CN104183830A - Preparation method of two-dimensional inorganic layered compound/graphene composite material - Google Patents
Preparation method of two-dimensional inorganic layered compound/graphene composite material Download PDFInfo
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- CN104183830A CN104183830A CN201410408483.9A CN201410408483A CN104183830A CN 104183830 A CN104183830 A CN 104183830A CN 201410408483 A CN201410408483 A CN 201410408483A CN 104183830 A CN104183830 A CN 104183830A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 64
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 150000001875 compounds Chemical class 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000005406 washing Methods 0.000 claims description 17
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- 239000003093 cationic surfactant Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical group [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 3
- 150000004770 chalcogenides Chemical class 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052723 transition metal Inorganic materials 0.000 claims description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 3
- 150000003624 transition metals Chemical class 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 240000002853 Nelumbo nucifera Species 0.000 claims description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 claims description 2
- 235000006510 Nelumbo pentapetala Nutrition 0.000 claims description 2
- 229920000075 poly(4-vinylpyridine) Polymers 0.000 claims description 2
- 229920000333 poly(propyleneimine) Polymers 0.000 claims description 2
- -1 polyethylene propyl-dimethyl ammonium chloride Polymers 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 11
- 239000006185 dispersion Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000009881 electrostatic interaction Effects 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 3
- 238000012983 electrochemical energy storage Methods 0.000 abstract description 2
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 230000005540 biological transmission Effects 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 31
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- BLJNPOIVYYWHMA-UHFFFAOYSA-N alumane;cobalt Chemical compound [AlH3].[Co] BLJNPOIVYYWHMA-UHFFFAOYSA-N 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 13
- 229910021641 deionized water Inorganic materials 0.000 description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 12
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 238000005349 anion exchange Methods 0.000 description 8
- NGTSQWJVGHUNSS-UHFFFAOYSA-N bis(sulfanylidene)vanadium Chemical compound S=[V]=S NGTSQWJVGHUNSS-UHFFFAOYSA-N 0.000 description 8
- 239000002135 nanosheet Substances 0.000 description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 5
- 229910000000 metal hydroxide Inorganic materials 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000004202 carbamide Substances 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 150000004692 metal hydroxides Chemical class 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000004317 sodium nitrate Substances 0.000 description 4
- 235000010344 sodium nitrate Nutrition 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000002055 nanoplate Substances 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 description 1
- GOPYZMJAIPBUGX-UHFFFAOYSA-N [O-2].[O-2].[Mn+4] Chemical class [O-2].[O-2].[Mn+4] GOPYZMJAIPBUGX-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- 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
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a two-dimensional inorganic layered compound/graphene composite material. The preparation method of the composite material comprises the following steps: preparing layered compound dispersion liquid with positive charges on the surface and oxidized graphene dispersion liquid with negative charges; mixing the two kinds of solution to perform self-assembling under an electrostatic interaction to obtain the ordered two-dimensional inorganic layered compound/graphene composite material assembled alternatively layer by layer; and carrying out reduction reaction on the composite material under certain conditions to obtain the two-dimensional inorganic layered compound/graphene composite material. According to the two-dimensional inorganic layered compound/graphene composite material, the two-dimensional inorganic layered compound and the graphene are assembled alternatively layer by layer under the electrostatic interaction; the required equipment has low requirement and is easy to operate; the graphene can provide a good electronic transmission channel for the inorganic layered material, so as to enhance the electrical conductivity of the inorganic layered material, prevent agglomeration, and achieve an important effect on the material structure stability. The two-dimensional inorganic layered compound/graphene composite material can be widely applied to the fields of catalytic and electrochemical energy storage fields.
Description
Technical field
The present invention relates to a kind of preparation method of Two-dimensional Inorganic lamellar compound/graphene composite material, belong to nano material and preparing technical field thereof.
Background technology
Two-dimensional Inorganic lamellar compound as stratiform transition metal hydroxide, stratiform transition metal oxide, laminated metal chalcogenide etc. because its unique layer structure attracted a lot of concerns.And research shows, these Two-dimensional Inorganic nonwoven fabric from filaments are peeled off into the thinner nanometer sheet of stable existence, these materials can show more excellent performance, have very large application potential aspect electrochemical energy storage.Yet poorly conductive is the main cause that limits these material application.
Than these semiconductors Two-dimensional Inorganic lamellar compound of insulating property (properties) even, Graphene is a kind of material with carbon element of monoatomic layer, has specific area large, good conductivity, intensity high.Yet Graphene is used separately and is easy to reunite, its actual specific area is significantly less than theoretical specific area, therefore, can not bring into play better its effect.
Patent CN103093967A discloses a kind of preparation method who prepares the cobalt aluminum bimetal hydroxide/redox graphene of lamellar structure, and the method is by being directly added to cobalt nitrate and aluminum nitrate mixed solution in graphene oxide, and backflow obtains.But the metal ion that this method is removed on absorption position grows into outside nano particle, in solution, also have a large amount of metal ions to generate double-metal hydroxide, form aggregating state and the contact of discord Graphene.Patent CN103641174A has described a kind of by the direct ultrasonic nano-sheet MnO that obtains of mixing of the dispersion liquid of nano-sheet manganese dioxide powder dispersion and graphene powder
2the preparation method of/graphene composite material.Yet composite material prepared by this method, only relies on ultrasonic effect, MnO
2with evenly combination effectively of Graphene.In patent CN102496480A, alkali source compound, nickel and aluminium salt precursor body are joined to hydro-thermal reaction in Graphene filter cake and make graphene/nickel-aluminum bimetal hydroxide.The method is high to equipment requirement, and nickel aluminum bimetal hydroxide differs and effectively grows into surely on the Graphene filter cake having reduced.
Summary of the invention
The object of the invention is to, for Two-dimensional Inorganic lamellar compound and the independent deficiency of using of Graphene, provides a kind of compound Two-dimensional Inorganic lamellar compound of simple possible and the preparation method of Graphene.
The present invention specifically comprises the following steps:
(1) Two-dimensional Inorganic lamellar compound presoma is peeled off into nanometer sheet in can reducing its solvent of peeling off energy, make positive charge on lamellar compound surface band, obtain positively charged lamellar compound solution, the mass ratio of lamellar compound and solvent is 1:1 ~ 1:20.
(2) by the surface of preparation with the lamellar compound solution of positive charge and with the graphene oxide solution of negative electrical charge in proportion 1:1 ~ 50:1 mix, standing 6 ~ 60h, there is precipitation, pour out supernatant liquor, centrifuge washing lower floor solution, obtains Two-dimensional Inorganic lamellar compound/graphene oxide composite material I.
(3) by Two-dimensional Inorganic lamellar compound/graphene oxide composite material I reduction, obtain Two-dimensional Inorganic lamellar compound/graphene composite material II.
Two-dimensional Inorganic lamellar compound presoma described in step (1) is stratiform transition metal hydroxide, stratiform transition metal oxide, laminated metal chalcogenide.
Described its solvent of peeling off energy that can reduce is formamide, Tetramethylammonium hydroxide, 1-METHYLPYRROLIDONE, isopropyl alcohol or N-N-dimethyl formamide etc.
Described make the lamellar compound lotus that becomes positively charged, if the positively charged of lamellar compound nanometer sheet own is directly peeled off into nanometer sheet, if lamellar compound itself is electronegative, with cationic surfactant, modify.Cationic surfactant can be hexadecyltrimethylammonium chloride, polyethylene propyl-dimethyl ammonium chloride, polypropylene amine hydrochloride, poly 4 vinyl pyridine etc.Described lamellar compound and the mass ratio of solvent are 1:1 ~ 1:20.
The solution with positive charge described in step (2) and with the graphene solution of negative electrical charge in proportion 1:1 ~ 20:1 mix.
Method of reducing described in step (3) has electronation, thermal reduction etc.Described its conductivity of Two-dimensional Inorganic lamellar compound/graphene composite material II is obviously better than Two-dimensional Inorganic lamellar compound/graphene oxide composite material I.
The present invention utilizes electrostatic interaction by Two-dimensional Inorganic lamellar compound and Graphene alternate group dress layer by layer, and both can carry out combination effectively by electrostatic force, the nano composite material that height of formation is orderly, and equipment needed thereby requires low, easy operating.Graphene not only can strengthen its conductivity for inorganic lamellar material provides good electron propagation ducts, has also prevented the reunion of self, the structural stability of material has been play a part important, has guaranteed that it is in many-sided application.
Accompanying drawing explanation
Fig. 1 is the mechanism schematic diagram of Two-dimensional Inorganic lamellar compound (surface band the positive charge)/graphene composite material prepared of the present invention.
Fig. 2 is the mechanism schematic diagram of Two-dimensional Inorganic lamellar compound (surface band the negative electrical charge)/graphene composite material prepared of the present invention.
Embodiment
Below in conjunction with embodiment, be intended to further illustrate the present invention, and unrestricted the present invention.
Embodiment 1
2.617g is analyzed to pure nickel nitrate and 1.125g to be analyzed in the deionized water that pure aluminum nitrate is dissolved in 50ml, 2.4g urea is dissolved in the deionized water of 50ml, two kinds of solution are mixed, proceed in autoclave, 100 ℃ of reaction 24h, filter, washing, obtains nickel aluminum bimetal hydroxide 60 ℃ of vacuumizes.The nickel aluminum bimetal hydroxide of 1g is joined in the nitric acid 1000ml solution of the sodium nitrate that contains 1.5M and 0.005M, in solution, pass into nitrogen 15min, drive carbon dioxide away.Above-mentioned solution is at room temperature shaken 1 day, the product obtaining is filtered, washing, obtains the nickel aluminum bimetal hydroxide after anion exchange 60 ℃ of vacuumizes.By the nickel aluminum bimetal hydroxide after anion exchange and formamide solution 1:1 mixing in mass ratio, shake 1 day, 2000rpm centrifuging and taking supernatant liquor, obtains the positively charged stratiform nickel aluminum bimetal hydroxide nanometer sheet solution 1 of peeling off.By the positively charged stratiform nickel aluminum bimetal hydroxide nanometer sheet solution 1 of peeling off and stannic oxide/graphene nano sheet solution 2 50:1 mixing in proportion, stir 10min, standing 24h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain nickel aluminum bimetal hydroxide/graphene oxide composite material 3, as shown in Figure 1.By composite material 200 ℃ of heat treatment 6h under nitrogen atmosphere, obtain nickel aluminum bimetal hydroxide/graphene composite material.Above-mentioned composite material is loaded on glass-carbon electrode, and in 1mol/L potassium hydroxide electrolyte, test has good electrocatalysis characteristic, can be applied to alkaline fuel cell.
Embodiment 2
1.746g is analyzed to pure nickel nitrate and 1.125g to be analyzed in the deionized water that pure aluminum nitrate is dissolved in 50ml, 1.8g urea is dissolved in the deionized water of 50ml, two kinds of solution are mixed, proceed in autoclave, 100 ℃ of reaction 24h, filter, washing, obtains nickel aluminum bimetal hydroxide 60 ℃ of vacuumizes.The nickel aluminum bimetal hydroxide of 1g is joined in the nitric acid 1000ml solution of the sodium nitrate that contains 1.5M and 0.005M, in solution, pass into nitrogen 15min, drive carbon dioxide away.Above-mentioned solution is at room temperature shaken 1 day, the product obtaining is filtered, washing, obtains the nickel aluminum bimetal hydroxide after anion exchange 60 ℃ of vacuumizes.By the nickel aluminum bimetal hydroxide after anion exchange and formamide solution 1:1 mixing in mass ratio, shake 1 day, 2000rpm centrifuging and taking supernatant liquor, obtains the positively charged stratiform nickel aluminum bimetal hydroxide nanometer sheet of peeling off.By the positively charged stratiform nickel aluminum bimetal hydroxide nanometer sheet solution of peeling off and the 20:1 mixing in proportion of stannic oxide/graphene nano sheet solution, stir 10min, standing 24h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain nickel aluminum bimetal hydroxide/graphene oxide composite material.By composite material 200 ℃ of heat treatment 6h under nitrogen atmosphere, obtain nickel aluminum bimetal hydroxide/graphene composite material.Above-mentioned composite material is loaded on glass-carbon electrode, and in 1mol/L potassium hydroxide electrolyte, test has good electrocatalysis characteristic, can be applied to alkaline fuel cell.
Embodiment 3
2.619g is analyzed to pure cobalt nitrate and 1.125g to be analyzed in the deionized water that pure aluminum nitrate is dissolved in 50ml, 2.4g urea is dissolved in the deionized water of 50ml, two kinds of solution are mixed, proceed in autoclave, 120 ℃ of reaction 24h, filter, washing, obtains cobalt aluminum bimetal hydroxide 60 ℃ of vacuumizes.The cobalt aluminum bimetal hydroxide of 1g is joined in the nitric acid 1000ml solution of the sodium nitrate that contains 1.5M and 0.005M, in solution, pass into nitrogen 15min, drive carbon dioxide away.Above-mentioned solution is at room temperature shaken 1 day, the product obtaining is filtered, washing, obtains the cobalt aluminum bimetal hydroxide after anion exchange 60 ℃ of vacuumizes.By the cobalt aluminum bimetal hydroxide after anion exchange and formamide solution 1:5 mixing in mass ratio, shake 1 day, 2000rpm centrifuging and taking supernatant liquor, obtains the layered cobalt aluminium duplex metal hydroxide nanometer sheet of peeling off.By the layered cobalt aluminium duplex metal hydroxide nanometer sheet solution of peeling off and the 50:1 mixing in proportion of stannic oxide/graphene nano sheet solution, stir 10min, standing 36h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain cobalt aluminum bimetal hydroxide/graphene oxide composite material.By composite material 200 ℃ of heat treatment 6h under nitrogen atmosphere, obtain cobalt aluminum bimetal hydroxide/graphene composite material.Above-mentioned composite material is made into electrode, and in 6mol/L potassium hydroxide electrolyte, test has good chemical property, can be applied to ultracapacitor.
Embodiment 4
1.746g is analyzed to pure cobalt nitrate and 1.125g to be analyzed in the deionized water that pure aluminum nitrate is dissolved in 50ml, 1.8g urea is dissolved in the deionized water of 50ml, two kinds of solution are mixed, proceed in autoclave, 120 ℃ of reaction 24h, filter, washing, obtains cobalt aluminum bimetal hydroxide 60 ℃ of vacuumizes.The cobalt aluminum bimetal hydroxide of 1g is joined in the nitric acid 1000ml solution of the sodium nitrate that contains 1.5M and 0.005M, in solution, pass into nitrogen 15min, drive carbon dioxide away.Above-mentioned solution is at room temperature shaken 1 day, the product obtaining is filtered, washing, obtains the cobalt aluminum bimetal hydroxide after anion exchange 60 ℃ of vacuumizes.By the cobalt aluminum bimetal hydroxide after anion exchange and formamide solution 1:5 mixing in mass ratio, shake 1 day, 2000rpm centrifuging and taking supernatant liquor, obtains the layered cobalt aluminium duplex metal hydroxide nanometer sheet of peeling off.By the layered cobalt aluminium duplex metal hydroxide nanometer sheet solution of peeling off and the 20:1 mixing in proportion of stannic oxide/graphene nano sheet solution, stir 10min, standing 36h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain cobalt aluminum bimetal hydroxide/graphene oxide composite material.By composite material 200 ℃ of heat treatment 6h under nitrogen atmosphere, obtain cobalt aluminum bimetal hydroxide/graphene composite material.Above-mentioned composite material is made into electrode, and in 6mol/L potassium hydroxide electrolyte, test has good chemical property, can be applied to ultracapacitor.
Embodiment 5
30% the hydrogen peroxide that measures 10% the tetramethyl ammonium hydroxide solution of 10ml and 2ml is made into the solution A of 20ml.The manganese chloride that weighs 0.594g is dissolved in the deionized water of 10ml and forms solution B.Solution A is joined in 15s in solution B, vigorous stirring 24h at room temperature then, 8000rpm centrifuge washing, is dispersed in water centrifugal precipitation of getting off, and ultrasonic 30min can form electronegative manganese dioxide nano-plates solution 4.20% the diallyl dimethyl ammoniumchloride solution 5 that measures 1ml joins in the manganese dioxide nano-plates solution of 100ml, under room temperature, stirs 2h, forms the modified manganese dioxide solution 6 of surface band positive charge, as shown in Figure 2.By the layered manganese oxide nanometer sheet solution of modification and the 1:1 mixing in proportion of stannic oxide/graphene nano sheet solution, stir 10min, standing 60h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain manganese dioxide/graphene oxide composite material 7.100mg composite material is dispersed in 100ml deionized water, adds the hydrazine hydrate of 1ml to the inside, 95 ℃ of oil bath reaction 6h, obtain manganese dioxide/graphene composite material.Above-mentioned composite material is made into electrode, in the metabisulfite solution of 1mol/L, has good capacitive property, can be applied to ultracapacitor.
Embodiment 6
The thioacetamide of the sodium vanadate of 2.399g and 2.254g is dissolved in the deionized water of 80ml, stirring at room 1h, then proceeds in autoclave, and 160 ℃ of reaction 24h, obtain vanadium disulfide presoma.Then the vanadium disulfide presoma of getting 40mg is dispersed in the deionized water of 60ml, passes into argon gas half an hour, drives oxygen away, sealing, ice-bath ultrasonic 3h, the electronegative vanadium disulfide nanometer sheet that obtains peeling off.Take 1mg hexadecyltrimethylammonium chloride and be made into 10ml solution, join in the vanadium disulfide nanometer sheet solution of 100ml, under room temperature, stir 2h, form the modification vanadium disulfide solution of surface band positive charge.By the stratiform vanadium disulfide nanometer sheet solution of modification and the 50:1 mixing in proportion of stannic oxide/graphene nano sheet solution, stir 10min, standing 10h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain vanadium disulfide/graphene oxide composite material.100mg composite material is dispersed in 100ml deionized water, adds the hydrazine hydrate of 1ml to the inside, 95 ℃ of oil bath reaction 6h, obtain vanadium disulfide/graphene composite material.Above-mentioned material is made into electrode, and the negative material as lithium battery, shows to have good application prospect.
Claims (6)
1. a preparation method for Two-dimensional Inorganic lamellar compound/graphene composite material, is characterized in that preparation process is as follows:
(1) Two-dimensional Inorganic lamellar compound presoma is peeled off into nanometer sheet in can reducing its solvent of peeling off energy; make positive charge on lamellar compound surface band; obtain positively charged lamellar compound solution, the mass ratio of lamellar compound and solvent is 1:1 ~ 1:20;
(2) by the surface of preparation with the nanometer sheet solution of positive charge and with the graphene oxide solution of negative electrical charge in proportion 1:1 ~ 50:1 mix, standing 6 ~ 60h, pour out supernatant liquor, centrifuge washing lower floor solution, obtains Two-dimensional Inorganic lamellar compound/graphene oxide composite material I;
(3) by Two-dimensional Inorganic lamellar compound/graphene oxide composite material I reduction, obtain Two-dimensional Inorganic lamellar compound/graphene composite material II.
2. according to the preparation method of the Two-dimensional Inorganic lamellar compound/graphene composite material described in claims 1, it is characterized in that: the Two-dimensional Inorganic lamellar compound presoma described in step (1) is stratiform transition metal hydroxide, stratiform transition metal oxide or laminated metal chalcogenide.
3. according to the preparation method of the Two-dimensional Inorganic lamellar compound/graphene composite material described in claims 1, it is characterized in that: its solvent of peeling off energy that can reduce described in step (1) is formamide, Tetramethylammonium hydroxide, 1-METHYLPYRROLIDONE, isopropyl alcohol or N-N-dimethyl formamide.
4. according to the preparation method of the Two-dimensional Inorganic lamellar compound/graphene composite material described in claims 1, it is characterized in that: described in step (1), make the lamellar compound lotus that becomes positively charged, if the positively charged of lamellar compound nanometer sheet of peeling off own, directly use, if the lamellar compound nanometer sheet of peeling off is electronegative, with cationic surfactant, modify, described cationic surfactant is hexadecyltrimethylammonium chloride, polyethylene propyl-dimethyl ammonium chloride, polypropylene amine hydrochloride or poly 4 vinyl pyridine.
5. according to the preparation method of the Two-dimensional Inorganic lamellar compound/graphene composite material described in claims 1, it is characterized in that: the solution with positive charge described in step (2) and with the graphene solution of negative electrical charge in proportion 1:1 ~ 20:1 mix.
6. according to the preparation method of the Two-dimensional Inorganic lamellar compound/graphene composite material described in claims 1, it is characterized in that: the method for reducing described in step (3) has electronation or thermal reduction.
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