CN106803461A - Directly soak the three-dimensional porous electrode preparation method of nickel foam-Graphene of reaction equation - Google Patents

Directly soak the three-dimensional porous electrode preparation method of nickel foam-Graphene of reaction equation Download PDF

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CN106803461A
CN106803461A CN201510833005.7A CN201510833005A CN106803461A CN 106803461 A CN106803461 A CN 106803461A CN 201510833005 A CN201510833005 A CN 201510833005A CN 106803461 A CN106803461 A CN 106803461A
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nickel foam
graphene
reaction
dimensional porous
foam
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余兴华
易秋珍
钟建夫
朱济群
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CHANGDE LIYUAN NEW MATERIAL Co Ltd
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CHANGDE LIYUAN NEW MATERIAL Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/36Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention discloses a kind of three-dimensional porous electrode preparation method of nickel foam Graphene for directly soaking reaction equation, nickel foam is cleaned using glacial acetic acid, acetone and ethanol successively, then dried placement after deionized water is cleaned;It is the graphene oxide water solution of 0.5mg/mL 5mg/mL to prepare mass concentration, then nickel foam is directly dipped into and wherein stands reaction, and reaction temperature is controlled as 30 °C 80 °C in this immersion process, soak time is 6 hours 2 hours, is consequently formed the nickel foam graphite ene product of three-dimensional porous structure.By the present invention, reduction reaction is rapidly completed by an immersion process that is simple, being easy to manipulation can only be passed through, and the Graphene of Direct precipitation growth in its surface of the substrate enhancement effect based on nickel foam, ultimately form the product of three-dimensional porous structure and high-specific surface area, overall reaction rate is accordingly drastically increased, and is particularly suited for high-volume large-scale production purposes.

Description

Directly soak the three-dimensional porous electrode preparation method of nickel foam-Graphene of reaction equation
Technical field
The invention belongs to combination electrode material preparation field, more particularly to a kind of three-dimensional porous electrode preparation method of nickel foam-Graphene for directly soaking reaction equation.
Background technology
Graphene is a kind of new carbon tightly packed by single layer of carbon atom, and its cellular crystal structure of unique hexagonal imparts the performances such as its excellent electricity, calorifics and mechanics and is widely used in electrode material, catalyst carrier, the absorption of gas and storage and the numerous areas such as separates.But the two-dimensional structure feature of Graphene causes that it is easy to reunite, directly reduce its specific surface area, limit the practical application of grapheme material, and it is then a kind of effective means for realizing its practical application that two-dimensional structure grapheme material is assembled into three-dimensional macro loose structure.
In the prior art, Chinese Academy of Sciences's chemistry grind make internal disorder or usurp Liu Yunqi et al. propose using the method for chemical vapor deposition, realize the three-dimensional structure of Graphene first on metal foam substrate, wherein by after metal foam substrate etching, the three-dimensional hollow porous network structure grapheme foam for obtaining has excellent conductive capability, huge specific surface area and heat endurance and chemical stability high, it is widely used in terms of high efficiency energy storage.Additionally, disclosing a kind of heating furnace for being up to 500 °C even 1100 °C using temperature in CN103903880A, CN102931437A the method that reduces generation nickel foam-Graphene electrode of super capacitor;Both disclose to first pass through immersion way and obtain deposition in the CN103258656A that CN103680974A, CN103545121A and inventor oneself propose early stage and have the nickel foam of graphene oxide, then reduction reaction is performed using electrode method, ascorbic acid or high-temperature heating method, so as to the method for being reduced into Graphene and be deposited on foam nickel surface graphene oxide.
But, further grind to make internal disorder or usurp and show, above-mentioned prior art is required to perform bar none extra, cumbersome reduction reaction so that graphene oxide is become into Graphene, either chemical gas-phase method, high-temperature heating or chemical reduction method, its expensive depositing device in these schemes(Tube furnace)And maintenance cost, and complexity preparation section and hot environment etc., the quality that accordingly all can greatly limit technique is handling, and significantly improves the cost of manufacture of material, thus as directly affecting the unfavorable factor of grapheme foam commercialized development.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art,The invention provides a kind of three-dimensional porous electrode preparation method of nickel foam-Graphene for directly soaking reaction equation,The concrete technology condition for wherein particularly soaking reaction by the type to its key reaction thing grind and makes internal disorder or usurp and design,Compared with the mode for performing all kinds of reduction reactions again after graphene oxide-foam nickel composite material is obtained in the prior art,Can only by simple,Reduction reaction is rapidly completed by an immersion process for being easy to manipulation,And the Graphene of Direct precipitation growth in its surface of the substrate enhancement effect based on nickel foam,Ultimately form the product of three-dimensional porous structure and high-specific surface area,Accordingly drastically increase overall reaction rate,Its foam product function admirable,Stability is high,It is provided simultaneously with technique and is easy to manipulation,Environmental protection,Low cost and the advantage of low energy consumption,It is therefore particularly suitable for the Graphene composite foam production occasion of high-volume large-scale production.
A kind of three-dimensional porous electrode preparation method of nickel foam-Graphene for directly soaking reaction equation, it is characterised in that the method comprises the following steps:
A () is cleaned nickel foam using glacial acetic acid, acetone and ethanol successively, then dry placement after deionized water is cleaned;
B it is the graphene oxide water solution of 0.5mg/mL 10mg/mL that () prepares mass concentration, then by step(A) nickel foam after processing directly is dipped into and wherein stands reaction, and reaction temperature is controlled as 30 °C 80 °C in this immersion process, and soak time is 12 hours 2 hours;In this way, in immersion process there is reduction reaction in Graphene, and spontaneous deposition is grown to Graphene on the foam nickel surface as conductive substrates, ultimately form the nickel foam-graphite ene product of three-dimensional porous structure.
Conceive more than, by the control to its key reaction parameter such as soak time, soaking temperature and charge ratio, an immersion process that is simple, being easy to manipulation can only be passed through, can be in the case of without other extra operations, graphene oxide is directly reduced into Graphene and spontaneous uniform deposition is grown on the surface of nickel foam, accordingly drastically increase overall reaction rate;At the same time, nickel foam acts not only as conductive substrates and carrys out deposited graphite alkene, also serve as the support frame and electrode current collecting body of three-dimensional grapheme structure, the grapheme foam electrode for so being obtained can make full use of the high-specific surface area of foam nickel base, so that the specific surface area of electrode material is significantly improved, the electrode material of the energy storage devices such as ultracapacitor, lithium ion battery and lithium-air battery is therefore particularly suitable for, while being also applied for loading nanometer electroactive material(Such as metal oxide or conducting polymer), further to lift the electrochemical energy storage characteristic of electrode.
As it is further preferred that in step(B) in, it is preferred to use aoxidize stripping method to prepare the graphene oxide water solution, and its mass concentration is further configured to 1mg/mL 2.5mg/mL.
As it is further preferred that in step(B) in, the reaction temperature is preferably 70 DEG C of 60C, and soak time is 6 hours 4 hours.
As it is further preferred that in step(B) in, the reaction temperature is most preferably from about 60 DEG C, and soak time is controlled to 6 hours or so.
As it is further preferred that in step(B) after, can also continue through electrochemistry potentiostatic electrodeposition technology to load polypyrrole or nano-manganese dioxide on the basis of the nickel foam of the three-dimensional porous structure for being formed-graphite ene product.
As it is further preferred that the above-mentioned three-dimensional porous electrode of nickel foam-Graphene preferably as ultracapacitor, lithium ion battery or lithium-air battery electrode.
In general, possesses following technological merit compared with prior art, mainly by the contemplated above technical scheme of the present invention:
1st, the critical craft for particularly soaking reaction by the type to key reaction thing grind and makes internal disorder or usurp and design, can be in the case where being reduced without cumbersome electrode, only pass through once immersion that is simple, being easy to manipulation, can obtain go back original production Graphene directly on a surface in nickel foam and form three-dimensional porous foam type structure, while the substrate enhancement effect based on nickel foam further improves reaction speed and product property;
2nd, the aspect that makes internal disorder or usurp is being ground to reaction mechanism, the nickel foam used in the present invention acts not only as conductive substrates for spontaneous deposited graphite alkene, the support frame of three-dimensional grapheme structure is also used as, especially promotes Graphene in the autonomous growth on its surface as electrode current collecting body in immersion;The composite foam product for being obtained possesses high-specific surface area, and the corresponding specific surface area for causing electrode material is significantly increased;
3rd, it is extensive according to preparation method raw material sources of the invention, and possess the advantage for being easy to manipulation, environmental protection, low cost and low energy consumption, it is therefore particularly suitable for the large-batch industrial scale manufacturing occasion of the load nanometer electroactive material of ultracapacitor, lithium ion battery and lithium-air battery etc energy storage device and metal oxide or conducting polymer etc.
Brief description of the drawings
Fig. 1 is the scanning electron microscope diagram piece of the large-area three-dimensional porous graphene foam product obtained by embodiment 1;
Fig. 2 is the large-area three-dimensional porous graphene foam obtained by embodiment 1(After removing base is low)The X-ray powder diffraction comparison diagram of product and graphene oxide;
Fig. 3 is that resulting Graphene composite foam in embodiment 9 continues to load the high power scanning electron microscope diagram after manganese dioxide;
Fig. 4 is large-area three-dimensional porous graphene foam obtained by the Graphene composite foam and embodiment of resulting load manganese dioxide in embodiment 9 cyclic voltammetric contrast curve respectively in the case where sweep speed is 50mV/s.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with drawings and Examples, the present invention will be described in further detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not intended to limit the present invention.As long as additionally, technical characteristic involved in invention described below each implementation method does not constitute conflict each other can just be mutually combined.
Embodiment 1
Nickel foam is cut into for example as 1cm is (long first)X 1cm are (wide)X 1mm are (high)Size, then cleaned using glacial acetic acid, acetone and ethanol, then by deionized water clean about 5 minutes after dry placement;
Then, it is preferred to use oxidation stripping method(Hummers methods)To prepare the graphene oxide water solution that mass concentration is 0.5mg/mL 10mg/mL, its detailed process is as follows:Take 1g natural flake graphite powder, it is stirred with the sodium nitrate of the 23mL concentrated sulfuric acids and 0.5g under condition of ice bath and is mixed, then slowly to addition 3g potassium permanganate in solution, after stirring 2 hours, temperature is risen to 35 degree, after continuing to stir 2 hours, it is slowly added to the deionized water of 46mL, then temperature is further increased to 95 degree, and maintain 30 minutes, then to the deionized water that about 100mL is added in solution, temperature adjustment is to normal temperature, add the hydrogenperoxide steam generator of 2mL, solution suction filtration is obtained into solid, watery hydrochloric acid and deionized water centrifuge washing are used successively, can obtain graphene oxide solution.
Then, cleaned nickel foam is directly dipped into the graphene oxide water solution of 3mg/mL and stands reaction, as another key reaction condition of the invention, the reaction temperature of wherein integral system is controlled as 60 °C, soak time is 5 hours, realize in the process and be reduced directly graphene oxide in immersion as the nickel foam of substrate, and deposition growing is Graphene on the surface of nickel foam, reaction takes out nickel foam after terminating, and surface is cleaned with deionized water, that is, form the nickel foam-graphite ene product of three-dimensional porous structure.
Understand that graphene sheet layer is uniformly intactly to be coated on the skeleton of nickel foam with reference to the electron scanning micrograph of Fig. 1, form throughout three-dimensional network structure;Additionally, testing visible, the characteristic peak of graphene oxide with reference to the X-ray powder diffraction in Fig. 2(002) disappear, shifted to high angle, occur in that the characteristic peak of Graphene(002), illustrate that graphene oxide is successfully reduced to Graphene by nickel foam.
Embodiment 2
Nickel foam is cut into for example as 1cm is (long first)X 1cm are (wide)X 1mm are (high)Size, then cleaned using glacial acetic acid, acetone and ethanol, then by deionized water clean 5 minutes after dry placement;
Then, it is preferred to use oxidation stripping method(Hummers methods)To prepare graphene oxide water solution, and its key parameter is adjusted to mass concentration 0.5mg/mL, then cleaned nickel foam is directly soaked and wherein stands reaction, the reaction temperature of wherein integral system is controlled as 80 °C, soak time is 2 hours, in the process graphene oxide is reduced directly as the nickel foam of substrate in immersion, and deposition growing is Graphene on the surface of nickel foam, reaction takes out nickel foam after terminating, and nickel foam-graphite ene product that surface forms three-dimensional porous structure is cleaned with deionized water.
Embodiment 3
Nickel foam is cut into for example as 1cm is (long first)X 1cm are (wide)X 1mm are (high)Size, then cleaned using glacial acetic acid, acetone and ethanol, then by deionized water clean 5 minutes after dry placement;
Then, it is preferred to use oxidation stripping method(Hummers methods)To prepare graphene oxide water solution, and its key parameter is adjusted to mass concentration 5mg/mL, then cleaned nickel foam is directly soaked and wherein stands reaction, the reaction temperature of wherein integral system is controlled as 30 °C, soak time is 6 hours, in the process graphene oxide is reduced directly as the nickel foam of substrate in immersion, and deposition growing is Graphene on the surface of nickel foam, reaction takes out nickel foam after terminating, and nickel foam-graphite ene product that surface forms three-dimensional porous structure is cleaned with deionized water.
Embodiment 4
Nickel foam is cut into for example as 1cm is (long first)X 1cm are (wide)X 1mm are (high)Size, then cleaned using glacial acetic acid, acetone and ethanol, then by deionized water clean 5 minutes after dry placement;
Then, it is preferred to use oxidation stripping method(Hummers methods)To prepare graphene oxide water solution, and its key parameter is adjusted to mass concentration 1mg/mL, then cleaned nickel foam is directly soaked and wherein stands reaction, the reaction temperature of wherein integral system is controlled as 40 °C, soak time is 5 hours, in the process graphene oxide is reduced directly as the nickel foam of substrate in immersion, and deposition growing is Graphene on the surface of nickel foam, reaction takes out nickel foam after terminating, and nickel foam-graphite ene product that surface forms three-dimensional porous structure is cleaned with deionized water.
Embodiment 5
Nickel foam is cut into for example as 1cm is (long first)X 1cm are (wide)X 1mm are (high)Size, then cleaned using glacial acetic acid, acetone and ethanol, then by deionized water clean after dry placement;
Then, it is preferred to use oxidation stripping method(Hummers methods)To prepare graphene oxide water solution, and its key parameter is adjusted to mass concentration 0.5mg/mL, then cleaned nickel foam is directly soaked and wherein stands reaction, the reaction temperature of wherein integral system is controlled as 80 °C, soak time is 2 hours, in the process graphene oxide is reduced directly as the nickel foam of substrate in immersion, and deposition growing is Graphene on the surface of nickel foam, reaction takes out nickel foam after terminating, and nickel foam-graphite ene product that surface forms three-dimensional porous structure is cleaned with deionized water.
Embodiment 6
Nickel foam is cut into for example as 1cm is (long first)X 1cm are (wide)X 1mm are (high)Size, then cleaned using glacial acetic acid, acetone and ethanol, then by deionized water clean 5 minutes after dry placement;
Then, it is preferred to use oxidation stripping method(Hummers methods)To prepare graphene oxide water solution, and its key parameter is adjusted to mass concentration 2.5mg/mL, then cleaned nickel foam is directly soaked and wherein stands reaction, the reaction temperature of wherein integral system is controlled as 55 °C, soak time is 3.5 hours, in the process graphene oxide is reduced directly as the nickel foam of substrate in immersion, and deposition growing is Graphene on the surface of nickel foam, reaction takes out nickel foam after terminating, and nickel foam-graphite ene product that surface forms three-dimensional porous structure is cleaned with deionized water.
Embodiment 7
Nickel foam is cut into for example as 1cm is (long first)X 1cm are (wide)X 1mm are (high)Size, then cleaned using glacial acetic acid, acetone and ethanol, then by deionized water clean 5 minutes after dry placement;
Then, it is preferred to use oxidation stripping method(Hummers methods)To prepare graphene oxide water solution, and its key parameter is adjusted to mass concentration 2mg/mL, then cleaned nickel foam is directly soaked and wherein stands reaction, the reaction temperature of wherein integral system is controlled as 55 °C, soak time is 3.5 hours, in the process graphene oxide is reduced directly as the nickel foam of substrate in immersion, and deposition growing is Graphene on the surface of nickel foam, reaction takes out nickel foam after terminating, and nickel foam-graphite ene product that surface forms three-dimensional porous structure is cleaned with deionized water.
Embodiment 8
Nickel foam is cut into for example as 1cm is (long first)X 1cm are (wide)X 1mm are (high)Size, then cleaned using glacial acetic acid, acetone and ethanol, then by deionized water clean 5 minutes after dry placement;
Then, it is preferred to use oxidation stripping method(Hummers methods)To prepare graphene oxide water solution, and its key parameter is adjusted to mass concentration 2.5mg/mL, then cleaned nickel foam is directly soaked and wherein stands reaction, the reaction temperature of wherein integral system is controlled as 80 °C, soak time is 3 hours, in the process graphene oxide is reduced directly as the nickel foam of substrate in immersion, and deposition growing is Graphene on the surface of nickel foam, reaction takes out nickel foam after terminating, and nickel foam-graphite ene product that surface forms three-dimensional porous structure is cleaned with deionized water.
Embodiment 9
Nickel foam is cut into for example as 1cm is (long first)X 1cm are (wide)X 1mm are (high)Size, then cleaned using glacial acetic acid, acetone and ethanol, then by deionized water clean 5 minutes after dry placement;
Then, it is preferred to use oxidation stripping method(Hummers methods)To prepare graphene oxide water solution, and its key parameter is adjusted to mass concentration 3mg/mL, then cleaned nickel foam is directly soaked and wherein stands reaction, the reaction temperature of wherein integral system is controlled as 60 °C, soak time is 4 hours, in the process graphene oxide is reduced directly as the nickel foam of substrate in immersion, and deposition growing is Graphene on the surface of nickel foam, reaction takes out nickel foam after terminating, and nickel foam-graphite ene product that surface forms three-dimensional porous structure is cleaned with deionized water;
Then, in three-electrode system, the three-dimensional porous grapheme foam that will be obtained is by electrochemistry potentiostatic electrodeposition technology come loaded nano manganese dioxide.Wherein potential setting is 1V, and sedimentation time is 5 minutes, and working electrode is three-dimensional porous grapheme foam, is gauze platinum electrode to electrode, and reference electrode is saturated calomel electrode, and electrolyte is the acetic acid manganese solution of 1mol/L.Understood with reference to the scanning electron microscope test in Fig. 3, the manganese dioxide pattern that electro-deposition is obtained is the loose structure that nanometer sheet is constituted.
In addition, the three-dimensional porous grapheme foam electrode prepared in manganese dioxide obtained above/grapheme foam combination electrode and embodiment 1 is circulated voltammetric scan test under conditions of 50mV/s respectively, it can be seen that after depositing manganese dioxide on grapheme foam, the area of cyclic voltammetric figure is significantly increased, and this illustrates that the storing up electricity performance of combination electrode is obviously improved.
Embodiment 10
Nickel foam is cut into for example as 1cm is (long first)X 1cm are (wide)X 1mm are (high)Size, then cleaned using glacial acetic acid, acetone and ethanol, then by deionized water clean 5 minutes after dry placement;
Then, it is preferred to use oxidation stripping method(Hummers methods)To prepare graphene oxide water solution, and its key parameter is adjusted to mass concentration 3mg/mL, then cleaned nickel foam is directly soaked and wherein stands reaction, the reaction temperature of wherein integral system is controlled as 60 °C, soak time is 4 hours, in the process graphene oxide is reduced directly as the nickel foam of substrate in immersion, and deposition growing is Graphene on the surface of nickel foam, reaction takes out nickel foam after terminating, and nickel foam-graphite ene product that surface forms three-dimensional porous structure is cleaned with deionized water;
Then, in three-electrode system, the three-dimensional porous grapheme foam that will be obtained loads polypyrrole by electrochemistry potentiostatic electrodeposition technology.Wherein potential setting is -0.8V, and sedimentation time is 6 minutes, and working electrode is three-dimensional porous grapheme foam, is gauze platinum electrode to electrode, and reference electrode is silver/silver chloride electrode, and electrolyte is the sodium perchlorate and pyrrole monomer of 0.2mol/L(Volume fraction is mixed solution 5%).
Those skilled in the art is readily appreciated that; the foregoing is only presently preferred embodiments of the present invention; it is not intended to limit the invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc. should be included within the scope of the present invention.

Claims (6)

1. the three-dimensional porous electrode preparation method of nickel foam-Graphene of reaction equation is directly soaked, it is characterised in that the method comprises the following steps:
Nickel foam is cleaned using glacial acetic acid, acetone and ethanol successively, then placement is dried after deionized water is cleaned;
It is the graphene oxide water solution of 0.5mg/mL 10mg/mL to prepare mass concentration, then by step(A) nickel foam after processing directly is dipped into and wherein stands reaction, and reaction temperature is controlled as 30 °C 80 °C in this immersion process, and soak time is 12 hours 2 hours;In this way, in immersion process there is reduction reaction in Graphene, and spontaneous deposition is grown to Graphene on the foam nickel surface as conductive substrates, ultimately form the nickel foam-graphite ene product of three-dimensional porous structure.
2. the method for claim 1, it is characterised in that in step(B) in, it is preferred to use aoxidize stripping method to prepare the graphene oxide water solution, and its mass concentration is further configured to 1mg/mL 2.5mg/mL.
3. method as claimed in claim 1 or 2, it is characterised in that in step(B) in, the reaction temperature is preferably 70 °C of 60C, and soak time is 6 hours 4 hours.
4. method as claimed in claim 3, it is characterised in that in step(B) in, the reaction temperature is most preferably from about 60 °C, and soak time is controlled to 6 hours or so.
5. the method for claim 1, it is characterised in that in step(B) after, on the basis of the nickel foam-graphite ene product of the three-dimensional porous structure for being formed, continue through electrochemistry potentiostatic electrodeposition technology to load polypyrrole or nano-manganese dioxide.
6. method as claimed in claim 5, it is characterised in that above-mentioned nickel foam-Graphene is three-dimensional
Electrode of the porous electrode preferably as ultracapacitor, lithium ion battery or lithium-air battery.
CN201510833005.7A 2015-11-26 2015-11-26 Directly soak the three-dimensional porous electrode preparation method of nickel foam-Graphene of reaction equation Pending CN106803461A (en)

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CN110706935A (en) * 2019-10-12 2020-01-17 刘沛源 rGO/FeOOH/rGO composite material, and preparation method and application thereof
CN110706935B (en) * 2019-10-12 2021-12-17 刘沛源 rGO/FeOOH/rGO composite material, and preparation method and application thereof
CN111454482A (en) * 2020-04-22 2020-07-28 江苏海洋大学 Application of water-soluble high molecular polymer in preparation of plastic conductive composite foam
CN111454482B (en) * 2020-04-22 2022-03-22 江苏海洋大学 Application of water-soluble high molecular polymer in preparation of plastic conductive composite foam
CN113772664A (en) * 2021-09-08 2021-12-10 长春工业大学 Nickel black-graphene composite photo-thermal conversion film and preparation method thereof

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