CN106486291B - A kind of NiO/rGO composite nano materials and preparation method thereof - Google Patents
A kind of NiO/rGO composite nano materials and preparation method thereof Download PDFInfo
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- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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- H01G11/22—Electrodes
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- 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
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- 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
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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H01M4/625—Carbon or graphite
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- 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
Abstract
The present invention discloses a kind of NiO/rGO composite nano materials and preparation method thereof.The NiO/rGO composite nano materials are the nano-complex of redox graphene and nickel oxide, and wherein redox graphene is the graphene nanoplatelets of single layer, and nickel oxide is nano particle, and nickel oxide（NiO）Nano particle is uniformly adhered to the surface of graphene oxide, forms clad structure.The present invention synthesizes NiO/rGO composite nano materials by solution methods, simple for process, and the additive amount of NiO and rGO is easily controllable, it can be achieved that effective controllable preparation.And NiO/rGO composite nano materials obtained are, it can be achieved that effective dispersion of the NiO particles on the surfaces rGO can be effectively increased the active site of reaction to reach larger specific surface area, so as to promote the response characteristic of the nanocomposite, expansion application field.
Description
Technical field
The present invention relates to the field of composite nano materials more particularly to a kind of metal oxides and graphene composite Nano material
Material and preparation method thereof.
Background technology
Nano material is because with many special fundamental propertys not available for traditional material, as bulk effect, surface are imitated
It answers, quantum size effect, macro quanta tunnel effect and Dielectric confinement effect etc. so that nano material has many special new
Function.In numerous nano materials, graphene is star's material in nano material, is regarded as most at the beginning of discovery
Thin but most tough material, 200 times more taller than best steel of fracture strength, and its maximum potential is the replacement as silicon
Product.Nickel oxide（NiO）Then it is widely used in battery, electrode material for super capacitor, is also widely used for the necks such as catalysis, sensing
Domain is that Nature comparison is special and a kind of widely used material in metal oxide materials.
Graphene is rational compound with the progress of nickel oxide nano material, the shared spy of two kinds of materials theoretically may be implemented
Point, the shortcomings that making up a kind of single nano material, while new synergistic effect can be also obtained, for example the lamellar structure of graphene can
To realize the position restriction to nickel oxide nanoparticle so that an effective dispersion may be implemented in nickel oxide nanoparticle, together
When graphene electric conductivity make the exchange that charge can also be realized between non-touching nickel oxide nanoparticle, this is for storage
The electrode material of energy device such as battery and ultracapacitor is helpful, while similarly anticipating to catalysis material and sensing material
Justice is great.Graphene is presently the most commonly redox graphene（rGO）, thus in the present invention we devise NiO with
The composite material of rGO, and being prepared using simple and practicable method is NiO/rGO composite nano materials in super electricity
The application in the fields such as container, lithium battery, catalysis, sensing provides critical material.
Invention content
It is an object of the invention to be directed to practical application request, a kind of NiO/rGO composite nano materials and its preparation are provided
Method.
The present invention provides a kind of NiO/rGO composite nano materials, are redox graphene（rGO）And nickel oxide
（NiO）Nano-complex, wherein rGO be single layer graphene nanoplatelets, NiO is nano particle, and NiO nano particles are equal
Even is attached to the surfaces rGO, forms clad structure.
The present invention also provides the preparation methods of above-mentioned NiO/rGO composite nano materials, include the following steps：
1）By the concentrated sulfuric acid（H2SO4）, potassium peroxydisulfate（K2S2O8）And phosphorus pentoxide（P2O5）Mixture be heated to 80
DEG C, it weighs a certain amount of graphite and is add to the above mixed solution and reacted, cooled to room temperature after the completion of reaction.Spend from
The careful eccentric cleaning of said mixture to PH is in neutrality by sub- water, and finally obtained solid is spontaneously dried 12h in air.
2）Using Hummers methods to passing through step 1）The graphite of pre-oxidation carries out after-treatment, first by step 1）In
To graphite oxide be added to and have cooled down to 0 DEG C of the concentrated sulfuric acid（H2SO4）In, then by potassium permanganate（KMnO4）In stirring and
It is slowly added under cooling condition, adding procedure will ensure that mixing bath temperature is no more than 20 DEG C slowly enough, will after the completion of addition
Mixed solution is warming up to 35 DEG C of reaction 2h, deionized water is then added, and the temperature of mixture is made to rise to 98 DEG C, by 15min
Afterwards, by a large amount of water and H2O2Aqueous solution is added to flask to terminate entire reaction, and mixed solution is cleaned to remove with HCl solution
Metal ion in solution finally cleans mixed solution with deionized water and is in neutrality to PH, the mixed solution after cleaning is spent
After ionized water dilution and ultrasound, just obtain dissolving good GO solution.
3）Weigh a certain amount of Nickelous nitrate hexahydrate（Ni(NO3)2∙6H2O）With citric acid (C6H8O7), it is configured to uniform molten
It is positioned over tube furnace reaction after liquid, certain reaction temperature is set, is waited after the completion of reacting, collecting reaction product nickel oxide（NiO）
It is dissolved in formation NiO solution in ammonium hydroxide, which is added to step 2）In obtained GO solution, it is transferred to after stirring evenly
It in the reaction kettle of polytetrafluoroethyllining lining, is then placed into baking oven and carries out hydro-thermal reaction, solid product is collected after the completion of reaction,
Filtering cleaning, you can obtain NiO/rGO composite nano materials.
Further, above-mentioned steps 1）In, H2SO4、K2S2O8、P2O5, graphite additional proportion be 6mL:2g:2g:1g,
Reaction time is 30 ~ 50min.
Further, above-mentioned steps 2）In, H2SO4、KMnO4, deionized water additional proportion be 46mL:6g:92mL.
Further, above-mentioned steps 2）In, Ni (NO3)2∙6H2O、C6H8O7Additional proportion be molar ratio 1:1.1, tubular type
Reaction temperature in stove is 190 ~ 200 DEG C, and hydrothermal temperature is 90 ~ 110 DEG C, and the hydro-thermal reaction time is 1 ~ 2h.
The useful achievement of the present invention is：
1) the NiO/rGO composite nano materials described in the method for the present invention, can be synthesized by solution methods, NiO and rGO
Additive amount it is easily controllable, thus NiO/rGO composite nano materials can realize effective controllable preparation.
2) NiO/rGO composite nano materials can have both the advantages of two kinds of materials of NiO and rGO, improve the electric property of the two,
Reach effective unification of high reaction activity and high conductivity, and form new synergistic effect, obtains more preferably comprehensive performance.
3) pass through rational reaction designing so that NiO nano particles are uniformly adhered to the surfaces rGO, NiO nano particles
Particle and particle can be realized by rGO, the charge-exchange between particle and substrate, so as to be effectively improved NiO as electricity
The performance of pole material, catalysis material, sensing material.
4) NiO/rGO composite nano materials described in, it can be achieved that NiO particles the surfaces rGO effective dispersion, to reach
Larger specific surface area can be effectively increased the active site of reaction, so as to promote the response characteristic of the nanocomposite, open up
Open up application field.
5) it is all prepared using solution methods, at low cost without vacuum equipment, technique is relatively simple, easily operated, can be real
Existing large-scale industrial production.
Description of the drawings
The redox graphene that Fig. 1 embodiments 2 are obtained by step 2（rGO）Scanning electron microscope（SEM）Figure；
The scanning electron microscope for the NiO/rGO composite nano materials that Fig. 2 embodiments 2 are obtained by step 3（SEM）Figure.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
1. by the 6 mL concentrated sulfuric acids（H2SO4）, 2 g potassium peroxydisulfates（K2S2O8）With 2 g phosphorus pentoxides（P2O5）Mixture
80 DEG C are heated to, 1 g graphite is weighed and is add to the above mixed solution and carry out reaction 30min, is naturally cooled to after the completion of reaction
Room temperature.The careful eccentric cleaning of said mixture to PH is in neutrality with deionized water, in air certainly by finally obtained solid
So dry 12h.
2. using Hummers methods to passing through step 1）The graphite of pre-oxidation carries out after-treatment, first by step 1）In
To graphite oxide be added to and have cooled down to 0 DEG C of the 46 mL concentrated sulfuric acids（H2SO4）In, then by 6 g potassium permanganate（KMnO4）
In stirring and being slowly added under cooling condition, adding procedure will ensure that mixing bath temperature is no more than 20 DEG C slowly enough, addition
Mixed solution is warming up to 35 DEG C of reaction 2h after the completion, 92 mL deionized waters are then added, and the temperature of mixture is made to rise to
98 DEG C, after 15min, by a large amount of water and H2O2Aqueous solution is added to flask to terminate entire reaction, is cleaned with HCl solution
Mixed solution finally cleans mixed solution with deionized water and is in neutrality to PH to remove the metal ion in solution.By what is obtained
Suspension is diluted with deionized water and has just obtained the good GO solution of dissolving after ultrasound.
3. it is 1 to weigh molar ratio:1.1 Nickelous nitrate hexahydrate（Ni(NO3)26H2O）With citric acid (C6H8O7), it is configured to
It is positioned in tube furnace after uniform solution, setting reaction temperature is 200 DEG C, is waited after the completion of reacting, collecting reaction product nickel oxide
（NiO）It is dissolved in ammonium hydroxide, NiO solution is added to step 1）In obtained GO solution, polytetrafluoroethyl-ne is transferred to after stirring evenly
In the reaction kettle of alkene liner, it is then placed into baking oven after the completion of 90 DEG C of 1 h of hydro-thermal reaction, reaction and collects solid product mistake
Filtering, which is washed, can obtain NiO/rGO composite nano materials.
Embodiment 2
1. by the 6 mL concentrated sulfuric acids（H2SO4）, 2 g potassium peroxydisulfates（K2S2O8）With 2 g phosphorus pentoxides（P2O5）Mixture
80 DEG C are heated to, 1 g graphite is weighed and is add to the above mixed solution and carry out reaction 40min, is naturally cooled to after the completion of reaction
Room temperature.The careful eccentric cleaning of said mixture to PH is in neutrality with deionized water, in air certainly by finally obtained solid
So dry 12h.
2. using Hummers methods to passing through step 1）The graphite of pre-oxidation carries out after-treatment, first by step 1）In
To graphite oxide be added to and have cooled down to 0 DEG C of the 46 mL concentrated sulfuric acids（H2SO4）In, then by 6 g potassium permanganate（KMnO4）
In stirring and being slowly added under cooling condition, adding procedure will ensure that mixing bath temperature is no more than 20 DEG C slowly enough, addition
Mixed solution is warming up to 35 DEG C of reaction 2h after the completion, 92 mL deionized waters are then added, and the temperature of mixture is made to rise to
98 DEG C, after 15min, by a large amount of water and H2O2Aqueous solution is added to flask to terminate entire reaction, is cleaned with HCl solution
Mixed solution finally cleans mixed solution with deionized water and is in neutrality to PH to remove the metal ion in solution.By what is obtained
Suspension is diluted with deionized water and has just obtained the good GO solution of dissolving after ultrasound.
3. it is 1 to weigh molar ratio:1.1 Nickelous nitrate hexahydrate（Ni(NO3)26H2O）With citric acid (C6H8O7), it is configured to
It is positioned in tube furnace after uniform solution, setting reaction temperature is 190 DEG C, is waited after the completion of reacting, collecting reaction product nickel oxide
（NiO）It is dissolved in ammonium hydroxide, NiO solution is added to step 1）In obtained GO solution, polytetrafluoroethyl-ne is transferred to after stirring evenly
In the reaction kettle of alkene liner, it is then placed into baking oven after the completion of 110 DEG C of 2 h of hydro-thermal reaction, reaction and collects solid product mistake
Filtering, which is washed, can obtain NiO/rGO composite nano materials.
Embodiment 3
1. by the 6 mL concentrated sulfuric acids（H2SO4）, 2 g potassium peroxydisulfates（K2S2O8）With 2 g phosphorus pentoxides（P2O5）Mixture
80 DEG C are heated to, 1 g graphite is weighed and is add to the above mixed solution and carry out reaction 50min, is naturally cooled to after the completion of reaction
Room temperature.The careful eccentric cleaning of said mixture to PH is in neutrality with deionized water, in air certainly by finally obtained solid
So dry 12h.
2. using Hummers methods to passing through step 1）The graphite of pre-oxidation carries out after-treatment, first by step 1）In
To graphite oxide be added to and have cooled down to 0 DEG C of the 46 mL concentrated sulfuric acids（H2SO4）In, then by 6 g potassium permanganate（KMnO4）
In stirring and being slowly added under cooling condition, adding procedure will ensure that mixing bath temperature is no more than 20 DEG C slowly enough, addition
Mixed solution is warming up to 35 DEG C of reaction 2h after the completion, 92 mL deionized waters are then added, and the temperature of mixture is made to rise to
98 DEG C, after 15min, by a large amount of water and H2O2Aqueous solution is added to flask to terminate entire reaction, is cleaned with HCl solution
Mixed solution finally cleans mixed solution with deionized water and is in neutrality to PH to remove the metal ion in solution.By what is obtained
Suspension is diluted with deionized water and has just obtained the good GO solution of dissolving after ultrasound.
3. it is 1 to weigh molar ratio：1.1 Nickelous nitrate hexahydrate（Ni(NO3)26H2O）With citric acid (C6H8O7), it is configured to
It is positioned in tube furnace after uniform solution, setting reaction temperature is 210 DEG C, is waited after the completion of reacting, collecting reaction product nickel oxide
（NiO）It is dissolved in ammonium hydroxide, NiO solution is added to step 1）In obtained GO solution, polytetrafluoroethyl-ne is transferred to after stirring evenly
In the reaction kettle of alkene liner, it is then placed into baking oven after the completion of 100 DEG C of 1.5 h of hydro-thermal reaction, reaction and collects solid product
Filtering cleaning can obtain NiO/rGO composite nano materials.
To the above various embodiments step 2）Graphene oxide obtained and last NiO/rGO composite nano materials obtained
It is scanned Electronic Speculum and observes its pattern.The redox graphene obtained by step 2 such as Fig. 1 embodiments 2（rGO）Scanning
Electronic Speculum（SEM）Figure, it can be seen that rGO is the graphene nanoplatelets of single layer.Fig. 2 is what embodiment 2 was obtained by step 3
The scanning electron microscope of NiO/rGO composite nano materials（SEM）Scheme, show that final product is NiO/rGO composite nano materials in figure,
NiO is nano particle, and NiO nano particles are uniformly adhered to rGO graphene nanoplatelets surface, form clad structure.
Claims (5)
1. a kind of preparation method of NiO/rGO composite nano materials, it is characterised in that include the following steps：
1) by dense H2SO4、K2S2O8And P2O5Mixture be heated to 80 DEG C, weigh a certain amount of graphite and be added in said mixture
Carry out pre-oxidation, cooled to room temperature after the completion of reaction, with deionized water by the careful eccentric cleaning of said mixture extremely
PH is in neutrality, and finally obtained solid is spontaneously dried 12h in air；
Wherein, dense H2SO4、K2S2O8、P2O5, graphite additional proportion be 6mL:2g:2g:1g；
2) after-treatment is carried out to the graphite by step 1) pre-oxidation, is first added to the graphite oxide obtained in step 1)
Have cooled down to 0 DEG C of dense H2SO4In, then by KMnO4In stirring and being slowly added under cooling condition, adding procedure is to ensure to mix
It closes solution temperature and is no more than 20 DEG C, mixed solution is warming up to 35 DEG C of reaction 2h after the completion of addition, deionized water is then added, and
The temperature of mixture is set to rise to 98 DEG C, after 15min, by a large amount of water and H2O2It is entire to terminate that aqueous solution is added to flask
Reaction, cleans mixed solution with HCl solution to remove the metal ion in solution, finally cleans mixed solution extremely with deionized water
PH is in neutrality；Mixed solution after cleaning is diluted with deionized water and has just obtained the good GO solution of dissolving after ultrasound；
3) a certain amount of Ni (NO are weighed3)2·6H2O and citric acid C6H8O7, the molar ratio of the two is 1：1.1, it is configured to uniform molten
It is positioned over tube furnace reaction after liquid, waits after the completion of reacting, collecting reaction product NiO is dissolved in ammonium hydroxide, which is added to
In the GO solution that step 2) obtains, it is transferred in the reaction kettle of polytetrafluoroethyllining lining after stirring evenly, is then placed into baking oven
Middle carry out hydro-thermal reaction, solid product filtering cleaning is collected after the completion of reaction can obtain NiO/rGO composite nano materials.
2. a kind of preparation method of NiO/rGO composite nano materials according to claim 1, it is characterised in that：In step 1),
The pre-oxidation time is 30~50min.
3. a kind of preparation method of NiO/rGO composite nano materials according to claim 1, it is characterised in that：In step 2),
Dense H2SO4、KMnO4, deionized water additional proportion be 46mL:6g:92mL.
4. a kind of preparation method of NiO/rGO composite nano materials according to claim 1, it is characterised in that step 3) middle pipe
The temperature reacted in formula stove is 190-210 DEG C.
5. a kind of preparation method of NiO/rGO composite nano materials according to claim 1, it is characterised in that water in step 3)
Thermal response temperature is 90-110 DEG C, time 1-2h.
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| WO2019095091A1 (en) * | 2017-11-14 | 2019-05-23 | The University Of Hong Kong | Nickel oxide decorated graphene oxide nanocomposite as a hole transport layer and method of manufacturing the same |
| CN108922792B (en) * | 2018-07-13 | 2020-01-07 | 黑龙江省科学院高技术研究院 | Preparation method of graphene/ZnO/NiO composite material |
| CN109056306A (en) * | 2018-09-12 | 2018-12-21 | 山东理工大学 | A kind of preparation method of NiO/Ni composite graphite alkene cladding cotton carbon fibre material |
| CN109187512B (en) * | 2018-09-17 | 2021-07-20 | 四川大学 | Catalytic luminescence analysis method and sensor device for detecting hydrogen sulfide based on nickel oxide |
| CN110690443B (en) * | 2019-09-29 | 2020-12-22 | 贵州梅岭电源有限公司 | Preparation method and application of lithium-rich manganese material with nickel element in gradient distribution |
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