CN106898504A - A kind of preparation method of the nano composite material based on Graphene - Google Patents
A kind of preparation method of the nano composite material based on Graphene Download PDFInfo
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- CN106898504A CN106898504A CN201710311734.5A CN201710311734A CN106898504A CN 106898504 A CN106898504 A CN 106898504A CN 201710311734 A CN201710311734 A CN 201710311734A CN 106898504 A CN106898504 A CN 106898504A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 55
- 239000000463 material Substances 0.000 title claims abstract description 46
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000725 suspension Substances 0.000 claims abstract description 23
- 150000002815 nickel Chemical class 0.000 claims abstract description 19
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 239000003002 pH adjusting agent Substances 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000002270 dispersing agent Substances 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- 230000004044 response Effects 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- 238000000354 decomposition reaction Methods 0.000 claims description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 5
- 235000019253 formic acid Nutrition 0.000 claims description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 5
- 229940078494 nickel acetate Drugs 0.000 claims description 5
- HZPNKQREYVVATQ-UHFFFAOYSA-L nickel(2+);diformate Chemical compound [Ni+2].[O-]C=O.[O-]C=O HZPNKQREYVVATQ-UHFFFAOYSA-L 0.000 claims description 5
- DITXJPASYXFQAS-UHFFFAOYSA-N nickel;sulfamic acid Chemical compound [Ni].NS(O)(=O)=O DITXJPASYXFQAS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 239000013049 sediment Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000004408 titanium dioxide Substances 0.000 claims description 5
- 239000002131 composite material Substances 0.000 abstract description 8
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 abstract description 7
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000006641 stabilisation Effects 0.000 abstract description 2
- 238000011105 stabilization Methods 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 6
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229960004424 carbon dioxide Drugs 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910001453 nickel ion Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 241000257465 Echinoidea Species 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
-
- 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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- 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
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Nanotechnology (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to a kind of preparation method of the nano composite material based on Graphene, with organic nickel salt and Graphene as raw material, nano composite material is prepared, preparing thinking is：Organic nickel salt is configured to acid solution; compounded with Graphene suspension and be aerated and constant pressure pyroreaction formation nickelous carbonate graphene composite structure after forming stabilization suspension, and carry out the nano composite material for protecting gas gradient sintering to obtain Graphene nickel protoxide.The present invention improves the stability of electric conductivity and morphosis；Preparation method is simple, is conducive to carrying out mass production, and low production cost.
Description
Technical field
The invention belongs to technical field of nano material, it is related to a kind of preparation side of the nano composite material based on Graphene
Method.
Background technology
In numerous carbon materials, Graphene or CNT are in recent years as the compound of carrier loaded nano-particle
By the new composite of a class of very big concern, this kind of compound is in all many-sides such as catalysis, electronics, optics, sensing
Illustrate many potential application performances, and research with material preparation method is constantly expanded with structure optimization.
Compared with CNT, Graphene can be regarded as the CNT for launching, also, Graphene possesses mechanical strength higher,
Larger specific surface area, cheap cost so that graphene-supported nano-particle compound has huge in terms of ultracapacitor
Big application potential.Meanwhile, the excellent electronic transmission performance of Graphene makes compound have prominent chemical property.Transition gold
Category oxide is most representational fake capacitance electrode material, and such as ruthenium-oxide, manganese dioxide, nickel oxide is all that specific capacitance is higher
Fake capacitance electrode material.Wherein, RuO2/H2SO4Water solution system is the most successful transition metal oxide base of current research
Capacitor, RuO2Electrode material can form high specific capacity, with good electric conductivity, but its price is high and to environment
Toxicity limits its large-scale application.Therefore, many research workers be devoted to finding cheap transition metal oxide and
Its composite substitutes ruthenium-oxide.NiO is wherein to study one of relatively broad cheaper alternative, and its theoretical capacity exists
More than 1000F/g, and cheap, the concern of extremely domestic and international researcher.In nature, NiO is tied with six sides
Structure, exists in the form of bunsenite stone, belongs to NaCl type cubic crystals.Nickel oxide oxygen content is indefinite, can be in certain scope
Change, its color shows grey black according to the order that oxygen content is reduced, and celadon is again to green.Due to the energy storage machine of NiO
Reason is that quick redox reaction occurs in electrode surface and body phase, produces Faraday pseudo-capacitance, therefore, the conduction of material
Property and morphosis are very big for the influence of the performance of electric capacity.
The content of the invention
The purpose of the present invention is exactly to provide a kind of electric conductivity and form for the defect for overcoming above-mentioned prior art to exist
The preparation method of constitutionally stable nano composite material.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of the nano composite material based on Graphene, its preparation process is as follows：
Step 1, organic nickel salt is put into absolute ethyl alcohol, and pH adjusting agent is added dropwise, and the nickel alcohol that pH is 4-6 is obtained after stirring
Liquid；
Step 2, after grapheme material is soaked into supersound washing, in addition distilled water, and adds dispersant, forms Graphene suspended
Liquid；
Step 3, under agitation, Graphene suspension is slowly added into nickel alcohol liquid, and titanium dioxide is passed through after being added dropwise to complete
Carbon gas carries out being aerated heating response 2-5h, obtains mixing suspension；
Step 4, constant pressure heating response 3-5h is added into reactor by mixing suspension, and cooled and filtered obtains mixed mixed precipitation
Thing；
Step 5, mixed sediment is put into Muffle furnace carries out protection gas gradient sintering decomposition 3-8h, obtains Graphene-oxidation
Sub- nickel nano composite material.
The preparation formula of the nano composite material needs love：
Organic nickel salt 15-20 parts, absolute ethyl alcohol 25-35 parts, pH adjusting agent 2-5 parts, Graphene 10-15 parts, distilled water 15-20
Part, dispersant 2-4 parts.
Organic nickel salt is using the one kind in nickel sulfamic acid, nickel acetate or nickel formate.
The pH adjusting agent is using the one kind in formic acid, acetic acid, hydrogen chloride.
The dispersant uses polyvinylpyrrolidone or polyoxyethylene polyoxypropylene.
Mixing speed in step 1 is 500-1000r/min, and the pH adjusting agent is added dropwise interval and is not less than 10min；Using
Compartment pH adjusting agent is added dropwise and ensure that pH regulating effects, while ensureing the stability of nickel ion, prevents pH to be mutated what is brought
Ion rendezvous problem.
It is the ethanol water of 70-90% that the solvent of the supersound washing in step 2 uses absolute ethyl alcohol or concentration of alcohol,
Supersonic frequency is 1-7kHz, and the ultrasonic time is 10-15min；Graphene is washed by the way of supersound washing, can not only
Good dispensing laundry effect is enough played, the impurity on surface is removed, while the discrete energy that ultrasound is produced can be to graphenic surface
Form Passivation Treatment.
Graphene suspension rate of addition in step 3 is 10-15mL/min, and the flow velocity of the aerated reaction is 10-
15mL/min, the temperature of the aerated reaction is 80-100 DEG C, and the pressure of the aerated reaction is 0.3-0.7MPa；Using slow
The mode of Graphene suspension is added dropwise can make full use of the effect of dispersant, Graphene is slowly dispersed in solution, molten
In agent transfer process reduce material reunion, using carbon dioxide as aerated reaction gas be in order to ensure Graphene with
The Combination of nickelous carbonate, reduces the respective reunion of Graphene and nickelous carbonate, it is ensured that the dispersiveness of Graphene and nickelous carbonate with mix
Effect, while organic nickel salt can be converted into nickelous carbonate by aerated reaction, can be by nickel ion precipitationization.
The temperature of the constant pressure heating response in step 4 is 130-180 DEG C, and pressure is 0.8-1.5MPa, is heated using constant pressure
Mode nickelous carbonate and graphite alkene reaction can be formed into Graphene-nickelous carbonate structure under the conditions of pressure and temperature.
Protection gas in step 5 uses the mode of nitrogen, the gradient sintering to be：1-2h is sintered under the conditions of 200 DEG C, so
The Isothermal sinter under the conditions of 300 DEG C afterwards；Can be by nickelous carbonate STRUCTURE DECOMPOSITION into nickel protoxide and two by the way of gradient sintering
Carbonoxide, forms the nano material of the Graphene-nickel protoxide structure of stabilization.
Compared with prior art, the invention has the characteristics that：
1）With organic nickel salt and Graphene as raw material, nano composite material is prepared, improve the steady of electric conductivity and morphosis
It is qualitative；Preparation method is simple, is conducive to carrying out mass production, and low production cost.
2）Nano composite material capacitive property prepared by the present invention has obtained large increase, is prepared using same method
Simple NiO electric capacity only has 225F/g, and composite electric capacity of the invention brings up to 505F/g, is doubled many.
3）Nano composite material specific capacitance prepared by the present invention is high, and good cycle, stability is strong.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of nickel oxide in composite obtained in embodiment 1.
Fig. 2 is composite charging and discharging curve obtained in embodiment 1.
Fig. 3 is the XRD spectrum of composite obtained in embodiment 1.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention
Premised on implemented, give detailed implementation method and specific operating process, but protection scope of the present invention is not limited to
Following embodiments.
Embodiment 1：
A kind of preparation method of the nano composite material based on Graphene, its preparation process is as follows：
Step 1, organic nickel salt is put into absolute ethyl alcohol, and pH adjusting agent is added dropwise, and the nickel alcohol that pH is 4-6 is obtained after stirring
Liquid；
Step 2, after grapheme material is soaked into supersound washing, in addition distilled water, and adds dispersant, forms Graphene suspended
Liquid；
Step 3, under agitation, Graphene suspension is slowly added into nickel alcohol liquid, and titanium dioxide is passed through after being added dropwise to complete
Carbon gas carries out being aerated heating response 2-5h, obtains mixing suspension；
Step 4, constant pressure heating response 3-5h is added into reactor by mixing suspension, and cooled and filtered obtains mixed mixed precipitation
Thing；
Step 5, mixed sediment is put into Muffle furnace carries out protection gas gradient sintering decomposition 3-8h, obtains Graphene-oxidation
Sub- nickel nano composite material.
The preparation formula of the nano composite material needs love：
Organic nickel salt 15-20 parts, absolute ethyl alcohol 25-35 parts, pH adjusting agent 2-5 parts, Graphene 10-15 parts, distilled water 15-20
Part, dispersant 2-4 parts.
Organic nickel salt is using the one kind in nickel sulfamic acid, nickel acetate or nickel formate.
The pH adjusting agent is using the one kind in formic acid, acetic acid, hydrogen chloride.
The dispersant uses polyvinylpyrrolidone or polyoxyethylene polyoxypropylene.
Mixing speed in step 1 is 500-1000r/min, and the pH adjusting agent is added dropwise interval and is not less than 10min.
It is the ethanol water of 70-90% that the solvent of the supersound washing in step 2 uses absolute ethyl alcohol or concentration of alcohol,
Supersonic frequency is 1-7kHz, and the ultrasonic time is 10-15min.
Graphene suspension rate of addition in step 3 is 10-15mL/min, and the flow velocity of the aerated reaction is 10-
15mL/min, the temperature of the aerated reaction is 80-100 DEG C, and the pressure of the aerated reaction is 0.3-0.7MPa.
The temperature of the constant pressure heating response in step 4 is 130-180 DEG C, and pressure is 0.8-1.5MPa.
Protection gas in step 5 uses the mode of nitrogen, the gradient sintering to be：1-2h is sintered under the conditions of 200 DEG C, so
The Isothermal sinter under the conditions of 300 DEG C afterwards.
The pattern of Fig. 1 sea urchin shapes is made up of netted nickel oxide nano piece, and the structure of this lamellar can be effectively
The contact area of increase active material and electrolyte, while being more beneficial for the electrochemical reaction process in the test of capacitive property
The short distance transport of ion, improves capacitive property, using Graphene as base material, can effectively improve leading for nickel oxide
Electrically, and with reference to electrode structure and special netted nickel oxide nano chip architecture, Graphene-nickel oxide composite material
Capacitive property provides the basis on structure and pattern；From Fig. 2 constant current charge-discharge diagrams, we can be calculated capacity measurement result
It is 505F/g；The XRD of product as shown in Figure 3, graphene/nickel oxide nano composite material, free from admixture in the product as seen from the figure
Peak.
Embodiment 2：
A kind of preparation method of the nano composite material based on Graphene, its preparation process is as follows：
Step 1, organic nickel salt is put into absolute ethyl alcohol, and pH adjusting agent is added dropwise, and the nickel alcohol that pH is 4-6 is obtained after stirring
Liquid；
Step 2, after grapheme material is soaked into supersound washing, in addition distilled water, and adds dispersant, forms Graphene suspended
Liquid；
Step 3, under agitation, Graphene suspension is slowly added into nickel alcohol liquid, and titanium dioxide is passed through after being added dropwise to complete
Carbon gas carries out being aerated heating response 2-5h, obtains mixing suspension；
Step 4, constant pressure heating response 3-5h is added into reactor by mixing suspension, and cooled and filtered obtains mixed mixed precipitation
Thing；
Step 5, mixed sediment is put into Muffle furnace carries out protection gas gradient sintering decomposition 3-8h, obtains Graphene-oxidation
Sub- nickel nano composite material.
The preparation formula of the nano composite material needs love：
Organic nickel salt 15-20 parts, absolute ethyl alcohol 25-35 parts, pH adjusting agent 2-5 parts, Graphene 10-15 parts, distilled water 15-20
Part, dispersant 2-4 parts.
Organic nickel salt is using the one kind in nickel sulfamic acid, nickel acetate or nickel formate.
The pH adjusting agent is using the one kind in formic acid, acetic acid, hydrogen chloride.
The dispersant uses polyvinylpyrrolidone or polyoxyethylene polyoxypropylene.
Mixing speed in step 1 is 500-1000r/min, and the pH adjusting agent is added dropwise interval and is not less than 10min.
It is the ethanol water of 70-90% that the solvent of the supersound washing in step 2 uses absolute ethyl alcohol or concentration of alcohol,
Supersonic frequency is 1-7kHz, and the ultrasonic time is 10-15min.
Graphene suspension rate of addition in step 3 is 10-15mL/min, and the flow velocity of the aerated reaction is 10-
15mL/min, the temperature of the aerated reaction is 80-100 DEG C, and the pressure of the aerated reaction is 0.3-0.7MPa.
The temperature of the constant pressure heating response in step 4 is 130-180 DEG C, and pressure is 0.8-1.5MPa.
Protection gas in step 5 uses the mode of nitrogen, the gradient sintering to be：1-2h is sintered under the conditions of 200 DEG C, so
The Isothermal sinter under the conditions of 300 DEG C afterwards.
Preparing the electric capacity of material, to be can be calculated by charge-discharge test be 505F/g.
Embodiment 3：
A kind of preparation method of the nano composite material based on Graphene, its preparation process is as follows：
Step 1, organic nickel salt is put into absolute ethyl alcohol, and pH adjusting agent is added dropwise, and the nickel alcohol that pH is 4-6 is obtained after stirring
Liquid；
Step 2, after grapheme material is soaked into supersound washing, in addition distilled water, and adds dispersant, forms Graphene suspended
Liquid；
Step 3, under agitation, Graphene suspension is slowly added into nickel alcohol liquid, and titanium dioxide is passed through after being added dropwise to complete
Carbon gas carries out being aerated heating response 2-5h, obtains mixing suspension；
Step 4, constant pressure heating response 3-5h is added into reactor by mixing suspension, and cooled and filtered obtains mixed mixed precipitation
Thing；
Step 5, mixed sediment is put into Muffle furnace carries out protection gas gradient sintering decomposition 3-8h, obtains Graphene-oxidation
Sub- nickel nano composite material.
The preparation formula of the nano composite material needs love：
Organic nickel salt 15-20 parts, absolute ethyl alcohol 25-35 parts, pH adjusting agent 2-5 parts, Graphene 10-15 parts, distilled water 15-20
Part, dispersant 2-4 parts.
Organic nickel salt is using the one kind in nickel sulfamic acid, nickel acetate or nickel formate.
The pH adjusting agent is using the one kind in formic acid, acetic acid, hydrogen chloride.
The dispersant uses polyvinylpyrrolidone or polyoxyethylene polyoxypropylene.
Mixing speed in step 1 is 500-1000r/min, and the pH adjusting agent is added dropwise interval and is not less than 10min.
It is the ethanol water of 70-90% that the solvent of the supersound washing in step 2 uses absolute ethyl alcohol or concentration of alcohol,
Supersonic frequency is 1-7kHz, and the ultrasonic time is 10-15min.
Graphene suspension rate of addition in step 3 is 10-15mL/min, and the flow velocity of the aerated reaction is 10-
15mL/min, the temperature of the aerated reaction is 80-100 DEG C, and the pressure of the aerated reaction is 0.3-0.7MPa.
The temperature of the constant pressure heating response in step 4 is 130-180 DEG C, and pressure is 0.8-1.5MPa.
Protection gas in step 5 uses the mode of nitrogen, the gradient sintering to be：1-2h is sintered under the conditions of 200 DEG C, so
The Isothermal sinter under the conditions of 300 DEG C afterwards.
Preparing the electric capacity of material, to be can be calculated by charge-discharge test be 505F/g.
The above-mentioned description to embodiment is to be understood that and use invention for ease of those skilled in the art.
Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel announcement of the invention, does not depart from improvement that scope made and modification all should be of the invention
Within protection domain.
Claims (10)
1. a kind of preparation method of the nano composite material based on Graphene, its preparation process is as follows：
Step 1, organic nickel salt is put into absolute ethyl alcohol, and pH adjusting agent is added dropwise, and the nickel alcohol that pH is 4-6 is obtained after stirring
Liquid；
Step 2, after grapheme material is soaked into supersound washing, in addition distilled water, and adds dispersant, forms Graphene suspended
Liquid；
Step 3, under agitation, Graphene suspension is slowly added into nickel alcohol liquid, and titanium dioxide is passed through after being added dropwise to complete
Carbon gas carries out being aerated heating response 2-5h, obtains mixing suspension；
Step 4, constant pressure heating response 3-5h is added into reactor by mixing suspension, and cooled and filtered obtains mixed mixed precipitation
Thing；
Step 5, mixed sediment is put into Muffle furnace carries out protection gas gradient sintering decomposition 3-8h, obtains Graphene-oxidation
Sub- nickel nano composite material.
2. a kind of preparation method of nano composite material based on Graphene according to claim 1, it is characterised in that institute
Stating the preparation formula of nano composite material needs love：
Organic nickel salt 15-20 parts, absolute ethyl alcohol 25-35 parts, pH adjusting agent 2-5 parts, Graphene 10-15 parts, distilled water 15-20
Part, dispersant 2-4 parts.
3. a kind of preparation method of nano composite material based on Graphene according to claim 2, it is characterised in that institute
Organic nickel salt is stated using the one kind in nickel sulfamic acid, nickel acetate or nickel formate.
4. a kind of preparation method of nano composite material based on Graphene according to claim 2, it is characterised in that institute
PH adjusting agent is stated using the one kind in formic acid, acetic acid, hydrogen chloride.
5. a kind of preparation method of nano composite material based on Graphene according to claim 2, it is characterised in that institute
Dispersant is stated using polyvinylpyrrolidone or polyoxyethylene polyoxypropylene.
6. a kind of preparation method of nano composite material based on Graphene according to claim 1, it is characterised in that step
Mixing speed in rapid 1 is 500-1000r/min, and the pH adjusting agent is added dropwise interval and is not less than 10min.
7. a kind of preparation method of nano composite material based on Graphene according to claim 1, it is characterised in that step
It is the ethanol water of 70-90% that the solvent of the supersound washing in rapid 2 uses absolute ethyl alcohol or concentration of alcohol, and supersonic frequency is
1-7kHz, the ultrasonic time is 10-15min.
8. a kind of preparation method of nano composite material based on Graphene according to claim 1, it is characterised in that step
Graphene suspension rate of addition in rapid 3 is 10-15mL/min, and the flow velocity of the aerated reaction is 10-15mL/min, described
The temperature of aerated reaction is 80-100 DEG C, and the pressure of the aerated reaction is 0.3-0.7MPa.
9. a kind of preparation method of nano composite material based on Graphene according to claim 1, it is characterised in that step
The temperature of the constant pressure heating response in rapid 4 is 130-180 DEG C, and pressure is 0.8-1.5MPa.
10. the preparation method of a kind of nano composite material based on Graphene according to claim 1, it is characterised in that
Protection gas in step 5 uses the mode of nitrogen, the gradient sintering to be：1-2h is sintered under the conditions of 200 DEG C, then 300
Isothermal sinter under the conditions of DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110655809A (en) * | 2019-10-29 | 2020-01-07 | 江苏华光粉末有限公司 | Polyamide wax modified sea urchin-shaped graphene and preparation method thereof, and anticorrosive powder coating and preparation process thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423897A (en) * | 2008-11-26 | 2009-05-06 | 东北大学 | Method for extracting nickel oxide from lateritic nickel |
| CN101863520A (en) * | 2010-06-17 | 2010-10-20 | 吕文广 | Preparation method of microporous ultrafine high activity nickel carbonate |
| CN102184781A (en) * | 2011-03-03 | 2011-09-14 | 上海大学 | Nano-nickel oxide/graphene composite material and preparation method thereof |
| CN103632857A (en) * | 2013-12-11 | 2014-03-12 | 西北师范大学 | Preparation method for nickel-oxide/ reduced-graphene-oxide nanosheet composite materials |
| KR20140035139A (en) * | 2012-09-13 | 2014-03-21 | 울산대학교 산학협력단 | Graphene/binary metal oxides nanocomposite and manufacturing method thereof |
| CN104795549A (en) * | 2015-03-20 | 2015-07-22 | 渤海大学 | Method for synthesizing graphene/nickel nano-composite material at room temperature |
-
2017
- 2017-05-05 CN CN201710311734.5A patent/CN106898504A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423897A (en) * | 2008-11-26 | 2009-05-06 | 东北大学 | Method for extracting nickel oxide from lateritic nickel |
| CN101863520A (en) * | 2010-06-17 | 2010-10-20 | 吕文广 | Preparation method of microporous ultrafine high activity nickel carbonate |
| CN102184781A (en) * | 2011-03-03 | 2011-09-14 | 上海大学 | Nano-nickel oxide/graphene composite material and preparation method thereof |
| KR20140035139A (en) * | 2012-09-13 | 2014-03-21 | 울산대학교 산학협력단 | Graphene/binary metal oxides nanocomposite and manufacturing method thereof |
| CN103632857A (en) * | 2013-12-11 | 2014-03-12 | 西北师范大学 | Preparation method for nickel-oxide/ reduced-graphene-oxide nanosheet composite materials |
| CN104795549A (en) * | 2015-03-20 | 2015-07-22 | 渤海大学 | Method for synthesizing graphene/nickel nano-composite material at room temperature |
Non-Patent Citations (4)
| Title |
|---|
| LINHAI ZHUO ET AL: "Trace Amounts of Water-Induced Distinct Growth Behaviors of NiO", 《ACS APPLIED MATERIALS & INTERFACES》 * |
| YUN HUANG ET AL: "Self-assembly of ultrathin porous NiO nanosheets/graphene hierarchical", 《JOURNAL OF MATERALS CHEMISTRY》 * |
| YUQIN ZOU ET AL: "NiO nanosheets grown on graphene nanosheets as superior anode materials", 《NANOSCALE》 * |
| 李秀艳: "超细NiO 粉体的制备及其应用研究进展", 《材料科学与工程学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110655809A (en) * | 2019-10-29 | 2020-01-07 | 江苏华光粉末有限公司 | Polyamide wax modified sea urchin-shaped graphene and preparation method thereof, and anticorrosive powder coating and preparation process thereof |
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Application publication date: 20170627 |