CN108609603B - Carbon foam containing graphene coating and preparation method thereof - Google Patents
Carbon foam containing graphene coating and preparation method thereof Download PDFInfo
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- CN108609603B CN108609603B CN201810591708.7A CN201810591708A CN108609603B CN 108609603 B CN108609603 B CN 108609603B CN 201810591708 A CN201810591708 A CN 201810591708A CN 108609603 B CN108609603 B CN 108609603B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
Abstract
The invention relates to a carbon bubble containing a graphene coatingThe foam is characterized in that the thickness of the coating is 0.5-5 mu m, the volume percentage of graphene in the coating is 20-30%, the difference between the thermal expansion coefficient of the carbon foam substrate and the thermal expansion coefficient of the coating containing the graphene is less than 15%, the diameter of the carbon foam cell is 50-200 mu m, the thermal conductivity is 0.036-0.685W/(m/K), and the density is 4.57-9.62kg/m3The compressive strength is 5-15MP, the porosity is more than 96 percent, the BET specific surface area is more than 250-600m2(ii) in terms of/g. The graphene-containing coating can effectively improve the mechanical property and the heat insulation property of the carbon foam, increase the specific surface area and provide rich functional groups, so that the graphene-containing coating has wide application prospects in the aspects of catalyst carriers, heat insulation materials and the like.
Description
Technical Field
The invention relates to a preparation method of foam, in particular to a preparation method of carbon foam with a graphene carbon coating, and belongs to the field of carbon materials.
Background
The carbon foam is a novel carbon material which is composed of porous bubbles and interconnected porous bubble walls, has a three-dimensional reticular structure, is in a sponge-like shape, has the characteristics of low density, high porosity, larger specific surface area, good adsorption performance, lower thermal expansion coefficient, low thermal conductivity coefficient and the like, can be used as a heat insulation material, a high-quality interlayer material, a capacity storage electrode, an energy absorption material, a catalyst carrier, a deodorizing agent and the like, and has wide application value in the fields of chemical industry, aerospace, electronics and the like.
Graphene is a two-dimensional material with a single atom thickness, and has a wide application prospect due to unique and excellent electrical, optical and mechanical properties since the discovery, graphene oxide is an important graphene derivative generated in the process of preparing graphene, the graphene oxide modified by chemical functionalization can be stably dispersed in a plurality of common organic solvents to form a stable graphene oxide suspension, the surface of the graphene oxide contains a large number of oxygen active groups, and the groups endow the graphene oxide with some new characteristics, such as dispersibility, hydrophilicity and compatibility with polymers, and improve the heat resistance of the polymers.
CN 200680051980.1 patent provides a process for the preparation of carbon foam containing a glassy carbon coating by coating a carbon foam with a glassy carbon coating by carbonizing a phenolic or polyurethane foam at elevated temperature in an inert atmosphere to produce carbon foam, then processing the foam into the desired shape, treating the surface with a fine or graphite powder, subsequently applying a resin to the surface of the carbon foam, and firing the coated carbon foam block to carbonize the resin into a glassy coating.
The application number CN 200710173126.9 provides a preparation method of a high-strength coal tar pitch carbon foam material, which comprises the steps of pyrolyzing coal tar pitch to prepare mesophase pitch, crushing, adding the mesophase pitch into a toluene solution for extraction and drying, adding the dried mesophase pitch into a high-pressure reaction kettle, vacuumizing, heating to a temperature above the pitch softening point, filling inert gas, keeping the temperature at 350-500 ℃ and the pressure at 6-80kg/cm2 for 240 minutes, releasing the pressure, cooling to room temperature to obtain the pitch carbon foam material, and preparing the carbon foam material under the protection of nitrogen at 1300-1600 ℃ to obtain the carbon foam material, wherein the compression strength of the carbon foam is more than 20 MPa.
The patent with application number CN 200910093957.4 provides a preparation method of a carbon foam heat insulation material added with hollow ceramic balls, which comprises the following steps: adding a surfactant, a foaming agent and hollow ceramic microspheres into phenolic resin in sequence according to a raw material formula, and uniformly dispersing the mixture by a mode of combining mechanical stirring and ultrasonic oscillation; adding a curing agent into the uniformly dispersed mixture, stirring, pouring into a mold, foaming and curing to obtain phenolic foam; and (3) after the phenolic foam is subjected to shelling treatment, putting the phenolic foam into a vacuum carbonization furnace, and heating the phenolic foam to 800 ℃ at the average speed of 0.5 ℃/min under the vacuum condition to obtain the carbon foam heat insulation material. The high-temperature heat-insulating material has the advantages of light weight, high strength, low heat conductivity, low thermal expansion coefficient, low cost, designability and the like
The carbon foam is limited in application due to the defects of low strength, fragility and insufficient toughness, the invention provides some ideas for improving the mechanical property of the carbon foam, a certain enhancement effect is obtained by adding an enhancement phase or a coating to improve the mechanical property of the carbon foam, and the graphene-containing coating prepared on the surface of the carbon foam can effectively improve the mechanical property and the heat insulation property of the carbon foam, increase the specific surface area and provide rich functional groups, so that the carbon foam has wide application prospects in the aspects of catalyst carriers, heat insulation materials and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides carbon foam containing a graphene coating and a preparation method thereof, and the carbon foam is characterized in that the thickness of the coating is 0.5-5 mu m, the volume percentage of graphene in the coating is 10-30%, the difference between the thermal expansion coefficient of a carbon foam substrate and the thermal expansion coefficient of the coating containing the graphene is less than 15%, the diameter of the foam cell of the carbon foam is 50-200 mu m, the thermal conductivity is 0.036-0.685W/(m/K), and the density is 4.57-9.62kg/m3The compressive strength is 5-15MP, the porosity is more than 96 percent, the BET specific surface area is more than 250-600m2/g。
The preparation method of the carbon foam containing the graphene carbon coating comprises the following steps in sequence:
(1) cleaning melamine formaldehyde foam with acetone, then cleaning with 10% ammonia water solution by mass fraction, then cleaning with distilled water, and then drying in an oven at 50-70 ℃ for 6-8 h;
(2) dispersing graphene powder in water, and performing ultrasonic oscillation for 1-3h to form a graphene aqueous solution, wherein the mass fraction of graphene is 5-10%, and the graphene is oxidized graphene passing 3500 meshes;
(3) adding the graphene aqueous solution prepared in the step (2) into a resin solution, mechanically stirring at the rotation speed of 500-plus-one 1000rpm for 1-2h, and then ultrasonically oscillating for 1-2h to prepare a uniformly dispersed mixed solution, wherein the viscosity of the mixed solution is 5-8MPa & s, and the resin is phenolic resin, epoxy resin or a mixture of the phenolic resin and the epoxy resin;
(4) putting the melamine formaldehyde foam treated in the step (1) into the mixed solution in the step (3) for vacuum pressurization and impregnation, wherein the pressurization is 0.5-2MPa, and the pressure maintaining time is 1-3 h;
(5) putting the melamine formaldehyde resin foam impregnated in the step (4) into an oven, and drying for 6-10h at the temperature of 80-150 ℃;
(6) and (3) putting the melamine formaldehyde resin bubbles dried in the step (5) into a vacuum pyrolysis furnace for pyrolysis, vacuumizing to 1-100Pa, taking flowing argon as protective gas, heating to 450-600 ℃ at the speed of 1-5 ℃/min, and preserving heat for 1-3h to obtain the carbon foam containing the graphene carbon coating.
The invention has the beneficial technical effects that:
(1) the composite material has low density, low heat conductivity coefficient and high compression strength, and can be used for heat-insulating material interlayers and thermal shock resistant materials; (2) the catalyst has higher specific surface area and abundant functional groups and can be used for the catalysis industry; (3) the bonding strength of the coating and the matrix is high; (4) the volume shrinkage reduction (4) in the pyrolysis process is simple in preparation process and low in cost.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will occur to those skilled in the art upon reading the present specification and which fall within the limits of the appended claims.
Example 1
The carbon foam containing the graphene coating is characterized in that the thickness of the coating is 2 mu m, the volume ratio of graphene in the coating is 22%, the difference between the thermal expansion coefficient of a carbon foam substrate and the thermal expansion coefficient of the coating containing the graphene is 11%, the diameter of cells of the carbon foam is 80 mu m, the thermal conductivity is 0.284W/(m/K), and the density is 5.68kg/m3A compressive strength of 6.87MP, a porosity of 98.4%, a BET specific surface area of more than 307m2/g。
The carbon foam containing the graphene carbon coating is characterized in that the preparation method comprises the following steps in sequence:
(1) cleaning a carbon foam precursor with acetone, then cleaning with an ammonia water solution with the mass fraction of 10%, then cleaning with distilled water, and then drying in an oven at 60 ℃ for 6.5h, wherein the precursor of the carbon foam is melamine formaldehyde foam;
(2) dispersing graphene powder in water, and performing ultrasonic oscillation for 2 hours to form a graphene aqueous solution, wherein the mass fraction of graphene is 8%, and the graphene is oxidized graphene which passes 3500 meshes;
(3) adding the graphene aqueous solution prepared in the step (2) into a resin solution, mechanically stirring at the rotating speed of 800rpm for 1h, and then ultrasonically oscillating for 2h to prepare a uniformly dispersed mixed solution, wherein the viscosity of the mixed solution is 6.4MPa & s, and the resin is phenolic resin, epoxy resin or a mixture of the phenolic resin and the epoxy resin;
(4) putting the melamine formaldehyde foam treated in the step (1) into the mixed solution in the step (3) for vacuum pressurization impregnation, wherein the pressurization is 1.5MPa, and the pressure maintaining time is 1.5 h;
(5) putting the melamine formaldehyde resin foam impregnated in the step (4) into an oven and drying for 7 hours at the temperature of 100 ℃;
(6) and (3) putting the melamine formaldehyde resin bubbles dried in the step (5) into a vacuum pyrolysis furnace for pyrolysis, vacuumizing to 60Pa, taking flowing argon as protective gas, heating to 480 ℃ at the speed of 2 ℃/min, and preserving heat for 2.5 hours to obtain the carbon foam containing the graphene carbon coating.
Example 2
A carbon foam containing a graphene coating is characterized in that the thickness of the coating is 4 microns, the volume proportion of graphene in the coating is 23 percent, the difference between the thermal expansion coefficient of a carbon foam substrate and the thermal expansion coefficient of the coating containing graphene is 10 percent, the diameter of a carbon foam cell is 90 microns, the thermal conductivity is 0.468W/(m/K), and the density is 7.46kg/m3A compressive strength of 12.5MP, a porosity of 98.9%, a BET specific surface area of more than 427m2/g。
A carbon foam comprising a graphene-carbon coating, characterized in that the preparation process comprises the following sequential steps:
(1) cleaning a carbon foam precursor with acetone, then cleaning with an ammonia water solution with the mass fraction of 10%, then cleaning with distilled water, and then drying in an oven at 65 ℃ for 7 hours, wherein the precursor of the carbon foam is melamine formaldehyde foam;
(2) dispersing graphene powder in water, and performing ultrasonic oscillation for 2 hours to form a graphene aqueous solution, wherein the mass fraction of graphene is 8%, and the graphene is oxidized graphene which passes 3500 meshes;
(3) adding the graphene aqueous solution prepared in the step (2) into a resin solution, mechanically stirring for 2h at the rotation speed of 500-plus-one 1000rpm, and then ultrasonically oscillating for 1h to prepare a uniformly dispersed mixed solution, wherein the viscosity of the mixed solution is 7.4MPa & s, and the resin is phenolic resin, epoxy resin or a mixture of the phenolic resin and the epoxy resin;
(4) putting the melamine formaldehyde foam treated in the step (1) into the mixed solution in the step (3) for vacuum pressurization impregnation, wherein the pressurization is 2MPa, and the pressure maintaining time is 3 hours;
(5) putting the melamine formaldehyde resin foam impregnated in the step (4) into an oven to be dried for 8 hours at the temperature of 100 ℃;
(6) and (3) putting the melamine formaldehyde resin bubbles dried in the step (5) into a vacuum pyrolysis furnace for pyrolysis, vacuumizing to 90Pa, taking flowing argon as protective gas, heating to 450-600 ℃ at a speed of 3 ℃/min, and preserving heat for 3h to obtain the carbon foam containing the graphene carbon coating.
The above description is only two specific embodiments of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modifications made by using the design concept should fall within the scope of infringing the protection of the present invention. However, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (2)
1. The carbon foam containing the graphene coating is characterized in that the thickness of the coating is 0.5-5 mu m, the volume percentage of graphene in the coating is 20-30%, the difference between the thermal expansion coefficient of a carbon foam substrate and the thermal expansion coefficient of the coating containing the graphene is less than 15%, the diameter of foam cells of the carbon foam is 50-200 mu m, the thermal conductivity is 0.036-0.685W/(m.K), and the density is 4.57-9.62kg/m3The compressive strength is 5-15MPa, the porosity is more than 96 percent, and the BET specific surface area is more than 250-600m2/g。
2. The graphene-coated carbon foam according to claim 1, wherein the preparation method comprises the following steps in sequence:
(1) cleaning melamine formaldehyde foam, then cleaning with 10% ammonia water solution by mass fraction, cleaning with distilled water, and then drying in an oven at 50-70 ℃ for 6-8 h;
(2) dispersing graphene powder in water, and performing ultrasonic oscillation for 1-3h to form a graphene aqueous solution, wherein the mass fraction of graphene is 5-10%, and the graphene is oxidized graphene passing 3500 meshes;
(3) adding the graphene aqueous solution prepared in the step (2) into a resin solution, mechanically stirring at the rotation speed of 500 plus materials at 1000rpm for 1-2h, and then ultrasonically oscillating for 1-2h to prepare a uniformly dispersed mixed solution, wherein the viscosity of the mixed solution is 5-8mPa & s, and the resin is phenolic resin, epoxy resin or a mixture of the phenolic resin and the epoxy resin;
(4) putting the melamine formaldehyde foam treated in the step (1) into the mixed solution in the step (3) for vacuum pressurization and impregnation, wherein the pressurization is 0.5-2MPa, and the pressure maintaining time is 1-3 h;
(5) putting the melamine formaldehyde resin foam impregnated in the step (4) into an oven, and drying for 6-10h at the temperature of 80-150 ℃;
(6) and (3) putting the melamine formaldehyde resin bubbles dried in the step (5) into a vacuum pyrolysis furnace for pyrolysis, vacuumizing to 1-100Pa, taking flowing argon as protective gas, heating to 450-600 ℃ at the speed of 1-5 ℃/min, preserving heat for 1-3h, and cooling along with the furnace to obtain the carbon foam containing the graphene carbon coating.
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| US20220008882A1 (en) * | 2018-10-29 | 2022-01-13 | China Petroleum & Chemical Corporation | Porous Composite Material Capable of Generating Electric Arc in Microwave Field, Preparation Method therefor, and Use thereof |
| CN109437147B (en) * | 2018-10-31 | 2020-12-29 | 石狮市川大先进高分子材料研究中心 | Preparation method of multifunctional carbon foam |
| CN109721945A (en) * | 2019-01-16 | 2019-05-07 | 苏州宏久航空防热材料科技有限公司 | A kind of high-dielectric constant inorganic foamed resin based composites substrate and preparation method thereof |
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| CN104151775A (en) * | 2014-08-01 | 2014-11-19 | 天津工业大学 | Preparation method of three-dimensional cross-linked graphene foam structure reinforced resin composite material |
| CN104591131A (en) * | 2015-01-27 | 2015-05-06 | 航天材料及工艺研究所 | Preparation method of high-thermal-conductivity graphene-enhanced foamy carbon |
| CN106783198A (en) * | 2016-11-18 | 2017-05-31 | 上海应用技术大学 | A kind of carbon foam combination electrode material of three dimensional elasticity N doping and preparation method thereof |
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| US10010859B2 (en) * | 2015-12-28 | 2018-07-03 | Nanotek Instruments, Inc. | Integral 3D graphene-carbon hybrid foam and devices containing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104151775A (en) * | 2014-08-01 | 2014-11-19 | 天津工业大学 | Preparation method of three-dimensional cross-linked graphene foam structure reinforced resin composite material |
| CN104591131A (en) * | 2015-01-27 | 2015-05-06 | 航天材料及工艺研究所 | Preparation method of high-thermal-conductivity graphene-enhanced foamy carbon |
| CN106783198A (en) * | 2016-11-18 | 2017-05-31 | 上海应用技术大学 | A kind of carbon foam combination electrode material of three dimensional elasticity N doping and preparation method thereof |
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