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Method for preparing ferric acetylacetonate-containing silicon carbonitride ceramic by precursor conversion method

A technology of iron acetylacetonate and precursors, applied in the field of inorganic non-metallic materials, can solve the problems of limiting the application of SiCN ceramics and poor microwave absorption performance, and achieve the effects of improving microwave absorption performance, increasing apparent porosity, and low preparation temperature

Active Publication Date: 2015-09-30
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] According to the research progress at home and abroad, although there are many studies on the preparation of iron-containing polysilazane precursor ceramic materials by introducing different iron sources, the microwave absorption performance of such materials is still poor. Therefore, SiCN ceramics are limited. Applications in military stealth materials and television broadcasting

Method used

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  • Method for preparing ferric acetylacetonate-containing silicon carbonitride ceramic by precursor conversion method
  • Method for preparing ferric acetylacetonate-containing silicon carbonitride ceramic by precursor conversion method
  • Method for preparing ferric acetylacetonate-containing silicon carbonitride ceramic by precursor conversion method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A kind of precursor method prepares SiCN ceramic method containing iron acetylacetonate, comprises steps as follows:

[0035] (1) Mixing: in N 2 Under the atmosphere, weigh 9.6g of polysilazane, 1g of α-methacrylic acid, and 0.4g of dicumyl peroxide, and stir on a constant temperature magnetic stirrer for 1h to obtain a mixed solution;

[0036] In the mixed solution, polysilazane: dicumyl peroxide is formulated according to the mass ratio of 96%: 4%, and α-methacrylic acid is 10% of the total mass of polysilazane and dicumyl peroxide;

[0037] (2) Cross-linking curing: the mixed solution obtained in step (1) is cured at a heating rate of 3°C / min from room temperature to 400°C for 2 hours;

[0038] (3) Pulverizing and ball milling: the solidified material obtained in step (2) is pulverized and ball milled in a vibrating ball mill, and crosses a 100-mesh sieve;

[0039] (4) Mixing: Weigh 0.1 g of iron acetylacetonate and 0.5 g of the powder obtained in step (3) and mix ...

Embodiment 2

[0046] A kind of precursor method prepares SiCN ceramic method containing iron acetylacetonate, the steps are as follows:

[0047] (1) Mixing: in N 2 Under the atmosphere, weigh 9.6g of polysilazane, 1g of α-methacrylic acid, and 0.4g of dicumyl peroxide, and stir on a constant temperature magnetic stirrer for 1h to obtain a mixed solution;

[0048] In the mixed solution, polysilazane: dicumyl peroxide is formulated according to the mass ratio of 96%: 4%, and α-methacrylic acid is 10% of the total mass of polysilazane and dicumyl peroxide;

[0049] (2) Cross-linking curing: the mixed solution obtained in step (1) is cured at a heating rate of 5°C / min from room temperature to 600°C for 4 hours;

[0050] (3) Pulverizing and ball milling: the solidified material obtained in step (2) is pulverized and ball milled in a vibrating ball mill, and crosses a 100-mesh sieve;

[0051] (4) Mixing: Weigh 0.1 g of iron acetylacetonate and 0.5 g of the powder obtained in step (3) and mix th...

Embodiment 3

[0056] A kind of precursor method prepares the magnetic SiCN ceramic method containing iron acetylacetonate, and the steps are as follows:

[0057] (1) Mixing: in N 2 Under the atmosphere, weigh 9.8g of polysilazane, 1g of α-methacrylic acid, and 0.2g of dicumyl peroxide, and stir on a constant temperature magnetic stirrer for 1h to obtain a mixed solution;

[0058] In the mixed solution, polysilazane: dicumyl peroxide is formulated according to the mass ratio of 98%: 2%, and α-methacrylic acid is 10% of the total mass of polysilazane and dicumyl peroxide;

[0059] (2) Cross-linking curing: the mixed solution obtained in step (1) is cured at a heating rate of 5° C. / min from room temperature to 400° C. for 6 hours;

[0060] (3) Pulverizing and ball milling: the solidified material obtained in step (2) is pulverized and ball milled in a vibration ball mill, and crosses a 200-mesh sieve;

[0061] (4) Mixing: Weigh 0.25 g of iron acetylacetonate and 0.5 g of the powder obtained ...

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Abstract

The invention relates to a method for preparing ferric acetylacetonate-containing silicon carbonitride ceramic by a precursor conversion method. The method comprises the following steps: (1) uniformly mixing polysilazane, alpha-methacrylic acid and dicumyl peroxide to obtain mixed solution; (2) solidifying the mixed solution; (3) crushing and ball-milling the solidified material; (4) uniformly mixing the powder and ferric acetylacetonate; (5) prepressing and shaping the uniformly mixed powder to obtain a green body; (6) pyrolyzing / sintering the green body at a temperature of 1000-1400 DEG C, and insulating to obtain the ferric acetylacetonate-containing silicon carbonitride ceramic. The material obtained by the method disclosed by the invention is good in high-temperature performance, and the introduced ferric acetylacetonate increases the apparent porosity of SiCN ceramic, reduces the volume density of the SiCN ceramic, remarkably improves the microwave absorption performance of the SiCN ceramic, and increases the electromagnetic wave attenuation coefficient.

Description

technical field [0001] The invention relates to a preparation method of iron-silicon-carbon-nitrogen ceramics containing acetylacetonate, in particular to a method for synthesizing iron-silicon-carbon-nitrogen ceramics containing acetylacetonate by a precursor conversion method, and belongs to the field of inorganic non-metallic materials. Background technique [0002] As a microwave absorbing material, SiCN ceramics have excellent high-temperature mechanical properties, thermal stability, chemical stability and environmental resistance. Electromagnetic wave shielding and absorbing materials are not only widely used in electronic countermeasures and stealth technology in the military, occupying a special position, but also in civilian applications, such as television broadcasting, radar technology, and microwave anechoic chambers. Because of the particularity of the application, the absorbing material not only requires good thinning properties, but also meets the requirement...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/622
Inventor 龚红宇冯玉润张玉军王仙丽郭学赵玉军
Owner SHANDONG UNIV
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