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Preparation method of glassy carbon material based on polymer prepolymer precursor

A technology of polymer prepolymer and glass carbon, which is applied in the field of glass carbon material preparation based on polymer prepolymer precursor, can solve the problems of long curing period and high product porosity, and shorten curing cycle and process conditions. The effect of optimizing and improving material properties

Active Publication Date: 2018-03-20
SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the problems of long curing period and high product porosity when preparing glassy carbon materials in the prior art, and provide a method for preparing glassy carbon materials based on polymer prepolymer precursors, which can greatly Reduce the porosity in the glassy carbon green body and the final glassy carbon material, improve the performance of the glassy carbon material, and at the same time effectively shorten the curing time and improve the efficiency of material preparation

Method used

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  • Preparation method of glassy carbon material based on polymer prepolymer precursor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The phenolic resin was dissolved in ethanol at a mass ratio of 30wt%.

[0034] The prepared polymer precursor solution in the mold is placed in a vacuum ultrasonic degassing device, and a vacuum pump is used to evacuate the ultrasonic degassing device to pre-remove the gas in the environment; the polymer precursor solution is heated in a water bath, to 5 o The heating rate of C / h is raised to 80 o C, insulation.

[0035] Ultrasonic degassing is carried out to the polymer precursor solution that is in the heat preservation state in the water bath, specifically: at 80 oC. Keep the vacuum ultrasonic device in a vacuum state with a vacuum degree of 5 kPa -45kPa. At the same time, turn on the ultrasonic degassing function of the device, the ultrasonic frequency is 20kHz, the ultrasonic power is 240W, and the vacuum ultrasonic time is 1-9min.

[0036] The polymer precursor solution after vacuum ultrasonic degassing was degassed with 5 o C / h heating rate from 80 o C warm...

Embodiment 2

[0041] The phenolic resin was dissolved in ethanol at a mass ratio of 40wt%.

[0042] The prepared polymer precursor solution in the mold was placed in a vacuum ultrasonic degassing device, and heated in a water bath in a vacuum environment to 5 o The heating rate of C / h is raised to 70 o C, insulation.

[0043] Ultrasonic degassing was performed on the polymer precursor solution kept warm in a water bath. Specifically: at 70 o C. Keep the vacuum ultrasonic device in a vacuum state with a vacuum degree of 5kPa; at the same time, turn on the ultrasonic degassing function of the device, the ultrasonic frequency is 20kHz, and the ultrasonic power is 240W. The vacuum ultrasonic time is 7min.

[0044] The polymer precursor solution after ultrasonic degassing was degassed at 5 o C / h heating rate from 70 o C warming up to 100 o C, keep warm for 2h; take 5 o The heating rate of C / h is raised to 120 o C, keep warm for 2h; o The heating rate of C / h is raised to 150 o C, keep ...

Embodiment 3

[0049] The phenolic resin was dissolved in ethanol at a mass ratio of 50wt%.

[0050] The prepared polymer precursor solution in the mold was placed in a vacuum ultrasonic degassing device, and heated in a water bath in a vacuum environment to 5 o The heating rate of C / h is raised to 90 o C, insulation.

[0051] Ultrasonic degassing was performed on the polymer precursor solution kept warm in a water bath. Specifically: at 90 o C. Keep the vacuum ultrasonic device in a vacuum state with a vacuum degree of 5kPa. At the same time, turn on the ultrasonic degassing function of the device, the ultrasonic frequency is 20kHz, and the ultrasonic power is 240W. The vacuum ultrasonic time is 7min.

[0052] The polymer precursor solution after vacuum ultrasonic degassing was degassed with 5 o C / h heating rate from 90 o C warming up to 100 o C, keep warm for 2h; take 5 o The heating rate of C / h is raised to 120 o C, keep warm for 2h; o The heating rate of C / h is raised to 150 ...

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Abstract

The invention discloses a glass carbon material preparation method based on high-molecular prepolymer precursor. The method comprises the following steps: dissolving a high-molecular prepolymer precursor into an organic solvent to generate a precursor solution, subjecting the precursor solution to low temperature curing and moulding to obtain a glass carbon blank; and subjecting the glass carbon blank to a carbonization treatment; wherein during the process of low temperature curing and moulding, a vacuum environment is maintained, when the temperature is raised to 70 to 90 DEG C, the temperature is maintained for a while, and during the constant temperature (70-90 DEG C) period, the precursor solution is subjected to an ultrasonic degasifying treatment. During the glass carbon preparation process, a vacuum ultrasonic degasifying technology is adopted to assist the polymer precursor curing, on one aspect, the porosity of prepared glass carbon material is greatly reduced, the physical properties such as wear resistant property, hardness, bend strength, and the like are enhanced at the same time, on the other aspect, the whole preparation period is greatly reduced.

Description

technical field [0001] The invention relates to a method for preparing a glassy carbon material, in particular to a method for preparing a glassy carbon material based on a polymer prepolymer precursor. Background technique [0002] As a new type of carbon material, glassy carbon is called glassy carbon because of its fracture morphology and structural characteristics similar to glass. Glassy carbon has excellent properties such as low density, high strength, high hardness, high electrical conductivity and high thermal conductivity, corrosion resistance, wear resistance, almost airtight and isotropic, and is widely used in electronics industry, semiconductor industry, metallurgical industry, Chemical industry, nuclear industry and medical fields, etc. [0003] At present, the polymer precursors used to prepare glassy carbon mainly include phenolic resin, epoxy resin modified phenolic resin, furfuryl alcohol resin, polyfurfuryl alcohol, polyvinyl chloride, polyimide, etc. T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/524
CPCC04B35/524
Inventor 张东生夏汇浩周兴泰杨新梅叶林凤冯尚蕾
Owner SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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