Beryllium-containing ceramic precursor preparation method

A ceramic precursor, beryllium acetone technology, applied in the field of polymer material preparation, can solve the problems of difficult large-scale production and application, high cost, etc., and achieve the effect of meeting the requirements of industrial production, low cost, and reduced growth

Active Publication Date: 2017-07-04
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the cost of electron beam irradiation non-melting method is high, and it is difficult to realize large-scale production and application; while the sintering aid method has been paid more and more attention by researchers because of its simple process operation and low cost.

Method used

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  • Beryllium-containing ceramic precursor preparation method
  • Beryllium-containing ceramic precursor preparation method
  • Beryllium-containing ceramic precursor preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 100 g of polycarbosilane (softening point 146-168° C., number average molecular weight 1200-1300), 20 g of beryllium acetylacetonate (20%), and toluene in sequence into a three-necked flask equipped with mechanical stirring, and stir to make the reaction liquid clear and transparent. After the solvent was distilled off by heating, the temperature of the reaction solution was raised to 180° C. under the protection of nitrogen, and the reaction was carried out for 16 hours. An orange-yellow transparent resinous product was obtained with a yield of 98%, a softening point of 200-210° C., a number-average molecular weight Mn=1956, and a molecular weight distribution α=1.52.

[0032] The resulting product contains beryllium silicon carbide infrared spectrum see figure 1 , sol-gel chromatogram (GPC spectrum) see figure 2 . Example 2

Embodiment 2

[0033] Add 100 g of polycarbosilane (softening point 196-210° C., number average molecular weight 1300-1460), 20 g of beryllium acetylacetonate (20%), and toluene into a three-necked flask equipped with mechanical stirring, and stir to make the reaction liquid clear and transparent. After the solvent was distilled off by heating, the temperature of the reaction solution was raised to 180° C. under the protection of nitrogen, and the reaction was carried out for 18 hours. An orange-yellow transparent resinous product was obtained with a yield of 96%, a softening point of 210-220° C., a number-average molecular weight Mn=1983, and a molecular weight distribution α=1.55.

[0034] Gained beryllium-containing silicon carbide product sol-gel chromatogram (GPC spectrum) see image 3 .

Embodiment 3

[0036] Add 100 g of polycarbosilane (softening point 218-240° C., number average molecular weight 1300-1710), 20 g of beryllium acetylacetonate (20%), and toluene in sequence into a three-neck flask equipped with mechanical stirring, and stir to make the reaction solution clear and transparent. After the solvent was distilled off by heating, the temperature of the reaction solution was raised to 180° C. under the protection of nitrogen, and the reaction was carried out for 15 hours. An orange-yellow transparent resinous product was obtained with a yield of 98%, a softening point of 230-260° C., a number-average molecular weight Mn=3805, and a molecular weight distribution а=2.28.

[0037] Gained beryllium-containing silicon carbide product sol-gel chromatogram (GPC spectrum) see Figure 4 .

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Abstract

The present invention provides a beryllium-containing ceramic precursor preparation method, which comprises: dissolving polycarbosilane and beryllium 2,4-pentanedionate in a solvent, uniformly mixing, and distilling to remove the solvent to obtain a mixture; and under a protection atmosphere, heating the mixture, and carrying out a coupling reaction to obtain the beryllium-containing ceramic precursor. According to the present invention, the prepared beryllium-containing ceramic precursor has characteristics of high thermal decomposition stability, simple preparation method and low cost, and meets the industrial production requirements.

Description

technical field [0001] The invention relates to a preparation method of a beryllium-containing ceramic precursor, in particular to a preparation method of a high-temperature-resistant beryllium-containing ceramic precursor, which belongs to the technical field of polymer material preparation. Background technique [0002] The precursor method is the main method for the development of SiC ceramics. It has the advantages of low reaction temperature, simple and easy control, easy molding, high product purity, and good performance, especially its unique process properties such as soluble and fusible. Fibers, ceramic-based composite materials (CMCs), binders, and preparation of ultrafine powders have been successfully applied, and have become a hot spot in the field of SiC ceramics. The preparation of continuous SiC ceramic fibers by the precursor method has been industrialized. Since Nippon Carbon first used this method to produce SiC fibers in 1980, the preparation technology h...

Claims

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Application Information

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IPC IPC(8): C08G77/60C04B35/565
CPCC04B35/571C08G77/60
Inventor 黄小忠王亚玲
Owner CENT SOUTH UNIV
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