CN111533113A - Preparation method of nano porous graphene - Google Patents
Preparation method of nano porous graphene Download PDFInfo
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- CN111533113A CN111533113A CN202010521141.3A CN202010521141A CN111533113A CN 111533113 A CN111533113 A CN 111533113A CN 202010521141 A CN202010521141 A CN 202010521141A CN 111533113 A CN111533113 A CN 111533113A
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- graphene
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- foamed nickel
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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
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
Abstract
The invention relates to a preparation method of a nano graphene material, which comprises the steps of carrying out etching pretreatment on a traditional foam substrate for growing graphene to obtain a foam substrate with a nano porous structure, and growing graphene on the surface of the foam substrate after reduction to obtain the graphene material with rich nano porous structures.
Description
Technical Field
The invention relates to a preparation method of a graphene capacitor material, in particular to a preparation method of a nano graphene material.
Background
Graphene is a novel two-dimensional structure material, is formed by tightly stacking sp2 hybridized atoms and comprises a plurality of atomic layer graphene nanosheets. The graphene has excellent electronic characteristics, high specific surface area, good mechanical toughness and wide application prospect.
Especially for application in supercapacitors, theoretically, a single layer of graphene sheets can provide about 2675m2Specific external surface area/g, and maximum specific capacitance 550F/g. However, in practical applications, single graphene sheets tend to be stacked again to form a multi-layer graphene structure, and the interlayer spacing of the multi-layer graphene structure is small, so that the outer surface of the multi-layer graphene structure can be used as an effective surface of a supercapacitor, and thus the specific outer surface area of graphene is greatly reduced, and the specific capacitance is only 90-170F/g.
In order to increase the specific external surface area of graphene applied to a supercapacitor, researchers have attempted to prepare graphene by injecting a mixed slurry containing graphene sheets and an electrolyte into the pores of a foam matrix, abandoning subsequent drying and compression, and avoiding re-stacking of graphene sheets. However, the pores of the common foam substrate are all in the micron level, and accordingly, the porous structure of the obtained graphene is also in the micron level, and although the prepared graphene has a certain promotion effect on the application of the graphene in the super capacitor due to the increase of the micron-level pores, the effect is still limited.
Therefore, the invention aims to provide a preparation method of the nano-porous graphene material.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a method for preparing a nano-porous graphene material, in the method, a traditional foam substrate for growing graphene is etched to obtain a foam substrate with a nano-porous structure, and graphene grows on the surface of the foam substrate after reduction, so that the graphene material with rich nano-porous structures can be obtained.
A preparation method of a nano-porous graphene material comprises the following steps:
preparation of nano porous foamed nickel
A. Carrying out acid cleaning treatment on the foamed nickel substrate, removing a surface oxidation film, then washing the foamed nickel substrate to be neutral by using deionized water and drying the foamed nickel substrate for later use;
B. b, placing the foamed nickel substrate obtained in the step A into a reaction kettle containing a urea solution for hydrothermal reaction at the temperature of 120 ℃ and 140 ℃ for 1-3 hours, taking out the foamed nickel substrate, washing and drying to obtain the foamed nickel substrate with the surface of a nano porous structure;
C. surface reduction, namely placing the foamed nickel substrate obtained in the step B in a reducing atmosphere for surface reduction, and reducing nickel oxides such as nickel oxide, nickel hydroxide, basic nickel carbonate and the like generated on the surface of the foamed nickel after hydrothermal reaction into a nickel simple substance to obtain a nano porous foamed nickel substrate which is used as a substrate for growing nano porous graphene;
growth of nanoporous graphene
D. Depositing graphene on the surface of the nano-porous foamed nickel substrate prepared in the step C by adopting a chemical vapor deposition method to obtain nano-porous graphene; the deposition time is 5-15 min;
removal of nano porous foam nickel substrate
And E, placing the nano porous foam nickel substrate with the nano porous graphene grown in the step D in an etching solution, and etching and removing the nano porous foam nickel substrate to obtain the single nano porous graphene.
Wherein the reducing atmosphere comprises hydrogen.
Further, the nano-porous graphene grown in the step D is reduced graphene or nitrogen-doped graphene.
Further, in the chemical vapor deposition method in step D, the nanoporous foam nickel substrate is heated to the growth temperature in advance, and then heated to 100-400 ℃ in a reducing atmosphere by using a carbon source or a nitrogen-containing carbon source, so as to deposit and form the nitrogen-doped graphene on the surface of the substrate.
Wherein the growth temperature is 700 ℃ and 900 ℃.
Further, the etching solution of step E is hydrochloric acid or ferric chloride solution.
In addition, in order to facilitate the transfer or pick-and-place of the prepared nanoporous graphene, a step F of depositing a PMMA thin layer on the surface of the nanoporous graphene is preferably performed between the steps D and E.
The preparation method of the nano porous graphene material provided by the invention has the following characteristics:
1. the method comprises the steps of carrying out hydrothermal etching treatment on common foamed nickel with micron-sized pores in advance, carrying out surface reduction to obtain a foamed nickel substrate with a nano-porous structure on the surface, and directly using the nano-porous foamed nickel substrate as a substrate for inducing growth of graphene, so that nano-porous graphene can be obtained, the proportion of the pore structure on the surface of the graphene can be effectively increased, and the specific capacitance of a graphene super capacitor can be effectively increased.
2. The method is simple, convenient, high in uniformity and good in controllability. And preparing graphene on the surface of the nickel by chemical vapor deposition, wherein the graphene grows epitaxially, and a large number of nano holes are formed on the contact surface of the graphene on the nickel substrate after the nickel substrate is removed by etching. And moreover, the graphene is prepared by adopting chemical vapor deposition, the thickness is easy to control, and the required number of layers or the required thickness of the graphene can be obtained.
3. The nitrogen-containing carbon source is directly used as the only raw material and is heated in a reducing atmosphere, so that the nitrogen-doped graphene can be directly obtained without introducing other impurities.
Detailed Description
In the following, preferred embodiments of the present invention and corresponding comparative examples are combined for comparative explanation so as to explain the technical effects of the present invention in detail.
Example 1
A preparation method of a nano-porous graphene material comprises the following steps:
preparation of nano porous foamed nickel
A. Carrying out acid cleaning treatment on the foamed nickel substrate, removing a surface oxidation film, then washing the foamed nickel substrate to be neutral by using deionized water and drying the foamed nickel substrate for later use;
B. b, placing the foamed nickel substrate obtained in the step A into a reaction kettle containing a urea solution for hydrothermal reaction at the temperature of 120 ℃ for 3 hours, taking out the foamed nickel substrate, washing and drying to obtain the foamed nickel substrate with the surface of a nano porous structure;
C. surface reduction, namely placing the foamed nickel substrate obtained in the step B in a hydrogen atmosphere for surface reduction, and reducing nickel oxides such as nickel oxide, nickel hydroxide, basic nickel carbonate and the like generated on the surface of the foamed nickel after hydrothermal reaction into a nickel simple substance to obtain a nano porous foamed nickel substrate which is used as a substrate for growing nano porous graphene;
growth of nanoporous graphene
D. Depositing graphene on the surface of the nano-porous foamed nickel substrate prepared in the step C by adopting a chemical vapor deposition method to obtain nano-porous graphene; the deposition time is 5 min;
removal of nano porous foam nickel substrate
And E, placing the nano porous foam nickel substrate with the nano porous graphene grown in the step D in a hydrochloric acid solution, and etching and removing the nano porous foam nickel substrate to obtain the single nano porous graphene.
In the chemical vapor deposition method in step D, the nanoporous foam nickel substrate is heated to 700 ℃ in advance, and then heated to 400 ℃ in a reducing atmosphere using a carbon source to deposit reduced graphene on the surface of the substrate.
Example 2
A preparation method of a nano-porous graphene material comprises the following steps:
preparation of nano porous foamed nickel
A. Carrying out acid cleaning treatment on the foamed nickel substrate, removing a surface oxidation film, then washing the foamed nickel substrate to be neutral by using deionized water and drying the foamed nickel substrate for later use;
B. b, placing the foamed nickel substrate obtained in the step A into a reaction kettle containing a urea solution for hydrothermal reaction at the temperature of 130 ℃ for 2 hours, taking out the foamed nickel substrate, washing and drying to obtain the foamed nickel substrate with the surface of a nano porous structure;
C. surface reduction, namely placing the foamed nickel substrate obtained in the step B in a hydrogen atmosphere for surface reduction, and reducing nickel oxides such as nickel oxide, nickel hydroxide, basic nickel carbonate and the like generated on the surface of the foamed nickel after hydrothermal reaction into a nickel simple substance to obtain a nano porous foamed nickel substrate which is used as a substrate for growing nano porous graphene;
growth of nanoporous graphene
D. Depositing graphene on the surface of the nano-porous foamed nickel substrate prepared in the step C by adopting a chemical vapor deposition method to obtain nano-porous graphene; the deposition time is 10 min;
removal of nano porous foam nickel substrate
And E, placing the nano porous foam nickel substrate with the nano porous graphene grown in the step D in a hydrochloric acid solution, and etching and removing the nano porous foam nickel substrate to obtain the single nano porous graphene.
In the chemical vapor deposition method in the step D, the nanoporous foam nickel substrate is heated to 800 ℃ in advance, and then heated to 200 ℃ in a reducing atmosphere by using a nitrogen-containing carbon source to deposit and form the nitrogen-doped graphene on the surface of the substrate.
Example 3
A preparation method of a nano-porous graphene material comprises the following steps:
preparation of nano porous foamed nickel
A. Carrying out acid cleaning treatment on the foamed nickel substrate, removing a surface oxidation film, then washing the foamed nickel substrate to be neutral by using deionized water and drying the foamed nickel substrate for later use;
B. b, placing the foamed nickel substrate obtained in the step A into a reaction kettle containing a urea solution for hydrothermal reaction at the temperature of 140 ℃ for 1 hour, taking out the foamed nickel substrate, washing and drying to obtain the foamed nickel substrate with the surface of a nano porous structure;
C. surface reduction, namely placing the foamed nickel substrate obtained in the step B in a hydrogen atmosphere for surface reduction, and reducing nickel oxides such as nickel oxide, nickel hydroxide, basic nickel carbonate and the like generated on the surface of the foamed nickel after hydrothermal reaction into a nickel simple substance to obtain a nano porous foamed nickel substrate which is used as a substrate for growing nano porous graphene;
growth of nanoporous graphene
D. Depositing graphene on the surface of the nano-porous foamed nickel substrate prepared in the step C by adopting a chemical vapor deposition method to obtain nano-porous graphene; the deposition time is 15 min;
F. depositing a PMMA thin layer on the surface of the nano porous graphene;
removal of nano porous foam nickel substrate
E, placing the nano porous foam nickel substrate with the nano porous graphene grown in the step D in an iron chloride solution, and etching and removing the nano porous foam nickel substrate to obtain single nano porous graphene;
in the chemical vapor deposition method in step D, the nanoporous foam nickel substrate is heated to 900 ℃ in advance, and then heated to 100 ℃ in a reducing atmosphere using a carbon source to deposit and form the nitrogen-doped graphene on the surface of the substrate.
Comparative example 1
With reference to example 1, steps B and C are omitted, the nickel foam obtained in step a is directly used as a substrate, and reduced graphene is deposited on the surface of the nickel foam by a chemical vapor deposition method.
Comparative example 2
With the example 2 as a reference, the steps B and C are omitted, the foamed nickel obtained in the step a is directly used as a substrate, and nitrogen-doped graphene is deposited on the surface of the foamed nickel by a chemical vapor deposition method.
In order to test the performance and effect of the graphene prepared by the present invention applied to a supercapacitor, the graphene prepared in examples 1 to 3 and comparative examples 1 to 2 was prepared into a supercapacitor, and the active mass load per unit area, the energy density per unit weight, and the volumetric energy density were tested, and the results are shown in the following table. Wherein the electrolyte used in the test was a 1mol/L sodium chloride solution.
| Graphene thickness (nm) | Active mass load per unit area (g/cm)2） | Energy Density per weight (Wh/kg) | Volumetric energy density (Wh/L) | |
| Example 1 | 1 | 35 | 56 | 44 |
| Example 2 | 2 | 37 | 58 | 41 |
| Example 3 | 2.5 | 36 | 59 | 39 |
| Comparative example 1 | 1 | 25 | 40 | 30 |
| Comparative example 2 | 2 | 26 | 42 | 29 |
As can be seen from the above table, the graphene prepared by the method provided by the invention has excellent active mass load per unit area, energy density per unit weight and volume energy density when applied to a super capacitor.
The invention provides a preparation method of a nano-porous graphene material. It should be noted that, for those skilled in the art of graphene, appropriate modifications or changes can be made to the present invention, and such modifications or changes also fall within the protection scope of the present invention.
Claims (8)
1. A preparation method of a nano-porous graphene material comprises the following steps:
preparation of nano porous foamed nickel
A. Carrying out acid cleaning treatment on the foamed nickel substrate, removing a surface oxidation film, then washing the foamed nickel substrate to be neutral by using deionized water and drying the foamed nickel substrate for later use;
B. b, placing the foamed nickel substrate obtained in the step A into a reaction kettle containing a urea solution for hydrothermal reaction at the temperature of 120 ℃ and 140 ℃ for 1-3 hours, taking out the foamed nickel substrate, washing and drying to obtain the foamed nickel substrate with the surface of a nano porous structure;
C. surface reduction, namely placing the foamed nickel substrate obtained in the step B in a reducing atmosphere for surface reduction, and reducing nickel oxides such as nickel oxide, nickel hydroxide, basic nickel carbonate and the like generated on the surface of the foamed nickel after hydrothermal reaction into a nickel simple substance to obtain a nano porous foamed nickel substrate which is used as a substrate for growing nano porous graphene;
growth of nanoporous graphene
D. Depositing graphene on the surface of the nano-porous foamed nickel substrate prepared in the step C by adopting a chemical vapor deposition method to obtain nano-porous graphene; the deposition time is 5-15 min;
removal of nano porous foam nickel substrate
And E, placing the nano porous foam nickel substrate with the nano porous graphene grown in the step D in an etching solution, and etching and removing the nano porous foam nickel substrate to obtain the single nano porous graphene.
2. The method for preparing a nanoporous graphene material according to claim 1, wherein: wherein the reducing atmosphere comprises hydrogen.
3. The method for preparing a nanoporous graphene material according to claim 1, wherein: and D, the nano porous graphene grown in the step D is reduced graphene or nitrogen-doped graphene.
4. The method for preparing a nanoporous graphene material according to claim 3, wherein: in the chemical vapor deposition method in the step D, the nanoporous foam nickel substrate is heated to the growth temperature in advance, and then the carbon source or the nitrogen-containing carbon source is heated to 100-400 ℃ in the reducing atmosphere to deposit and form the nitrogen-doped graphene on the surface of the substrate.
5. The method for preparing a nanoporous graphene material according to claim 4, wherein: the growth temperature is 700 ℃ and 900 ℃.
6. The method for preparing a nanoporous graphene material according to claim 1, wherein: and E, the etching solution is hydrochloric acid or ferric chloride solution.
7. The method for preparing a nanoporous graphene material according to claim 1, wherein: and F, performing a step of depositing a PMMA thin layer on the surface of the nano-porous graphene.
8. A nanoporous graphene material prepared by the method of any one of claims 1 to 7.
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| CN202010521141.3A CN111533113A (en) | 2020-06-10 | 2020-06-10 | Preparation method of nano porous graphene |
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| CN202010521141.3A CN111533113A (en) | 2020-06-10 | 2020-06-10 | Preparation method of nano porous graphene |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102013330A (en) * | 2010-11-16 | 2011-04-13 | 浙江大学 | Film for graphene/porous nickel oxide composite super capacitor and preparation method thereof |
| CN102674321A (en) * | 2011-03-10 | 2012-09-19 | 中国科学院金属研究所 | Graphene foam with three dimensional fully connected network and macroscopic quantity preparation method thereof |
| US20140030590A1 (en) * | 2012-07-25 | 2014-01-30 | Mingchao Wang | Solvent-free process based graphene electrode for energy storage devices |
| US20140110049A1 (en) * | 2012-10-19 | 2014-04-24 | The Hong Kong University Of Science And Technology | Three Dimensional Interconnected Porous Graphene-Based Thermal Interface Materials |
| CN105244191A (en) * | 2015-10-27 | 2016-01-13 | 渤海大学 | Manganese cobalt oxide porous nanometer sheet/foam nickel compound electrode material preparation method |
| CN108677191A (en) * | 2018-05-30 | 2018-10-19 | 大连交通大学 | A kind of nano wire skeleton three-dimensional porous foams nickel and preparation method thereof |
-
2020
- 2020-06-10 CN CN202010521141.3A patent/CN111533113A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102013330A (en) * | 2010-11-16 | 2011-04-13 | 浙江大学 | Film for graphene/porous nickel oxide composite super capacitor and preparation method thereof |
| CN102674321A (en) * | 2011-03-10 | 2012-09-19 | 中国科学院金属研究所 | Graphene foam with three dimensional fully connected network and macroscopic quantity preparation method thereof |
| US20140030590A1 (en) * | 2012-07-25 | 2014-01-30 | Mingchao Wang | Solvent-free process based graphene electrode for energy storage devices |
| US20140110049A1 (en) * | 2012-10-19 | 2014-04-24 | The Hong Kong University Of Science And Technology | Three Dimensional Interconnected Porous Graphene-Based Thermal Interface Materials |
| CN105244191A (en) * | 2015-10-27 | 2016-01-13 | 渤海大学 | Manganese cobalt oxide porous nanometer sheet/foam nickel compound electrode material preparation method |
| CN108677191A (en) * | 2018-05-30 | 2018-10-19 | 大连交通大学 | A kind of nano wire skeleton three-dimensional porous foams nickel and preparation method thereof |
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