technology, applied in inorganic chemistry, chemical instruments and methods, nitrogen compounds, etc., can solve problems such as unfavorable industrial utilization, low yield of solid polyborazane, etc. chemical application, shortening the preparation time, the effect of shortening the preparation time

Active Publication Date: 2021-11-26
北京玻钢院复合材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, in the method of Fazen, P.J., under the condition of vacuuming and 70°C, borazine needs more than 48h to change from liquid to solid polyborazine, which is unfavorable for industrialized utilization, while solid polyborazine The productive rate is lower than the productive rate of the present invention

Method used

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  • Low-reactivity inorganic boron nitride powder and preparation method thereof
  • Low-reactivity inorganic boron nitride powder and preparation method thereof
  • Low-reactivity inorganic boron nitride powder and preparation method thereof

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preparation example Construction

[0029] A preparation method of low reactivity inorganic boron nitride powder, comprising the steps of:

[0030] S1) Add borazine into the autoclave, feed inert gas, and increase the pressure to 1MPa-5MPa; after increasing the pressure, the temperature is raised to 100-175°C for the first time, and the first holding time is 3.5-6h; Raise the temperature to 125-200°C for the second time, and the second holding time is 0.5-3h to obtain a solid product;

[0031] S2) The solid product is pulverized and refined to obtain inorganic boron nitride powder with low reactivity.

[0032] Specifically, the inert gas includes at least one of nitrogen and argon.

[0033] Specifically, the inert gas is argon.

[0034] Specifically, the temperature T of the first heating 1 and the temperature T of the second heating 2 meet T 2 = T 1 +25.

[0035] Specifically, the first holding time t 1 and the second holding time t 2 meet t 1 =t 2 +3

[0036] Specifically, argon gas was introduced,...

Embodiment 1

[0042]The preparation of sample 1 (inorganic boron nitride powder with low reactivity) includes the following steps:

[0043] Add 2kg of borazine into the autoclave, feed in nitrogen, and raise the pressure to 1MPa; after boosting the pressure, raise the temperature to 175°C for the first time and keep it for 6h; raise the temperature for the second time to 200°C and keep it for 3h to obtain a solid product ;

[0044] The solid product was pulverized and refined to obtain a low-reactivity inorganic boron nitride powder, that is, sample 1.

[0045] The yield of sample 1 was 1.85kg, and the yield was 92.6%.

[0046] Grind sample 1 into powder, after grinding, carry out infrared scanning, such as figure 1 As shown, the infrared spectrum of sample 1 shows that there are stretching vibration peaks of B-H and N-H with weak absorption and small peak area, but at 1350cm -1 The strong and large-area absorption peak is the stretching vibration peak of B-N. Through the comparison of ...

Embodiment 2

[0050] The preparation of sample 2 (inorganic boron nitride powder with low reactivity) includes the following steps:

[0051] Put 4kg of borazine in a stainless steel iron box, then place it in an autoclave, blow in nitrogen, and raise the pressure to 3MPa; after boosting, raise the temperature to 125°C for the first time and keep it warm for 6h; raise the temperature to 150°C for the second time ℃, keep warm for 3h, obtain solid product;

[0052] The solid product was pulverized and refined to obtain a low-reactivity inorganic boron nitride powder, namely sample 2.

[0053] The yield of sample 2 was 3.72kg, and the yield was 93.1%.

[0054] Grind sample 2 into powder, after grinding, carry out infrared scanning, such as figure 2 As shown, the infrared spectrum of sample 2 shows that there are stretching vibration peaks of B-H and N-H with weak absorption and small peak area, but at 1350cm -1 The strong and large-area absorption peak is the stretching vibration peak of B-N...

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Abstract

The invention relates to the technical field of inorganic materials, in particular to low-reactivity inorganic boron nitride powder and a preparation method thereof. The preparation method comprises the following steps: adding borazine into a high-pressure kettle, introducing inert gas, and raising the pressure to 1-5 MPa; after boosting, raising the temperature to 100-150 DEG C for the first time, and keeping the temperature for 0.5-6 hours; raising the temperature to 150-200 DEG C for the second time, and keeping the temperature for 0.5-3 hours to obtain a solid product; crushing and refining the solid product to obtain the low-reactivity inorganic boron nitride powder. Through the design of the preparation method of the low-reactivity inorganic boron nitride powder, the technical problems that in the prior art, the inorganic boron nitride powder needs to be obtained under a high-temperature condition and has high requirements on equipment and the like, and meanwhile, the obtained inorganic boron nitride powder is low in porosity and moderate in looseness degree and reaction activity are solved.

Description

technical field [0001] The invention relates to the technical field of inorganic materials, in particular to a low-reactivity inorganic boron nitride powder and a preparation method thereof. Background technique [0002] Hexagonal boron nitride (h-BN) has a hexagonal layer structure similar to graphite, commonly known as "white graphite". It has excellent dielectric properties and chemical stability, and can be used to prepare h-BN ceramics and c-BN ceramics , h-BN ceramic radome, h-BN ceramic microwave tube energy transmission window and clamping rod materials and other products or components. The common preparation methods of hexagonal boron nitride ceramics include pressureless sintering, hot pressing sintering, reaction sintering, self-propagating method, and CVD method. The raw materials used in these methods are usually boron nitride ceramic powder, boron powder, boric acid, ammonia gas, ring Borazane, etc. Among them, boron nitride ceramic powder, boron powder, bori...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/064
CPCC01B21/0646C01P2002/82
Inventor 彭喆柴笑笑李松高龙飞安楠
Owner 北京玻钢院复合材料有限公司
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