CN108172793B - Method for preparing three-dimensional carbon foam/graphene oxide-based composite material through centrifugal separation - Google Patents
Method for preparing three-dimensional carbon foam/graphene oxide-based composite material through centrifugal separation Download PDFInfo
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Abstract
A method for preparing a three-dimensional carbon foam/graphene oxide-based composite material by centrifugal separation comprises the following steps: (1) pretreating melamine-formaldehyde resin foam, and thermally cracking the melamine-formaldehyde resin foam under the inert atmosphere condition to prepare a three-dimensional carbon foam framework; (2) immersing the three-dimensional carbon foam skeleton into the graphene oxide dispersion liquid or the graphene oxide-based composite material dispersion liquid, and repeatedly extruding to obtain carbon foam adsorbed with graphene oxide or the graphene oxide-based composite material; (3) placing the mixture into a centrifuge tube or a centrifuge bottle with a partition plate with a sieve pore structure, starting a centrifuge, and realizing solid-liquid separation through the partition plate under the centrifugal action; (4) and drying the separated solid phase to remove water. The method is simple and easy to implement, avoids harsh preparation environment, saves a large amount of time, can controllably adjust the content of the graphene oxide in the composite material, and can realize large-scale production; the product has good flexibility and conductivity.
Description
Technical Field
The invention belongs to the technical field of three-dimensional graphene-based composite materials, and particularly relates to a method for preparing a three-dimensional carbon foam/graphene oxide-based composite material through centrifugal separation.
Background
Graphene is a two-dimensional honeycomb structure formed by stacking single-layer carbon atoms, and is the thinnest two-dimensional nano material with the best conductivity and the highest mechanical property discovered so far. The existing preparation of graphene or graphene oxide mostly adopts physical methods such as Chemical Vapor Deposition (CVD) method and chemical methods (Hummers). In order to meet the urgent needs of the new energy field, various porous three-dimensional graphene or composite materials thereof with large specific surface area are prepared and used in the fields of high-performance super capacitors, lithium ion batteries, sodium ion batteries and the like.
At present, the preparation method of the three-dimensional graphene mainly comprises a Chemical Vapor Deposition (CVD) method, a hydrothermal method, a template method and the like. The CVD method for preparing the three-dimensional graphene is very complex, the graphene is firstly deposited on three-dimensional nickel foam, then the three-dimensional nickel foam is soaked by hydrochloric acid to remove metal, and finally the three-dimensional graphene is obtained, and the three-dimensional structure generally has no good flexibility; chinese patent with patent application No. 201010183833.8, entitled graphene foam and method for preparing the same, discloses a method for preparing graphene foam as follows: 1) placing the metal foam material into a vacuum tube furnace, and calcining under a non-oxidizing atmosphere; 2) depositing graphene on the calcined metal foam material by adopting a chemical vapor deposition method; 3) removing foam metal in the obtained graphene modified metal foam material; and then sequentially washing the obtained foam material with deionized water, ethanol and diethyl ether, taking out and drying to finally obtain the graphene foam.
According to the hydrothermal method, graphene oxide dispersion liquid is placed in a reaction kettle and placed in an oven at 180-200 ℃ for hydrothermal treatment to prepare the three-dimensional graphene hydrogel, the hydrogel generally needs freeze drying to keep a good three-dimensional structure, but the freeze drying process generally needs a long time (more than 24 hours); a chinese patent having a patent application number of 201310370268.X, entitled mesoporous graphene foam and a preparation method thereof, discloses hydrothermal preparation of a magnesium oxide texture structure and preparation of mesoporous graphene foam using texture magnesium oxide as a template, and the mesoporous graphene foam material has a rich mesoporous structure and excellent electrical properties.
Compared with the former two methods, the template method is relatively simple, and only graphene or graphene oxide needs to be copied on the template, such as a sacrificial template method and an impregnation method. The chinese patent with the patent application number of 201610992467.8, entitled method for preparing graphene foam material by furfuryl ketone aldehyde resin, graphene foam material and application thereof discloses a method for preparing graphene foam material by furfuryl ketone aldehyde resin, which comprises adding non-carbon atoms and substances easy to remove at high temperature into the furfuryl ketone aldehyde resin, curing and molding, and then carrying out high-temperature carbonization and graphitization in an inert gas environment, thereby forming a novel graphene foam material with a hexagonal or pentagonal two-dimensional or three-dimensional polyhedral crystal network structure. Chinese patent No. 201310292634.4, entitled three-dimensional graphene-based foam material preparation method, discloses that a polymer foam material is used as a template, a polymer foam material containing graphene oxide is obtained by a simple impregnation method, and then the polymer foam is heat-treated under an oxygen-free condition to obtain a three-dimensional graphene-based foam material; the method can prepare graphene-based foam macroscopic bodies with three-dimensional continuous structures.
In summary, the existing preparation method of the three-dimensional graphene composite material generally requires a harsh environment (CVD method) or a long post-treatment time (freeze-drying by immersion method), and it is difficult to realize rapid preparation and large-scale production of the three-dimensional graphene or the composite material thereof, especially difficult to controllably prepare the three-dimensional graphene-based composite material with a fixed graphene oxide content.
Disclosure of Invention
In order to solve the problems of the existing preparation technology of the three-dimensional graphene oxide composite material, the invention provides a method for preparing the three-dimensional carbon foam/graphene oxide-based composite material by centrifugal separation.
The technical scheme for realizing the purpose of the invention is carried out according to the following steps:
(1) preparing a three-dimensional carbon foam framework: cleaning melamine-formaldehyde resin foam with distilled water and ethanol respectively, immersing the melamine-formaldehyde resin foam in absolute ethyl alcohol for ultrasonic treatment, washing off impurities, taking out the melamine-formaldehyde resin foam, drying or air-drying the melamine-formaldehyde resin foam to remove the absolute ethyl alcohol, heating the melamine-formaldehyde resin foam to 800-1000 ℃ at the speed of 5-10 ℃/min under the condition of inert atmosphere, preserving the temperature for 2-5 hours for thermal cracking, and cooling the melamine-formaldehyde resin foam to the normal temperature along with a furnace to obtain a conductive three-dimensional carbon foam framework;
(2) carbon foam adsorption: immersing the three-dimensional carbon foam framework into the graphene oxide dispersion liquid or the graphene oxide-based composite material dispersion liquid for 3-20 min, and repeatedly extruding the three-dimensional carbon foam framework to ensure saturated adsorption to obtain carbon foam adsorbed with graphene oxide or the graphene oxide-based composite material; the concentration of the graphene oxide dispersion liquid is 0.5-6.0 mg/mL, and the concentration of the graphene oxide-based composite material dispersion liquid is 0.5-6.0 mg/mL;
(3) centrifugal separation: placing the partition plate with the sieve pore structure in a centrifuge tube or a centrifuge bottle, taking out the carbon foam adsorbed with the graphene oxide or graphene oxide-based composite material, placing the carbon foam on the partition plate of the centrifuge tube or the centrifuge bottle, and then placing the centrifuge tube or the centrifuge bottle in a centrifuge; starting a centrifugal machine, and realizing solid-liquid separation through a partition plate under the centrifugal action, wherein a liquid phase is a separated graphene oxide dispersion liquid or graphene oxide-based composite material dispersion liquid, and a solid phase is a three-dimensional carbon foam framework wrapping graphene oxide nano sheets or graphene oxide-based composite material nano sheets;
(4) and drying the solid phase to remove water, and preparing the three-dimensional carbon foam/graphene oxide-based composite material.
In the method, the rotating speed of a centrifugal machine is 500-10000 rpm when centrifugal separation is carried out, and the centrifugal time is 5-20 min.
In the method, the ultrasonic frequency during ultrasonic treatment is 60Hz, and the time is 30-60 min.
In the method, the drying temperature in the step (4) is 60-80 ℃, and the time is 30-120 min.
In the method, the three-dimensional carbon foam/graphene oxide-based composite material contains 3-16% of graphene oxide or graphene oxide-based composite material by weight.
The graphene oxide dispersion liquid is prepared by a Hummers method or chemical oxidation stripping.
The graphene oxide-based composite dispersion liquid is a graphene oxide/polyaniline dispersion liquid prepared by growing polyaniline nanoparticles on graphene oxide sheet layers in situ by a chemical method, or a graphene oxide/manganese dioxide composite dispersion liquid, a graphene oxide/tin hydroxide composite dispersion liquid, a graphene oxide/nickel hydroxide composite dispersion liquid or a graphene oxide/cobalt hydroxide composite dispersion liquid prepared by growing metal oxides or hydroxides on graphene oxide sheet layers by a hydrothermal method.
Compared with the prior art, the invention has the characteristics and beneficial effects that:
(1) the centrifugal separation method is adopted to prepare the three-dimensional carbon foam/graphene oxide-based composite material, the method is simple and easy to implement, compared with the traditional CVD method and hydrothermal method, the harsh growth environment can be avoided, a large amount of time is saved, especially the content proportion of graphene oxide can be controlled and adjusted, and the large-scale production can be realized;
(2) because the matrix material adopts carbonized three-dimensional foam, and a great amount of graphene oxide or composite material sheets thereof are wrapped on the foam framework by a centrifugal separation method; therefore, the prepared product has good flexibility, conductivity and hierarchical pore structure, and is particularly suitable for preparing electrode materials of supercapacitors, lithium ion batteries and sodium ion batteries or adsorbing pollutants in sewage, such as oil stains, heavy metal ions and the like.
Drawings
FIG. 1 is a photographic image of the appearance of a melamine-formaldehyde resin foam before and after thermal decomposition in example 1 of the present invention; in the figure, the left side is before thermal cracking, and the right side is after thermal cracking;
FIG. 2 is an SEM photograph of a three-dimensional carbon foam skeleton in example 1 of the present invention;
fig. 3 is an SEM photograph of the three-dimensional carbon foam/graphene oxide-based composite material in example 1 of the present invention; the distribution of the graphene oxide nanosheets in the carbon foam backbone can be seen in comparison with fig. 2.
Detailed Description
The heating and heat-preserving equipment adopted in the embodiment of the invention is a tubular furnace.
The model of SEM observation equipment used in the embodiments of the present invention is JSM-7500F scanning electron microscope (japan electronics).
The melamine-formaldehyde resin foams in the examples of the present invention are commercially available products.
The inert atmosphere in the embodiment of the invention is nitrogen atmosphere or argon atmosphere.
In the embodiment of the invention, the ultrasonic frequency during ultrasonic treatment is 60Hz, and the time is 30-60 min.
In the embodiment of the invention, the partition plate is positioned in the middle of the centrifugal tube or the centrifugal bottle, and the surface of the partition plate is provided with a plurality of sieve holes.
In the embodiment of the invention, the rotating speed of the centrifugal machine during centrifugal separation is 500-10000 rpm.
The preparation method of the graphene oxide solution adopted in the embodiment of the invention comprises the following steps: putting 80mL of concentrated sulfuric acid into a round-bottom flask, putting the round-bottom flask into a constant-temperature water bath at the temperature of 80 ℃, adding 15g of potassium persulfate and 15g of phosphorus pentoxide, and magnetically stirring until the concentrated sulfuric acid is completely dissolved; then 20g of graphite powder is added, and the mixture is continuously stirred for 5 hours; cooling to room temperature, filtering, washing with water until the filtrate is neutral to obtain pre-oxidized graphite; adding the pre-oxidized graphite powder into 800ml of concentrated sulfuric acid, placing a reactor in an ice water bath with the temperature not exceeding 5 ℃, adding 100g of potassium permanganate, and uniformly stirring; then the reactor is transferred to a constant temperature water bath with the temperature of 30 ℃ for continuous magnetic stirring for 2 hours, then the reactor is transferred to an ice water bath with the temperature not exceeding 5 ℃, water is added to dilute the materials to 4L of total volume, and 90mL of H with the weight concentration of 38 percent is slowly added2O2Then, generating uniform orange suspension; standing overnight to generate precipitate, pouring out supernatant, filtering the precipitate, washing with water until filtrate is neutral, and finally performing centrifugal separation to obtain concentrated graphite oxide; diluting the concentrated graphite oxide to 500mL by using deionized water, continuously carrying out ultrasonic treatment for 4h, stripping the graphite oxide to obtain a graphene oxide aqueous solution, and measuring by adopting a freeze-drying methodThe fixed concentration is 8.0 mg/mL; the graphene oxide aqueous solution is added with water to adjust the concentration, so that the graphene oxide dispersion liquid with the concentration required in the embodiment is prepared.
The following examples are given to illustrate specific embodiments of the present invention, and the embodiments of the present invention are not limited to the examples.
Example 1
The concentration of the graphene oxide dispersion solution adopted is 3.0 mg/mL:
respectively cleaning melamine-formaldehyde resin foam with distilled water and ethanol, immersing the melamine-formaldehyde resin foam in absolute ethyl alcohol for ultrasonic treatment, washing off impurities, taking out the melamine-formaldehyde resin foam, air-drying the melamine-formaldehyde resin foam to remove the absolute ethyl alcohol, heating the melamine-formaldehyde resin foam to 800 ℃ at the speed of 5 ℃/min under the condition of inert atmosphere, preserving the temperature for 5 hours for thermal cracking, and cooling the melamine-formaldehyde resin foam to the normal temperature along with a furnace to obtain a conductive three-dimensional carbon foam framework; the photographs of the appearance before and after thermal cracking are shown in FIG. 1; SEM photographs of the three-dimensional carbon foam skeleton are shown in fig. 2;
immersing the three-dimensional carbon foam framework into the graphene oxide dispersion liquid for 20min, and repeatedly extruding the three-dimensional carbon foam framework to ensure saturated adsorption to obtain carbon foam adsorbed with graphene oxide;
placing the partition plate with the sieve pore structure in a centrifuge tube or a centrifuge bottle, taking out the carbon foam adsorbed with the graphene oxide or graphene oxide-based composite material, placing the carbon foam on the partition plate of the centrifuge tube or the centrifuge bottle, and then placing the centrifuge tube or the centrifuge bottle in a centrifuge; starting a centrifugal machine, and realizing solid-liquid separation through a partition plate under the centrifugal action, wherein the rotating speed of the centrifugal machine is 10000rpm, and the centrifugal time is 5 min; the liquid phase is separated graphene oxide dispersion liquid, the solid phase is a three-dimensional carbon foam framework wrapping graphene oxide nano sheets, and the three-dimensional carbon foam/graphene oxide composite material is prepared by drying the three-dimensional carbon foam framework at 60 ℃ for 60 min; 3% of graphene oxide by weight; the SEM photograph is shown in FIG. 3.
Example 2
The method is the same as example 1, except that:
(1) the concentration of the graphene oxide dispersion liquid is 2.0 mg/mL;
(2) heating to 1000 ℃ at the speed of 10 ℃/min, and preserving heat for 2h for cracking;
(3) soaking for 10 min;
(4) the rotating speed of the centrifuge is 2000rpm, and the centrifugation time is 10 min;
(5) and drying the solid phase at 80 ℃ for 30min, wherein the solid phase contains 9% of graphene oxide by weight percentage.
Example 3
The method is the same as example 1, except that:
(1) the concentration of the graphene oxide dispersion liquid is 6.0 mg/mL;
(2) heating to 900 ℃ at the speed of 8 ℃/min, and preserving heat for 3h for cracking;
(3) soaking for 3 min;
(4) the rotating speed of the centrifuge is 500rpm, and the centrifuging time is 20 min;
(5) and drying the solid phase at 70 ℃ for 45min, wherein the solid phase contains 16% of graphene oxide by weight percent.
Example 4
The graphene oxide-based composite material dispersion liquid adopted is graphene oxide/polyaniline dispersion liquid with the concentration of 3.5mg/mL, and the preparation method comprises the following steps:
mixing 10mL of hydrochloric acid with the concentration of 2mol/L and 10mL of graphene oxide solution with the concentration of 6mg/mL, uniformly stirring, adding 1mL of aniline, and uniformly stirring to obtain solution A; 0.93g of ammonium persulfate is dissolved in 20mL of hydrochloric acid with the concentration of 1mol/L and is uniformly stirred to be used as a solution B; respectively putting the A, B solution into ice water with the temperature not more than 5 ℃ for cooling for 10min, then pouring the B solution into the A solution, stirring for 2min, putting into an ice water bath with the temperature not more than 5 ℃ for standing reaction for 24h, centrifuging after the reaction is finished, washing with water until the filtrate is neutral, and then adding water to prepare 3.5mg/mL graphene oxide/polyaniline dispersion;
cleaning melamine-formaldehyde resin foam with distilled water and ethanol respectively, immersing the melamine-formaldehyde resin foam in absolute ethyl alcohol for ultrasonic treatment, washing off impurities, taking out the melamine-formaldehyde resin foam, air-drying the melamine-formaldehyde resin foam to remove the absolute ethyl alcohol, heating the melamine-formaldehyde resin foam to 800 ℃ at the speed of 5-10 ℃/min under the condition of inert atmosphere, preserving the temperature for 5 hours for thermal cracking, and cooling the melamine-formaldehyde resin foam to the normal temperature along with a furnace to obtain a conductive three-dimensional carbon foam framework;
immersing the three-dimensional carbon foam framework into the graphene oxide/polyaniline dispersion liquid for 3min, and repeatedly extruding the three-dimensional carbon foam framework to ensure saturated adsorption to obtain carbon foam adsorbed with the graphene oxide-based composite material;
placing the partition plate with the sieve pore structure in a centrifuge tube or a centrifuge bottle, taking out the carbon foam adsorbed with the graphene oxide-based composite material, placing the carbon foam on the partition plate of the centrifuge tube or the centrifuge bottle, and then placing the centrifuge tube or the centrifuge bottle in the centrifuge; starting a centrifugal machine, and realizing solid-liquid separation through a partition plate under the centrifugal action, wherein the rotating speed of the centrifugal machine is 7000rpm, and the centrifugal time is 5 min; the liquid phase is separated graphene oxide-based composite dispersion liquid, and the solid phase is a three-dimensional carbon foam framework wrapping graphene oxide-based composite nanosheets. Baking the mixture at 60 ℃ for 120min to prepare a three-dimensional carbon foam/graphene oxide-based composite material; 5.3 percent of graphene oxide-based composite material according to weight percentage.
Example 5
The graphene oxide-based composite material dispersion liquid adopted is graphene oxide/manganese dioxide dispersion liquid with the concentration of 4.0mg/mL, and the preparation method comprises the following steps:
adding 60mg of potassium permanganate into 50mL of graphene oxide aqueous solution with the concentration of 2.0mg/mL for ultrasonic treatment for 5min, magnetically stirring for 30min to uniformly disperse the potassium permanganate, then placing the potassium permanganate into a polytetrafluoroethylene reaction kettle, carrying out hydrothermal treatment in an oven at 150 ℃ for 12h, naturally cooling, carrying out centrifugal separation, washing a solid phase for three times, and then adding water to prepare graphene oxide/manganese dioxide dispersion with the concentration of 4.0 mg/mL;
the rest of the process was the same as example 4 except that:
(1) heating to 850 ℃ at the speed of 5-10 ℃/min, preserving heat for 4.5h for thermal cracking,
(2) immersing the three-dimensional carbon foam framework into the graphene oxide/manganese dioxide dispersion liquid for 5 min;
(3) the rotating speed of the centrifuge is 8000rpm, and the centrifuging time is 8 min;
(4) and drying the solid phase at 65 ℃ for 50min, wherein the graphene oxide-based composite material is 5% by weight.
Example 6
The graphene oxide-based composite material dispersion liquid adopted is graphene oxide/tin hydroxide dispersion liquid with the concentration of 4.5mg/mL, and the preparation method comprises the following steps:
adding 90mg of sodium stannate trihydrate into 40mL of graphene oxide aqueous solution with the concentration of 3mg/mL for ultrasonic treatment for 5min, magnetically stirring for 30min, adding 120mg of urea for continuous ultrasonic treatment for 5min to uniformly disperse the urea, putting the mixture into a polytetrafluoroethylene reaction kettle, carrying out hydrothermal treatment in an oven at 180 ℃ for 24h, naturally cooling, carrying out centrifugal separation, washing a solid phase until the filtrate is neutral, and adding water to prepare graphene oxide/tin hydroxide dispersion with the concentration of 4.5 mg/mL.
The rest of the process was the same as example 4 except that:
(1) raising the temperature to 1000 ℃ at the speed of 5-10 ℃/min, preserving the temperature for 3 hours for thermal cracking,
(2) immersing the three-dimensional carbon foam skeleton into graphene oxide/tin hydroxide dispersion liquid for 15 min;
(3) the rotating speed of the centrifuge is 2000rpm, and the centrifuging time is 15 min;
(4) and drying the solid phase at 80 ℃ for 30min, wherein the graphene oxide-based composite material is 12% by weight.
Example 7
The graphene oxide-based composite material dispersion liquid adopted is graphene oxide/nickel hydroxide dispersion liquid with the concentration of 5.0mg/mL, and the preparation method comprises the following steps:
adding 70mg of nickel nitrate hexahydrate into 50mL of graphene oxide aqueous solution with the concentration of 2.5mg/mL, performing ultrasonic treatment for 5min, performing magnetic stirring for 30min, adding 60mg of urea, performing ultrasonic treatment for 10min continuously to disperse the urea uniformly, then placing the mixture into a polytetrafluoroethylene reaction kettle, performing hydrothermal treatment in an oven at 160 ℃ for 12h, naturally cooling, performing centrifugal separation, washing a solid phase until the filtrate is neutral, and then adding water to prepare graphene oxide/nickel hydroxide dispersion with the concentration of 5.0 mg/mL;
the rest of the process was the same as example 4 except that:
(1) heating to 950 ℃ at the speed of 5-10 ℃/min, preserving the heat for 2.5h for thermal cracking,
(2) immersing the three-dimensional carbon foam skeleton into the graphene oxide/nickel hydroxide dispersion liquid for 18 min;
(3) the rotating speed of the centrifuge is 1000rpm, and the centrifugation time is 18 min;
(4) and drying the solid phase at 75 ℃ for 40min, wherein the graphene oxide-based composite material is 13% by weight.
Example 8
The graphene oxide-based composite material dispersion liquid adopted is graphene oxide/cobalt hydroxide dispersion liquid with the concentration of 6.0mg/mL, and the preparation method comprises the following steps:
adding 80mg of cobalt acetate tetrahydrate into 60mL of graphene oxide aqueous solution with the concentration of 2.0mg/mL, performing ultrasonic treatment for 5min, performing magnetic stirring for 30min, adding 120mg of hexamethylenetetramine, continuing ultrasonic treatment for 5min to uniformly disperse the mixture, then putting the mixture into a polytetrafluoroethylene reaction kettle, performing hydrothermal treatment for 10h in an oven at 150 ℃, performing centrifugal separation after natural cooling, washing a solid phase until the filtrate is neutral, and adding water to prepare a dispersion solution with the concentration of 6.0 mg/mL;
the rest of the process was the same as example 4 except that:
(1) heating to 900 ℃ at the speed of 5-10 ℃/min, preserving the heat for 2h for thermal cracking,
(2) immersing the three-dimensional carbon foam skeleton into the graphene oxide/cobalt hydroxide dispersion liquid for 20 min;
(3) the rotating speed of the centrifuge is 500rpm, and the centrifuging time is 20 min;
(4) and drying the solid phase at 70 ℃ for 50min, wherein the graphene oxide-based composite material is 16% by weight.
Claims (1)
1. A method for preparing a three-dimensional carbon foam/graphene oxide-based composite material by centrifugal separation is characterized by comprising the following steps:
(1) preparing a three-dimensional carbon foam framework: cleaning melamine-formaldehyde resin foam with distilled water and ethanol respectively, immersing the melamine-formaldehyde resin foam in absolute ethyl alcohol for ultrasonic treatment, washing off impurities, taking out the melamine-formaldehyde resin foam, drying or air-drying the melamine-formaldehyde resin foam to remove the absolute ethyl alcohol, heating to 800-1000 ℃ at the speed of 5-10 ℃/min under the condition of inert atmosphere, preserving heat for 2-5 hours for thermal cracking, cooling to the normal temperature along with a furnace, and preparing a conductive three-dimensional carbon foam framework;
(2) carbon foam adsorption: immersing the three-dimensional carbon foam framework into the graphene oxide dispersion liquid for 3-20 min, and repeatedly extruding the three-dimensional carbon foam framework to ensure saturated adsorption to obtain carbon foam adsorbed with graphene oxide; the concentration of the graphene oxide dispersion liquid is 0.5-6.0 mg/mL; the graphene oxide dispersion liquid is prepared by a Hummers method;
(3) centrifugal separation: placing the partition plate with the sieve pore structure in a centrifuge tube or a centrifuge bottle, taking out the carbon foam adsorbed with the graphene oxide, placing the carbon foam on the partition plate of the centrifuge tube or the centrifuge bottle, and then placing the centrifuge tube or the centrifuge bottle in the centrifuge; starting a centrifugal machine, and realizing solid-liquid separation through a partition plate under the centrifugal action, wherein a liquid phase is separated graphene oxide dispersion liquid, and a solid phase is a three-dimensional carbon foam framework wrapping graphene oxide nanosheets; the rotating speed of a centrifugal machine is 500-10000 rpm when centrifugal separation is carried out, and the centrifugal time is 5-20 min;
(4) drying the solid phase to remove water, wherein the drying temperature is 60-80 ℃, and the drying time is 30-120 min, so as to prepare the three-dimensional carbon foam/graphene oxide-based composite material; the weight percentage of the graphene oxide in the three-dimensional carbon foam/graphene oxide-based composite material is 3-16%.
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| CN109728268B (en) * | 2018-12-14 | 2020-11-20 | 北京理工大学 | Flexible self-supporting composite material, preparation method and application thereof |
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