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Preparation method of raspberry-shaped SiCxNyOz microspheres converted by polysilazane

A technology of polysilazane and raspberry, which is applied in the field of micron ceramic powder preparation, can solve the problems of complex preparation process and achieve the effects of simple preparation method, good loss and absorption, and good high temperature stability

Active Publication Date: 2021-07-02
NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation process of the above materials is more complicated

Method used

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  • Preparation method of raspberry-shaped SiCxNyOz microspheres converted by polysilazane
  • Preparation method of raspberry-shaped SiCxNyOz microspheres converted by polysilazane
  • Preparation method of raspberry-shaped SiCxNyOz microspheres converted by polysilazane

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Embodiment 1

[0027] This embodiment includes the following steps:

[0028]Step 1, preparing divinylbenzene, carbon-carbon double bond-containing polysilazane, 2,2'-azobisisobutyronitrile and acetonitrile into a mixed liquid; the quality of divinylbenzene in the mixed liquid is two 20% of the total mass of vinylbenzene and polysilazane containing carbon-carbon double bonds, the mass of the 2,2'-azobisisobutyronitrile is the total mass of divinylbenzene and polysilazane containing carbon-carbon double bonds 2% of the quality, the ratio of the quality of the acetonitrile to the total mass of divinylbenzene and carbon-carbon double bond polysilazane is 16:1;

[0029] Step 2. Put the mixed liquid obtained in Step 1 into a round-bottomed flask, pass it through argon gas, heat it to 50°C for 10 hours, then wash it repeatedly with methanol and tetrahydrofuran, vacuum filter and vacuum dry it for 24 hours to obtain initial powder;

[0030] Step 3. Under the protection of nitrogen, the initial pow...

Embodiment 2

[0061] The preparation method of the present embodiment comprises the following steps:

[0062] Step 1, preparing divinylbenzene, carbon-carbon double bond-containing polysilazane, 2,2'-azobisisobutyronitrile and acetonitrile into a mixed liquid; the quality of divinylbenzene in the mixed liquid is two 15% of the total mass of vinylbenzene and polysilazane containing carbon-carbon double bonds, the mass of the 2,2'-azobisisobutyronitrile is the total mass of divinylbenzene and polysilazane containing carbon-carbon double bonds 1.5% of the mass, the ratio of the mass of the acetonitrile to the total mass of divinylbenzene and carbon-carbon double bond polysilazane is 16:1;

[0063] Step 2: Put the mixed liquid obtained in Step 1 into a round-bottomed flask, pass through nitrogen gas, heat to 55°C for 12 hours, then wash repeatedly with methanol and tetrahydrofuran, vacuum filter and vacuum dry for 24 hours to obtain the initial Powder;

[0064] Step 3. Under the protection of...

Embodiment 3

[0082] The preparation method of the present embodiment comprises the following steps:

[0083] Step 1, preparing divinylbenzene, carbon-carbon double bond-containing polysilazane, 2,2'-azobisisobutyronitrile and acetonitrile into a mixed liquid; the quality of divinylbenzene in the mixed liquid is two 25% of the total mass of vinylbenzene and polysilazane containing carbon-carbon double bonds, and the mass of 2,2'-azobisisobutyronitrile is the total mass of divinylbenzene and polysilazane containing carbon-carbon double bonds. 2.5% of the mass, the ratio of the mass of the acetonitrile to the total mass of divinylbenzene and carbon-carbon double bond polysilazane is 16:1;

[0084] Step 2. Put the mixed liquid obtained in Step 1 into a round-bottomed flask, pass it through argon gas, heat it to 60°C for 8 hours, then wash it repeatedly with methanol and tetrahydrofuran, vacuum filter and dry it in vacuum for 24 hours to obtain initial powder;

[0085] Step 3. Under the prote...

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Abstract

The invention discloses a preparation method of raspberry-shaped SiCxNyOz microspheres converted by polysilazane, and the method comprises the following steps: 1, using divinyl benzene, polysilazane containing carbon-carbon double bonds, 2,2'-azodiisobutyronitrile and acetonitrile to prepare a mixed liquid; 2, carrying out heating reaction on the mixed liquid, repeatedly conducting washing, and carrying out vacuum filtration and vacuum drying to obtain initial powder; and 3, carrying out sintering treatment under the protection of an inert atmosphere, and conducting cooling to room temperature to obtain the raspberry-shaped SiCxNyOz microspheres. The raspberry-shaped SiCxNyOz microspheres with a large number of nanoscale protrusions formed on the surfaces and a secondary micro-nano structure are obtained by controlling the proportion of solute, an initiator and solvent, the heating reaction temperature and the sintering temperature rise rate, and the raspberry-shaped SiCxNyOz microspheres have a large number of nanoscale interfaces and are beneficial to loss and absorption of electromagnetic wave energy, so that the raspberry-shaped SiCxNyOz microspheres have good wave-absorbing performance and is expected to be applied to the civil or military field as a wave-absorbing agent or a wave-absorbing coating.

Description

technical field [0001] The invention belongs to the technical field of micron ceramic powder preparation, in particular to a raspberry-shaped SiC transformed from polysilazane x N y o z Microsphere preparation method. Background technique [0002] With the rapid development of civilian Internet of Things electromagnetic compatibility technology, electromagnetic anti-jamming technology and military stealth technology, the importance of electromagnetic shielding and absorbing materials has become increasingly prominent, especially as high-temperature components of advanced weapons used in aircraft engines, fighter jet nozzles, cruise High-temperature wave-absorbing coatings and structural wave-absorbing materials such as missile end caps are the key to improving the country's advanced weapon stealth technology. Materials that are light in weight, thin in thickness, high in electromagnetic wave absorption rate and wide in effective absorption spectrum, and resistant to high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/626
CPCC04B35/58C04B35/626C04B2235/483
Inventor 李珍宝贺加贝刘学谦
Owner NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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