Preparation method of glassy carbon products and glassy carbon products

Abstract

The invention discloses a preparation method of glassy carbon products. The preparation method comprises the following steps of step 1, firstly, enabling graphene to be dispersed in deionized water by using a surfactant to obtain a graphene solution, and thoroughly mixing high molecular polymer powder with the graphene solution so as to obtain mixed slurry in which the mass ratio of the graphene to the high molecular polymer is (0.1-1) to 100; step 2, drying the mixed slurry, then performing dry method ball milling, and performing humidifying treatment on material powder after ball milling is completed; step 3, performing die pressing and shaping on the powder material after the humidifying treatment is completed, and then performing low temperature curing so as to obtain the glassy carbon blanks; step 4, in the environment of being free from oxygen or in the inert environment, performing carbonization treatment on the glassy carbon blanks; and step 5, performing graphitizing. The invention further discloses the glassy carbon products prepared by the method. Compared with the prior art, the production cycle can be greatly shortened, the properties of the glassy carbon products are improved, and the produced glassy carbon products are free from limitation of specifications and shapes.

Description

Technical field

[0001] The invention relates to a preparation method of glass charcoal products and glass charcoal products prepared by the method. Background technique

[0002] Because of its excellent properties such as low density, high strength, high hardness, high electrical conductivity and high thermal conductivity, corrosion resistance, wear resistance, almost airtightness and isotropy, glassy carbon is widely used in the electronics industry, semiconductor industry, and metallurgical industry. , Chemical industry, nuclear industry and medical fields. The polymer prepolymer precursors for preparing glassy carbon materials mainly include phenolic resin, furfuryl alcohol resin, polyfurfuryl alcohol, polyvinyl chloride, polyimide and so on. At present, the preparation of glass charcoal mainly adopts the casting molding method. The basic process is to dissolve the high molecular polymer in an alcohol solvent, solidify at a low temperature or add a curing agent to form a gree...

Examples

preparation example Construction

[0023] The preparation method of the glass charcoal product of the present invention specifically includes the following steps:

[0024] Step 1. Disperse graphene in deionized water using a surfactant to obtain a graphene solution; then fully mix the polymer powder and the graphene solution to obtain the mass ratio between graphene and polymer (0.1~1): 100 mixed slurry;

[0025] The high molecular polymer can be phenolic resin, furfuryl alcohol resin, polyfurfuryl alcohol, polyvinyl chloride, polyimide and other existing polymeric prepolymer precursors used in the preparation of glass charcoal, preferably phenolic resin or furfuryl alcohol resin Or polyfurfuryl alcohol.

[0026] In order to solve the problem of the dispersibility of graphene in the water phase and the uniformity of its mixing with high molecular polymers, surfactants need to be used; the surfactants can be cetyltrimethylammonium bromide, ten Existing surfactants such as sodium dialkylbenzene sulfonate and Tween-80....

Embodiment 1

[0039] According to the mass ratio of graphene to phenolic resin of 0.05:100, the slurry was prepared and put into a ball mill for ball milling for 5 hours at a speed of 400 rpm.

[0040] Take out the high molecular polymer slurry prepared in the above steps and put it into the drying box. o Dry for 10h under C condition.

[0041] Put the dried material block in the above step into a ball mill for 5 hours and pass through a 200 mesh sieve.

[0042] Put the powder sieved in the above steps into a constant temperature and humidity box for humidity adjustment, and control the moisture content of the powder to 10%.

[0043] The powder obtained in the above steps is put into a self-made mold (cavity size is 50×50×10mm) and pressed into shape, the pressure holding time is 5min, the molding pressure is 90MPa, and the mold clamping rate is 0.2mm / s.

[0044] The green body after compression molding in the above steps is subjected to low temperature curing treatment. When curing at low temperatu...

Embodiment 2

[0049] According to the mass ratio of graphene to phenolic resin of 0.1:100, the slurry was prepared and put into a ball mill for ball milling for 5 hours at a speed of 400 rpm.

[0050] Take out the slurry prepared in the above steps and put it into the drying box. o Dry for 10h under C condition.

[0051] Put the dried material block in the above step into a ball mill for 5 hours and pass through a 200 mesh sieve.

[0052] Put the powder after drying in the above steps into a constant temperature and humidity box for humidity adjustment, and control the moisture content of the powder to 10%.

[0053] The powder obtained in the above steps is put into a self-made mold (cavity size is 50×50×10mm) and pressed into shape, the pressure holding time is 5min, the molding pressure is 30MPa, and the mold clamping rate is 0.2mm / s.

[0054] The low-temperature curing treatment of the green body after the press molding in the above steps. When curing at low temperature, use 1 o The heating rate ...

Technical field

[0001] The invention relates to a preparation method of glass charcoal products and glass charcoal products prepared by the method. Background technique

[0002] Because of its excellent properties such as low density, high strength, high hardness, high electrical conductivity and high thermal conductivity, corrosion resistance, wear resistance, almost airtightness and isotropy, glassy carbon is widely used in the electronics industry, semiconductor industry, and metallurgical industry. , Chemical industry, nuclear industry and medical fields. The polymer prepolymer precursors for preparing glassy carbon materials mainly include phenolic resin, furfuryl alcohol resin, polyfurfuryl alcohol, polyvinyl chloride, polyimide and so on. At present, the preparation of glass charcoal mainly adopts the casting molding method. The basic process is to dissolve the high molecular polymer in an alcohol solvent, solidify at a low temperature or add a curing agent to form a gree...

Examples

preparation example Construction

[0023] The preparation method of the glass charcoal product of the present invention specifically includes the following steps:

[0024] Step 1. Disperse graphene in deionized water using a surfactant to obtain a graphene solution; then fully mix the polymer powder and the graphene solution to obtain the mass ratio between graphene and polymer (0.1~1): 100 mixed slurry;

[0025] The high molecular polymer can be phenolic resin, furfuryl alcohol resin, polyfurfuryl alcohol, polyvinyl chloride, polyimide and other existing polymeric prepolymer precursors used in the preparation of glass charcoal, preferably phenolic resin or furfuryl alcohol resin Or polyfurfuryl alcohol.

[0026] In order to solve the problem of the dispersibility of graphene in the water phase and the uniformity of its mixing with high molecular polymers, surfactants need to be used; the surfactants can be cetyltrimethylammonium bromide, ten Existing surfactants such as sodium dialkylbenzene sulfonate and Tween-80....

Embodiment 1

[0039] According to the mass ratio of graphene to phenolic resin of 0.05:100, the slurry was prepared and put into a ball mill for ball milling for 5 hours at a speed of 400 rpm.

[0040] Take out the high molecular polymer slurry prepared in the above steps and put it into the drying box. o Dry for 10h under C condition.

[0041] Put the dried material block in the above step into a ball mill for 5 hours and pass through a 200 mesh sieve.

[0042] Put the powder sieved in the above steps into a constant temperature and humidity box for humidity adjustment, and control the moisture content of the powder to 10%.

[0043] The powder obtained in the above steps is put into a self-made mold (cavity size is 50×50×10mm) and pressed into shape, the pressure holding time is 5min, the molding pressure is 90MPa, and the mold clamping rate is 0.2mm / s.

[0044] The green body after compression molding in the above steps is subjected to low temperature curing treatment. When curing at low temperatu...

Embodiment 2

[0049] According to the mass ratio of graphene to phenolic resin of 0.1:100, the slurry was prepared and put into a ball mill for ball milling for 5 hours at a speed of 400 rpm.

[0050] Take out the slurry prepared in the above steps and put it into the drying box. o Dry for 10h under C condition.

[0051] Put the dried material block in the above step into a ball mill for 5 hours and pass through a 200 mesh sieve.

[0052] Put the powder after drying in the above steps into a constant temperature and humidity box for humidity adjustment, and control the moisture content of the powder to 10%.

[0053] The powder obtained in the above steps is put into a self-made mold (cavity size is 50×50×10mm) and pressed into shape, the pressure holding time is 5min, the molding pressure is 30MPa, and the mold clamping rate is 0.2mm / s.

[0054] The low-temperature curing treatment of the green body after the press molding in the above steps. When curing at low temperature, use 1 o The heating rate ...