Method for preparing Si-C-N-based ceramic microspheres

A ceramic microsphere, si-c-n technology, applied in the field of new materials, can solve the problems of cumbersome microsphere preparation process and few reports of Si-C-N based ceramic microspheres, and achieve the effect of less steps, regular shape and smooth surface

Inactive Publication Date: 2014-08-13
深圳市峰源化工新材料股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, there are few reports on the preparation of Si-C-N-based ceramic microspheres by the transformation method of organosilicon polymer precursors.
In the prior art, polyvinylsilazane (PVSZ) microspheres are first prepared by precipitation copolymerization method, and then Si-C-N composite ceramic microspheres are obtained through sintering, but the preparation process of microspheres in this method is cumbersome, and Many ceramic precursors cannot obtain microspheres by precipitation polymerization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take PSN-2 (note: the molecular structure formula is The same below) is the main starting material to prepare Si-C-N-based ceramic microspheres: 0.6g of linear polystyrene (specification: molecular weight is 250000, unless otherwise specified in this patent, all used are polystyrene of this specification Styrene) was dissolved in 15ml of anhydrous THF, and then 3g of PSN-2 was added, and ultrasonic and stirring were repeated to dissolve it completely. Use a vacuum device with a liquid nitrogen cold trap to slowly extract the solvent, take out the precipitated solid (a mixture of polystyrene and PSN-2), keep it at 180°C for 2h for cross-linking reaction, and dissolve the cross-linked product in 30ml of THF In the process, remove the precipitate, obtain the suspension and carry out fractional centrifugation, then use anhydrous THF to wash the separated product twice, dry it in vacuum at 50 ° C for 24 hours, and place it in argon atmosphere in a tube furnace Carry out si...

Embodiment 2

[0036] Preparation of Si-C-N-based ceramic microspheres with PSN-2 as the main starting material: 0.9g of linear polystyrene (specification: random polystyrene, molecular weight in the range of 800-5000) was dissolved in 20ml of anhydrous THF , and then add 3g of PSN-2, repeated ultrasonic and stirring, to make it completely dissolved. Use a vacuum device with a liquid nitrogen cold trap to slowly extract the solvent, take out the precipitated solid (a mixture of polystyrene and PSN-2), keep it at 180°C for 2h to carry out the cross-linking reaction, and dissolve the cross-linked product in 30ml of In THF water, remove the precipitate, obtain the suspension, and perform fractional centrifugation, then use THF to wash the separated product twice, dry it in vacuum at 50°C for 24 hours, and place it in a tube furnace under an argon atmosphere Carry out sintering, temperature rising program: heating rate is 5° C. / min, 750° C. for 4 hours.

Embodiment 3

[0038] Take polymethylsilazane (note: molecular structure formula is ) as the main starting material to prepare Si-C-N-based ceramic microspheres: 3g of polymethylhydrogensilazane was dissolved in 15ml of anhydrous THF, then 0.6g of linear polystyrene was added, ultrasonic and stirred repeatedly, Let it dissolve completely. Use a vacuum device with a liquid nitrogen cold trap to slowly extract the solvent, take out the precipitated solid (a mixture of polystyrene and polymethylhydrogensilazane), keep it at 180°C for 2h to carry out the crosslinking reaction, and dissolve the crosslinked product In an appropriate amount of anhydrous THF, remove the precipitate, obtain the suspension, and carry out fractional centrifugation, then use anhydrous THF to wash the separated product twice, vacuum-dry it at 50°C for 24 hours, and place it in a tube The sintering is carried out in an argon atmosphere in a type furnace, and the heating program is as follows: the heating rate is 5°C / min...

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Abstract

The invention relates to a method for preparing Si-C-N-based ceramic microspheres. The method comprises the following steps: dissolving polysilazane and polystyrene at a certain ratio as well as organic metal compounds into an appropriate solvent through a solution mixing process, performing solvent evaporation for causing phase separation of a polymer mixed system so as to obtain ceramic precursor spherical droplets, then performing low-temperature crosslinking to solidify the spherical droplets into microspheres, and performing centrifugal separation and pyrolysis, thereby obtaining the Si-C-N-based ceramic microspheres. The method is simple to operate, low in requirement on experiment condition and suitable for preparing ceramic microspheres of various materials, and just comprises a few of steps; the prepared ceramic microspheres are regular in shape and smooth in surface; the method can be widely applied to preparation of ceramic microspheres of multiple components.

Description

technical field [0001] The invention relates to the field of new materials, in particular to a method for preparing Si-C-N-based ceramic microspheres. Background technique [0002] Silicone polymer precursor conversion method has the characteristics of good molecular designability, low crosslinking temperature, easy processing and molding, low ceramic conversion cracking temperature and good performance of ceramic products. It is used in ceramic fibers, ceramic coatings, ceramic powders and It has been widely used in the preparation of ceramic matrix composites. Due to its unique application advantages, ceramic microspheres have received sufficient attention and been widely used in high-tech ceramics, catalysis, medicine, separation, extraction and other fields. [0003] However, there are few reports on the preparation of Si-C-N-based ceramic microspheres by conversion of organosilicon polymer precursors. In the prior art, polyvinylsilazane (PVSZ) microspheres are first p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/515C04B35/622
Inventor 孔杰张晓飞陈立新孟拉拉
Owner 深圳市峰源化工新材料股份有限公司
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