CN114429868A - Preparation method of sandwich-structure graphene/cobaltosic sulfide nickel electrode material - Google Patents
Preparation method of sandwich-structure graphene/cobaltosic sulfide nickel electrode material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 69
- 239000007772 electrode material Substances 0.000 title claims abstract description 30
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000008367 deionised water Substances 0.000 claims abstract description 32
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 32
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 31
- 239000010439 graphite Substances 0.000 claims abstract description 31
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 31
- 229910003266 NiCo Inorganic materials 0.000 claims abstract description 30
- 239000012528 membrane Substances 0.000 claims abstract description 27
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 20
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims abstract description 13
- 239000004202 carbamide Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000011888 foil Substances 0.000 claims abstract description 13
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 12
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000000967 suction filtration Methods 0.000 claims abstract description 11
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims description 29
- 238000009210 therapy by ultrasound Methods 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000006249 magnetic particle Substances 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 238000003828 vacuum filtration Methods 0.000 claims description 6
- 229910001868 water Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 239000010410 layer Substances 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 239000011229 interlayer Substances 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 239000002114 nanocomposite Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 13
- 239000003990 capacitor Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 4
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- KAEHZLZKAKBMJB-UHFFFAOYSA-N cobalt;sulfanylidenenickel Chemical compound [Ni].[Co]=S KAEHZLZKAKBMJB-UHFFFAOYSA-N 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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Abstract
The invention discloses a preparation method of a sandwich structure graphene/cobaltosic sulfide nickel electrode material, which comprises the following steps: firstly, taking a graphite foil as an anode and a platinum wire as a cathode, carrying out electrochemical stripping, dissolving in deionized water, and carrying out suction filtration on formed graphene centrifugate to form a film; then adding NiCl2·6H2O、CoCl2·6H2Mixing O and urea, and carrying out hydrothermal treatment to obtain NiCo (OH) powder; mixing NiCo (OH) powder, thiourea and H2Mixing O, and carrying out hydrothermal reaction to obtain magnetic NiCo2S4(ii) a Mixing NiCo2S4Dissolving in deionized water, pouring on the film formed before, and performing suction filtration to form a double-layer film; will be provided withPouring the graphene centrifugate on the double-layer membrane, performing suction filtration again to form a membrane, and drying to obtain the graphene nano-composite membrane. The sandwich structure electrode material promotes the transmission of ions and electrons; NiCo2S4In the middle of the interlayer, a part of pseudo capacitance is provided, and the electrochemical performance of the material is improved.
Description
Technical Field
The invention belongs to the technical field of electrode material preparation, and particularly relates to sandwich-structured graphene/cobaltosic sulfide nickel alloy(NiCo2S4) A preparation method of the electrode material.
Background
With the demand of human society for energy, the research and development of novel energy storage and conversion devices such as lithium ion batteries, fuel cells, solar cells and super capacitors are of great importance. In particular, the super capacitor has received much attention from the scientific community in recent years due to the advantages of high energy density of the battery and high power density of the conventional capacitor. Graphene has good conductivity, excellent electron mobility and large specific surface area as an excellent supercapacitor electrode material. However, due to van der waals force and pi-pi bond stacking, graphene on a solution or a substrate is easy to undergo irreversible aggregation during preparation, storage, testing and the like, which is not favorable for full utilization of the specific surface area.
The self-supporting graphene (SGr) has good mechanical strength and high surface energy, and the generated wrinkle morphology reduces the agglomeration to a certain extent. However, the SCr is still an electric double layer capacitor in nature, which results in a generally small capacitor and difficulty in meeting the energy requirement in practical applications. The combination of the SCR and the conductive polymer can obviously improve the capacitance performance. The method is an effective method for preparing the electrode of the super capacitor by combining graphene and nickel cobalt sulfide to obtain the composite material with the sandwich structure.
Disclosure of Invention
The invention aims to provide graphene/NiCo with a sandwich structure2S4The preparation method of the electrode material solves the problems of low conductivity and poor stability caused by doping a current collector and a binder in the preparation of the existing electrode material.
The technical scheme adopted by the invention is that the graphene/NiCo with a sandwich structure2S4The preparation method of the electrode material is implemented according to the following steps:
step 1, using graphite foil as a carbon electrode, namely an anode, and using a platinum wire as a cathode for electrochemical stripping of graphite to obtain stripped graphene;
step 3, filtering the graphene centrifugate to form a membrane;
step 4, mixing NiCl2·6H2O、CoCl2·6H2Mixing O and urea, carrying out ultrasonic treatment, and transferring the mixture into a high-pressure reaction kettle to carry out hydrothermal treatment to obtain a hydrothermal product; vacuum filtering the hydrothermal product with deionized water, and drying to obtain NiCo (OH) powder;
Step 6, magnetic particles NiCo2S4Dissolving in deionized water, mixing uniformly, performing ultrasonic treatment, pouring on the film formed in the step 3, and performing suction filtration to form a film;
and 7, pouring the graphene centrifugate in the step 2 onto the membrane formed in the step 6, performing suction filtration again to form a membrane, and drying to obtain the sandwich-structured exfoliated graphene-NiCo2S4-exfoliating graphene electrode material.
The present invention is also characterized in that,
in the step 1, the method specifically comprises the following steps: the graphite foil and platinum electrode were placed at 0.1M (NH)4)2SO4And then applying a positive voltage of 9.9V to a graphite electrode to perform electrochemical stripping, after the graphite stripping is finished, performing vacuum filtration on the product by using deionized water, and using a filter membrane with the pore diameter of 0.45 mu m during the filtration to obtain the stripped graphene.
In step 4, NiCl2·6H2O、CoCl2·6H2The molar ratio of O to urea is 1: 1: 3.
in the step 4, the ultrasonic treatment time is 25 min; the hydrothermal reaction temperature is 150 ℃ and 180 ℃, and the hydrothermal reaction time is 22-26 h.
In the step 5, the mass ratio of NiCo (OH) powder to thiourea is 1: 2.
in the step 5, the ultrasonic treatment time is 10-30 min; the hydrothermal reaction temperature is 180 ℃ and 260 ℃, and the hydrothermal reaction time is 8-16 h.
The invention has the beneficial effects that: the peeled graphene-NiCo with the sandwich structure is prepared by a simple vacuum-assisted suction filtration film forming method2S4Stripping the composite film of graphene to obtain a flexible, self-supporting composite electrode material. The thin film electrode material with a sandwich structure is obtained by a simple preparation method, and the transmission of ions and electrons is promoted; NiCo2S4In the middle of the interlayer, a part of pseudo-capacitance is provided, the whole electrochemical performance is improved, a self-supporting structure without a current collector and a bonding agent is formed, and the self-supporting structure has high conductivity, flexibility and mechanical stability. Prepared exfoliated graphene-NiCo with sandwich structure2S4The graphene-exfoliated composite film used as an electrode has a specific capacity of about 0.0631mF cm-2。
Drawings
FIG. 1 shows a sandwich structure of exfoliated graphene-NiCo prepared in examples 1 to 3 of the present invention2S4Cyclic voltammetry plots of the exfoliated graphene electrode material.
Detailed Description
The present invention will be described in detail with reference to the following detailed description and accompanying drawings.
The invention relates to sandwich structure graphene/cobaltosic sulfide nickel (NiCo)2S4) The preparation method of the electrode material is implemented according to the following steps:
step 1, using graphite foil as a carbon electrode, namely an anode, using a platinum wire as a cathode, and performing electrochemical stripping on graphite, wherein the graphite foil and the platinum electrode are placed at 0.1M (NH)4)2SO4Performing electrochemical stripping by applying a positive voltage of 9.9V to a graphite electrode, performing vacuum filtration on the product by using deionized water after graphite stripping is completed, and filtering by using a filter membrane with the pore diameter of 0.45 mu m to obtain stripped graphene;
the centrifugal speed is 3000r/min, and the centrifugal time is 20 min;
step 3, filtering the graphene centrifugate to form a membrane;
step 4, mixing NiCl2·6H2O、CoCl2·6H2Mixing O and urea, carrying out ultrasonic treatment, and transferring the mixture into a high-pressure reaction kettle to carry out hydrothermal treatment to obtain a hydrothermal product; vacuum filtering the hydrothermal product with deionized water, and drying to obtain NiCo (OH) powder;
NiCl2·6H2O、CoCl2·6H2the molar ratio of O to urea is 1: 1: 3;
the ultrasonic treatment time is 25 min; the hydrothermal reaction temperature is 150 ℃ and 180 ℃, and the hydrothermal reaction time is 22-26 h;
The mass ratio of NiCo (OH) powder to thiourea is 1: 2;
the ultrasonic treatment time is 10-30 min; the hydrothermal reaction temperature is 180 ℃ and 260 ℃, and the hydrothermal reaction time is 8-16 h;
step 6, magnetic particle NiCo2S4Dissolving in deionized water, uniformly mixing by ultrasonic waves, pouring on the film formed in the step (3), and filtering to form a film;
and 7, pouring the graphene centrifugate in the step 2 onto the membrane formed in the step 6, performing suction filtration again to form a membrane, and drying to obtain the sandwich-structured exfoliated graphene-NiCo2S4-exfoliating graphene electrode material.
Example 1
The invention relates to graphene/NiCo with a sandwich structure2S4The preparation method of the electrode material is implemented according to the following steps:
step 1, using graphite foil as a carbon electrode, namely an anode, using a platinum wire as a cathode, and performing electrochemical stripping on graphite, wherein the graphite foil and the platinum electrode are placed at 0.1M (NH)4)2SO4Performing electrochemical stripping by applying a positive voltage of 9.9V to a graphite electrode, performing vacuum filtration on the product by using deionized water after graphite stripping is completed, and filtering by using a filter membrane with the pore diameter of 0.45 mu m to obtain stripped graphene;
the centrifugal speed is 3000r/min, and the centrifugal time is 20 min;
step 3, filtering the graphene centrifugate to form a membrane;
step 4, mixing NiCl2·6H2O、CoCl2·6H2Mixing O and urea, carrying out ultrasonic treatment, and transferring the mixture into a high-pressure reaction kettle to carry out hydrothermal treatment to obtain a hydrothermal product; vacuum filtering the hydrothermal product with deionized water, and drying at 80 ℃ for 12h to obtain NiCo (OH) powder;
NiCl2·6H2O、CoCl2·6H2the molar ratio of O to urea is 1: 1: 3;
the ultrasonic treatment time is 25 min; the hydrothermal reaction temperature is 160 ℃, and the hydrothermal reaction time is 24 hours;
The mass ratio of NiCo (OH) powder to thiourea is 1: 2;
the ultrasonic treatment time is 30 min; the hydrothermal reaction temperature is 180 ℃, and the hydrothermal reaction time is 16 h;
step 6, magnetic particle NiCo2S4Dissolving in deionized water, uniformly mixing by ultrasonic waves, pouring on the film formed in the step (3), and filtering to form a film;
and 7, pouring the graphene centrifugate in the step 2 onto the membrane formed in the step 6, performing suction filtration again to form a membrane, and drying to obtain the sandwich-structured exfoliated graphene-NiCo2S4-exfoliating graphene electrode material. Exfoliated graphiteAlkene, NiCo2S4And the molar ratio of the exfoliated graphene is 3: 1: 3.
example 2
The invention relates to graphene/NiCo with a sandwich structure2S4The preparation method of the electrode material is implemented according to the following steps:
step 1, using graphite foil as a carbon electrode, namely an anode, using a platinum wire as a cathode, and performing electrochemical stripping on graphite, wherein the graphite foil and the platinum electrode are placed at 0.1M (NH)4)2SO4Performing electrochemical stripping by applying a positive voltage of 9.9V to a graphite electrode, performing vacuum filtration on the product by using deionized water after graphite stripping is completed, and filtering by using a filter membrane with the pore diameter of 0.45 mu m to obtain stripped graphene;
the centrifugal speed is 3000r/min, and the centrifugal time is 20 min;
step 3, filtering the graphene centrifugate to form a membrane;
step 4, mixing NiCl2·6H2O、CoCl2·6H2Mixing O and urea, carrying out ultrasonic treatment, and transferring the mixture into a high-pressure reaction kettle to carry out hydrothermal treatment to obtain a hydrothermal product; vacuum filtering the hydrothermal product with deionized water, and drying to obtain NiCo (OH) powder;
NiCl2·6H2O、CoCl2·6H2the molar ratio of O to urea is 1: 1: 3;
the ultrasonic treatment time is 25 min; the hydrothermal reaction temperature is 150 ℃, and the hydrothermal reaction time is 22 h;
The mass ratio of NiCo (OH) powder to thiourea is 1: 2;
the ultrasonic treatment time is 30 min; the hydrothermal reaction temperature is 200 ℃, and the hydrothermal reaction time is 12 h;
step 6, magnetic particles NiCo2S4Dissolving in deionized water, uniformly mixing by ultrasonic waves, pouring on the film formed in the step (3), and filtering to form a film;
and 7, pouring the graphene centrifugate in the step 2 onto the membrane formed in the step 6, performing suction filtration again to form a membrane, and drying to obtain the sandwich-structured exfoliated graphene-NiCo2S4-exfoliating graphene electrode material. Stripping graphene and NiCo2S4And the molar ratio of the exfoliated graphene is 2: 1: 2.
example 3
The invention relates to graphene/NiCo with a sandwich structure2S4The preparation method of the electrode material is implemented according to the following steps:
step 1, using graphite foil as a carbon electrode, namely an anode, using a platinum wire as a cathode, and performing electrochemical stripping on graphite, wherein the graphite foil and the platinum electrode are placed at 0.1M (NH)4)2SO4Performing electrochemical stripping by applying a positive voltage of 9.9V to a graphite electrode, performing vacuum filtration on the product by using deionized water after graphite stripping is completed, and filtering by using a filter membrane with the pore diameter of 0.45 mu m to obtain stripped graphene;
the centrifugal speed is 3000r/min, and the centrifugal time is 20 min;
step 3, filtering the graphene centrifugate to form a membrane;
step 4, mixing NiCl2·6H2O、CoCl2·6H2Mixing O and urea, carrying out ultrasonic treatment, and transferring the mixture into a high-pressure reaction kettle to carry out hydrothermal treatment to obtain a hydrothermal product; vacuum filtering the hydrothermal product with deionized water, and drying to obtain NiCo (OH) powder;
NiCl2·6H2O、CoCl2·6H2the molar ratio of O to urea is 1: 1: 3;
the ultrasonic treatment time is 25 min; the hydrothermal reaction temperature is 150 ℃, and the hydrothermal reaction time is 22 h;
The mass ratio of NiCo (OH) powder to thiourea is 1: 2;
the ultrasonic treatment time is 25 min; the hydrothermal reaction temperature is 180 ℃, and the hydrothermal reaction time is 15 h;
step 6, magnetic particle NiCo2S4Dissolving in deionized water, uniformly mixing by ultrasonic waves, pouring on the film formed in the step (3), and filtering to form a film;
and 7, pouring the graphene centrifugate in the step 2 onto the membrane formed in the step 6, performing suction filtration again to form a membrane, and drying to obtain the sandwich-structured exfoliated graphene-NiCo2S4-exfoliating graphene electrode material. Stripping graphene and NiCo2S4And the molar ratio of the exfoliated graphene is 1: 1: 1.
the sandwich-structured exfoliated graphene-NiCo prepared in examples 1 to 32S4Exfoliation of graphene electrode materials as self-supporting electrodes, PVA/H3PO4The gel was tested for its performance as an electrolyte. The assembled device was used for cyclic voltammetry measurements using a coster electrochemical workstation. Fig. 1 is a plot of cyclic voltammetry and specific capacity versus current density, which maintained good shape as scan rate increased.
Claims (6)
1. The preparation method of the sandwich structure graphene/cobaltosic sulfide nickel electrode material is characterized by comprising the following steps:
step 1, using graphite foil as a carbon electrode, namely an anode, and using a platinum wire as a cathode for electrochemical stripping of graphite to obtain stripped graphene;
step 2, dissolving the stripped graphene in deionized water, performing ultrasonic treatment, and then centrifuging to form a graphene centrifugate;
step 3, filtering the graphene centrifugate to form a membrane;
step 4, mixing NiCl2·6H2O、CoCl2·6H2Mixing O and urea, carrying out ultrasonic treatment, and transferring the mixture into a high-pressure reaction kettle to carry out hydrothermal treatment to obtain a hydrothermal product; vacuum filtering the hydrothermal product with deionized water, and drying to obtain NiCo (OH) powder;
step 5, mixing NiCo (OH) powder, thiourea and H2O mixing, ultrasonic treating, transferring into a high-pressure reaction kettle for hydrothermal reaction, and vacuum filtering the obtained hydrothermal product with deionized water to obtain magnetic particle NiCo2S4;
Step 6, magnetic particle NiCo2S4Dissolving in deionized water, mixing uniformly, pouring on the film formed in the step (3), and filtering to form a film;
and 7, pouring the graphene centrifugate in the step 2 onto the membrane formed in the step 6, performing suction filtration again to form a membrane, and drying to obtain the sandwich-structured exfoliated graphene-NiCo2S4-exfoliating graphene electrode material.
2. The preparation method of the sandwich structure graphene/cobaltosic sulfide nickel electrode material according to claim 1, wherein the step 1 specifically comprises the following steps: graphite foil and platinum electrode were placed at 0.1M (NH)4)2SO4And then applying a positive voltage of 9.9V to a graphite electrode to perform electrochemical stripping, after the graphite stripping is finished, performing vacuum filtration on the product by using deionized water, and using a filter membrane with the pore diameter of 0.45 mu m during the filtration to obtain the stripped graphene.
3. The method for preparing the sandwich structure graphene/cobaltosic sulfide nickel electrode material according to claim 1, wherein in the step 4, NiCl is added2·6H2O、CoCl2·6H2The molar ratio of O to urea is 1: 1: 3.
4. the preparation method of the sandwich structure graphene/cobaltosic sulfide nickel electrode material according to claim 1, wherein in the step 4, the ultrasonic treatment time is 25 min; the hydrothermal reaction temperature is 150 ℃ and 180 ℃, and the hydrothermal reaction time is 22-26 h.
5. The preparation method of the sandwich structure graphene/cobaltosic sulfide nickel electrode material according to claim 1, wherein in the step 5, the mass ratio of NiCo (OH) powder to thiourea is 1: 2.
6. the preparation method of the sandwich structure graphene/cobaltosic sulfide nickel electrode material according to claim 1, wherein in the step 5, the ultrasonic treatment time is 10-30 min; the hydrothermal reaction temperature is 180 ℃ and 260 ℃, and the hydrothermal reaction time is 8-16 h.
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