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SiHfOC ceramic microspheres and preparation method thereof

A technology of ceramic microspheres and microspheres, which is applied in the field of ceramic microspheres, can solve problems such as limited applications, and achieve the effect of smooth surface, short preparation cycle and regular shape

Active Publication Date: 2022-07-08
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ternary system SiOC ceramics has the advantages of good high temperature stability and excellent oxidation resistance, but due to its metastable ternary structure at high temperatures, phase separation and carbothermal reduction reactions occur, which limits its application in the high temperature field. Applications
In the prior art, there is no use of metal alkoxide (such as hafnium acetylacetonate) to modify the polysilazane precursor followed by high-temperature heat treatment to finally obtain ceramic microspheres uniformly doped with nanophase

Method used

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  • SiHfOC ceramic microspheres and preparation method thereof
  • SiHfOC ceramic microspheres and preparation method thereof
  • SiHfOC ceramic microspheres and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Polysilazane and divinylbenzene with a mass ratio of 2:1 and a certain amount of OP-10 (divinylbenzene: OP-10=1:1) were added dropwise to the pure acetonitrile solution, and then the The above solution was transferred to an ultrasonic cleaner for further mixing with an ultrasonic power of 100W to obtain a homogeneous emulsion system, and then the emulsion was transferred to an autoclave for solidification for 8h, and the solid product was separated by a suction filtration device. Wash several times with deionized water and anhydrous ethanol, and dry in an oven at 80°C;

[0040] The product of step 1 and a certain amount of hafnium acetylacetonate (PSN microspheres: hafnium acetylacetonate = 8:2) were added to the xylene solution for uniform mixing, and then transferred to a three-necked flask to carry out a polymerization reaction at 80 °C, After the reaction, suction filtration, washing and drying are performed to obtain Hf-modified PSN microspheres;

[0041] The prod...

Embodiment 2

[0044] According to the volume ratio of deionized water:acetonitrile=2:8, a mixed solution was prepared and mixed evenly on a magnetic stirrer, and then polysilazane and divinylbenzene with a mass ratio of 2:1 and a certain amount of OP-10 (divinylbenzene: OP-10=1:1) was added dropwise to the above mixed solution, and then the above solution was transferred to an ultrasonic cleaner for further mixing with an ultrasonic power of 100W to obtain a homogeneous emulsion system, and then transferred the emulsion to a high-pressure reactor to solidify for 10 hours, and separated the solid product through a suction filtration device. During the suction filtration process, it was washed several times with deionized water and anhydrous ethanol, and dried in an oven at 80 °C. ;

[0045] The product of step 1 and a certain amount of hafnium acetylacetonate (PSN microspheres: hafnium acetylacetonate = 8:2) were added to the xylene solution for uniform mixing, and then transferred to a thre...

Embodiment 3

[0049] According to the volume ratio of deionized water:acetonitrile=3:7, a mixed solution was prepared and mixed evenly on a magnetic stirrer, and then polysilazane and divinylbenzene with a mass ratio of 2:1 and a certain amount of OP-10 (divinylbenzene: OP-10=1:1) was added dropwise to the above mixed solution, and then the above solution was transferred to an ultrasonic cleaner for further mixing with an ultrasonic power of 100W to obtain a homogeneous emulsion Then the emulsion was transferred to a high-pressure reactor for solidification for 8 hours, and the solid product was separated by a suction filtration device. During the suction filtration process, it was washed several times with deionized water and anhydrous ethanol, and dried in an oven at 80 °C. ;

[0050] The product of step 1 and a certain amount of hafnium acetylacetonate (PSN microspheres: hafnium acetylacetonate = 8:2) were added to the xylene solution for uniform mixing, and then transferred to a three-n...

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Abstract

The invention relates to SiHfOC ceramic microspheres and a preparation method thereof.The preparation method comprises the steps that polysilazane, divinyl benzene and OP-10 are dissolved in a proper solvent according to a certain proportion through a solution blending method, then the evenly-mixed solution is transferred into a high-pressure reaction kettle, curing is conducted in a constant-temperature drying oven, and PSN microspheres are obtained; hafnium acetylacetonate, the PSN microspheres and a xylene solution are added into a three-necked flask for a polymerization reaction, then low-temperature crosslinking, cracking and heat treatment are sequentially carried out, and finally the SiHfOC microspheres are prepared. Compared with the prior art, the method has the advantages that the operation is simple, the experimental condition requirement is low, no catalyst is added, the obtained ceramic microspheres are regular in shape, controllable in size and smooth in surface, and the Hf-containing nanocrystals can be uniformly embedded in the surfaces and the interiors of the SiHfOC microspheres. The method is suitable for preparing the ceramic microspheres with various components.

Description

technical field [0001] The invention belongs to the technical field of ceramic microspheres, and relates to a SiHfOC ceramic microsphere and a preparation method. Background technique [0002] With the rapid development of aerospace technology, the field of hypersonic vehicles has become an important direction for the development of countries around the world. The huge test of ultra-high temperature extreme environment applications has put forward more stringent requirements for the structure and thermal protection components of aircraft. Among them, ultra-high temperature ceramic materials have high melting point, high strength, good high temperature stability and excellent thermal shock resistance. received extensive attention. Polymer-converted ceramics are often used in the preparation of silicon-based ceramic composites due to the composite design of components at the molecular level, thereby realizing the controllable preparation of ceramic composition, structure and ...

Claims

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Application Information

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IPC IPC(8): C04B35/56C04B35/571C04B35/577C04B35/622
CPCC04B35/5603C04B35/571C04B35/5622C04B35/622C04B2235/6562C04B2235/95Y02E60/10
Inventor 李贺军张雪萌孙佳张育育王雨祺
Owner NORTHWESTERN POLYTECHNICAL UNIV
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