CN106340391A - Graphene/nickel hydroxide composite material and preparation method thereof, and electrode material - Google Patents
Graphene/nickel hydroxide composite material and preparation method thereof, and electrode material Download PDFInfo
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- CN106340391A CN106340391A CN201610978102.XA CN201610978102A CN106340391A CN 106340391 A CN106340391 A CN 106340391A CN 201610978102 A CN201610978102 A CN 201610978102A CN 106340391 A CN106340391 A CN 106340391A
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- H—ELECTRICITY
- 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
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- 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
- 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 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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- 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
Abstract
The invention provides a preparation method of a graphene/nickel hydroxide composite material. The method comprises that oxidized graphene, water, hexamethylene tetramine and a nickel source are mixed, heated and reacted to obtain the graphene/nickel hydroxide composite material. A simple hydrothermal method is used to synchronize generation of nanometer nickel hydroxide with reduction of oxidized graphene, two-phase combination is carried out in source and microscopic levels, and the composite material in which nanometer nickel hydroxide is attached to the sheet-shaped graphene uniformly is prepared. The composite material combines the advantages that graphene has a large specific surface area and high conductivity with that nanometer nickel hydroxide is high in the specific capacity, and the composite material has high integrated performance when being used for a super capacitor.
Description
Technical field
The present invention relates to electrode material technical field, more particularly, to Graphene/nickel hydroxide composite, its preparation method
With electrode material.
Background technology
As a kind of new energy-storage travelling wave tube, it combines the feature of electrostatic container and chemical cell to ultracapacitor, tool
Have the advantages that power density is big, good cycle and environmentally safe, therefore, ultracapacitor is widely used in energy and returns
The fields such as receipts, electric capacity automobile and instrument and meter, are a kind of huge technology of application prospect.
Electrode material is the core of energy-storage travelling wave tube, and the thing phase composition of material and microstructure decide the physico of material
Learn performance.Big specific surface area not only can produce considerable electric double layer capacitance, and provides for the electrochemical reaction of fake capacitance
More active sites；Suitable pore-size distribution is conducive to electrolyte to penetrate in electrode and redox reaction occurs, and also helps double
The discharge and recharge reaction of electric layer.Therefore, preparation specific surface area is big and the material of porous pattern and being combined using composite mixed preparation
Material is the study hotspot in ultracapacitor field.
When material with carbon element is as electrode material for super capacitor, specific surface area effective rate of utilization is very low, is because it contains greatly
The micropore of amount, and the micropore that these apertures are less than 2nm can not be effectively formed electric double layer.Graphene (rgo) is with sp2Hybridized orbit
, as the problems referred to above during electrode material, there is not expansion in the bi-dimensional cellular cancellated individual layer carbon atom of composition
Scattered problem, and specific surface area is big, can modify substantial amounts of functional group thereon so as to have high pliability, excellent leading
Electrical property, high chemical stability and heat endurance and wide voltage window etc..Therefore, Graphene both can improve electrode material
The electric conductivity of material and electro-chemical activity, can improve the cyclical stability of electrode material, as electrode material for super capacitor again
There is absolute predominance.
But single Graphene electrodes material is than limited capacitance, internal resistance is larger.In order to improve graphene-based electrode further
The chemical property of material, can be compounded to form composite by the certain heteroatom of doping introducing or with other materials,
Form certain fake capacitance.Nickel hydroxide is typical p-type broad-band gap hydroxide, is produced by the redox reaction of ni ion
Raw fake capacitance, has high specific capacity and big energy density, and chemical property is good, low cost, often by independent or be combined and be used for
Electrode material for super capacitor.
Therefore, if by the Graphene with special construction and the ni (oh) with fake capacitance2Compound, form combination electrode,
Due to complex effect, the composite obtaining certainly will have more excellent chemical property.
At present, researcher has been also carried out the compound, for example: using tradition sides such as mechanical mixture of Graphene and nickel hydroxide
Method, but Graphene and ni (oh)2It is difficult to compound uniform, the simply mixing in macroscopic aspect, so that this compound advantage is significantly cut
Weak.Therefore, it is intended to obtain homogeneous composite, plays its compound advantage, consider from the nucleating growth that microcosmic point is crystal grain outstanding
For important.Wherein, although coprecipitation is poor with the simple homogeneity of chemical reduction method, the work such as electrodeposition process and chemical polymerization
Skill is again excessively complicated, is not suitable for large-scale industrial production, still needs to improve.
Content of the invention
Present invention solves the technical problem that being to provide a kind of preparation method of Graphene/nickel hydroxide composite, this
Graphene/nickel hydroxide composite the uniformity of application preparation preferably, has preferable chemical property as electrode material.
In view of this, this application provides a kind of preparation method of Graphene/nickel hydroxide composite, comprising:
Graphene oxide, water, hexamethylenetetramine are mixed with nickel source, heating, after reaction, obtain Graphene/nickel hydroxide
Composite；Described nickel source is to ionize out ni in water2+Nickel source.
Preferably, also include after described reaction:
Freeze-drying after the product obtaining is washed.
Preferably, the temperature of described heating is 140～200 DEG C, and the temperature retention time of described heating is 16～24h.
Preferably, in described mixed mixed liquor, the concentration of described pregnancy urotropine is 0.1～2mol/l, described nickel
The concentration in source is 0.1～2mol/l.
Preferably, the ratio of described graphene oxide and described water is (0.01～2) g: 100ml.
Preferably, described nickel source is one of nickel sulfate and nickel nitrate or two kinds.
Present invention also provides a kind of Graphene/nickel hydroxide composite, including Graphene be compound in described graphite
The nickel hydroxide on alkene surface.
Preferably, described nickel hydroxide and the mass ratio of Graphene are (3～5): 1.
Preferably, described nickel hydroxide is α-ni (oh)2.
Present invention also provides a kind of electrode material, described electrode material is prepared by the preparation method described in such scheme
Or such scheme described in Graphene/nickel hydroxide composite.
This application provides a kind of preparation method of Graphene/nickel hydroxide composite, it is particularly as follows: by graphite oxide
Alkene, water, hexamethylenetetramine are mixed with nickel source, heating, obtain Graphene/nickel hydroxide composite after reaction.The application exists
During preparing Graphene/nickel hydroxide composite, using hydro-thermal method by the reduction of graphene oxide and nanometer hydroxide
The generation of nickel is carried out simultaneously, makes Graphene and nickel hydroxide carry out the compound of two-phase, the nanometer hydrogen of preparation on a microscopic level
Nickel oxide is uniformly attached to the graphenic surface of lamellar, defines Graphene/nickel hydroxide composite.
The composite of the application preparation is mutually tied by the extensive chemical effect of nickel hydroxide and graphenic surface functional group
Close and conductive, electronics from the oxidized defect of Graphene to nickel hydroxide transmit, lead to nickel hydroxide negatively charged, formation nickel hydroxide
The unilateal conduction behavior of nano-particle, thus improve the chemical property of nickel hydroxide；The graphite of composite set simultaneously
The electrochemical double layer electric capacity of alkene and quasi- faraday's electric capacity, finally improve the electrochemistry of Graphene/nickel hydroxide composite
Energy.
Brief description
Fig. 1 is the tem photo of the Graphene/nickel hydroxide composite of the embodiment of the present invention 1 preparation；
The illustraton of model of the Graphene that Fig. 2 provides for the present invention/nickel hydroxide composite；
Fig. 3 is Graphene/nickel hydroxide composite, single-phase graphite alkene and the single-phase hydrogen-oxygen of the embodiment of the present invention 1 preparation
Change the cv curve map of nickel；
Fig. 4 is Graphene/nickel hydroxide composite, single-phase graphite alkene and the single-phase hydrogen-oxygen of the embodiment of the present invention 1 preparation
Change the gcd curve map of nickel.
Specific embodiment
For a further understanding of the present invention, with reference to embodiment, the preferred embodiment of the invention is described, but
It should be appreciated that these descriptions are simply to further illustrate the features and advantages of the present invention, rather than to the claims in the present invention
Limit.
The embodiment of the invention discloses a kind of preparation method of Graphene/nickel hydroxide composite, comprising:
Graphene oxide, water, hexamethylenetetramine are mixed with nickel source, heating, after reaction, obtain Graphene/nickel hydroxide
Composite；Described nickel source is to ionize out ni in water2+Nickel source.
As shown in Fig. 2 illustraton of model prepared by Graphene/nickel hydroxide composite that Fig. 2 provides for the present invention, can by figure
Know, the reduction of the generation of nano-sized nickel hydroxide and Graphene is carried out by the application using the hydro-thermal method of process is simple simultaneously, from root
Two-phase is carried out on source and microcosmic point be combined, prepared nano-sized nickel hydroxide and be uniformly attached to formation on the Graphene of lamellar
Composite.The composite of the application preparation has bigger serface, good electric conductivity and the nanometer hydrogen-oxygen of Graphene concurrently
Change the big advantage of nickel specific capacity, make composite be used for ultracapacitor excellent combination property.
According to the present invention, during preparing Graphene/nickel hydroxide composite, first raw material is mixed
Close, described raw material includes graphene oxide (go), water, hexamethylenetetramine and can ionize out ni in water2+Nickel source；The application
The source of graphene oxide (go), hexamethylenetetramine and nickel source is all had no particular limits, be commercially available prod or according to this
Mode known to skilled person prepares.In order that raw material mixes, the process of above-mentioned raw materials mixing is concrete
For:
Graphene oxide is dispersed in water, using the ultrasonic 1～3h of ultrasonic device, adds nickel source and six methines four
Amine, magnetic agitation 20～40min, obtain mixed liquor.
In above process, the ratio of described graphene oxide and water is preferably (0.01～2) g: 100ml, in embodiment
In, the ratio of described graphene oxide and water is more preferably (0.05～1.0) g: 100ml.In the mixed liquor of above-mentioned preparation, institute
The concentration stating hexamethylenetetramine is preferably 0.1～2mol/l, and in an embodiment, the concentration of described hexamethylenetetramine is more preferably
For 0.5～1.5mol/l；The concentration of described nickel source is preferably 0.1～2mol/l, and in an embodiment, the concentration of described nickel source is more excellent
Elect 0.5～1.5mol/l as.The concentration of above-mentioned raw materials and proportionate relationship are to the pattern of composite and performance important.
Wherein, the concentration of hexamethylenetetramine and nickel source decides the pattern of nickel hydroxide, particle diameter and dispersiveness in composite, both
Excessive concentration is too low or relative scale not in the range of all can cause nickel hydroxide particle diameter excessive or too small, pattern is irregular,
It is led to be difficult dispersed in graphene layer.The application has no particular limits to described nickel source, as long as energy in water
Ionize out ni2+Nickel source, example, described nickel source be nickel sulfate (niso4·6h2O) with nickel nitrate (ni (no3)2) in
One or two.
After mixing raw material, the application preferably imports mixed liquor in ptfe autoclave and is reacted, with
When airtight hydro-thermal tank heated, after reaction, that is, obtain Graphene/nickel hydroxide composite.In above process, described plus
The temperature of heat is preferably 140～200 DEG C, in an embodiment, more preferably 160～180 DEG C of the temperature of described heating, described heating
Temperature retention time be 16～24h, time of described insulation is more preferably 18～20h；The temperature of above-mentioned heating and temperature retention time
It is pattern and the performance important factor in order of composite.Wherein, the temperature and time that it is critical only that insulation of hydro-thermal method, such as
Fruit temperature is too low or the time is too short, and the generation of nickel hydroxide and the reduction of Graphene are not abundant, and component and pattern are imperfect, and
Temperature retention time is too high or overlong time, can lead to more side reactions and the generation of agglomeration, these are all unfavorable for compound
Formed and performance.In above-mentioned course of reaction, described hexamethylenetetramine, as precipitating reagent, provides oh-, with ni2+In conjunction with
Generate ni (oh)2, it, again as template, regulates and controls ni (oh)2Pattern, specifically, (ch2)6n4(hmt) as template and heavy
Shallow lake agent, in initial nucleation process, (ch2)6n4(hmt) as ph buffer, oh is slowly released by thermal decomposition-, meanwhile,
Hmt, as template, carries ni2+It is determined that ni2+Position, make ni2+With oh-Form body-centered octahedral structure, ni2+It is located at
Octahedral body-centered, oh-In octahedral six vertex positions, this octahedral structure arrangement form octahedral in two dimensional surface
Body layer, is superimposed in the presence of the layer hydrogen bond that hydroxyl on a neighboring layer is formed with layer, arranged in parallel on c-axis direction, forms water
Magnesite structure is α-ni (oh)2；During this there is reduction reaction in graphene oxide (go) simultaneously, generates Graphene (rgo), stone
Black alkene (rgo) and nickel hydroxide (ni (oh)2) between pass through ni (oh)2Mutual suction-operated and rgo oxide group between is multiple
Close, and this kind of suction-operated is ni (oh)2In the o coupling that exists of the oxide group on ni and rgo surface formed.
This process specifically there occurs the reduction process of the hydrolysis of hexamethylenetetramine, the precipitation of nickel hydroxide and graphene oxide, specifically
Chemical reaction is as follows:
(ch2)6n4+10h2o→6hcho+4nh3·h2o；
nh3·h2o→nh4 ++oh-:
ni2++2oh-→ni(oh)2；
go→rgo.
For the ease of the application of Graphene/nickel hydroxide composite, the product that above-mentioned reaction is preferably obtained by the application
Washed, then carried out freeze-drying, finally given Graphene/nickel hydroxide composite.In this step, described washing with
Described freeze-drying is technological means well known to those skilled in the art, is not particularly limited herein.
The present invention under hydrothermal conditions, the precipitation of the reduction of graphene oxide and nickel hydroxide is carried out simultaneously, generation
Nickel hydroxide is interacted with Graphene, so that the nickel hydroxide of Emission in Cubic is fallen on the two dimensional surface of Graphene, forms compound phase
Graphene/nickel hydroxide (rgo/ni (oh)2) composite.
Present invention also provides a kind of Graphene/nickel hydroxide composite being prepared by said method, described multiple
Condensation material is made up of with the nickel hydroxide being compounded in graphenic surface Graphene.
The Graphene of the present invention/nickel hydroxide composite is by the phase between nickel hydroxide and Graphene oxide group
Interaction is combined together, and nano-sized nickel hydroxide is uniformly attached on the Graphene of lamellar.
Graphene in Graphene in the application/nickel hydroxide composite and ni (oh)2Have one's own work to do, ni (oh)2Carry
For the ratio electric capacity of composite, Graphene provides the passage of electric transmission, and both ratio is too small or cross mostly can not be maximum
The composite performance of this composite of performance of degree, the mass ratio of nickel hydroxide described herein and Graphene be preferably (3～
5): 1, as ni (oh)2When ratio with Graphene is about 4: 1, its chemical property is optimum state.Now, ni
(oh)2Can be evenly dispersed on graphene substrate, ni (oh)2Prevent the stacking between graphene layer, prevent its specific surface area
Overlapping waste, and Graphene is ni (oh)2Redox reaction provide splendid place, for reaction electronics and ion pass
Defeated provide multiple broad passage, now composite reach optimum chemical property.In described composite, hydroxide
Ni in nickel2+With oh-Form body-centered octahedral structure, ni2+Positioned at octahedral body-centered, oh-In octahedral six summits position
Put, this octahedral structure arrangement form octahedral layer in two dimensional surface, the hydrogen that layer and layer hydroxyl on a neighboring layer is formed
It is superimposed in the presence of key, arranged in parallel on c-axis direction, forming shepardite structure is α-ni (oh)2.
Present invention also provides a kind of electrode material, described electrode material prepared by such scheme or such scheme institute
The Graphene stated/nickel hydroxide composite.
Above-mentioned electrode material can be the electrode material of ultracapacitor or the electrode material of lithium ion battery,
This application is had no particular limits；Preferably, herein described electrode material is the electrode material of ultracapacitor
Material.
Above-mentioned ultracapacitor is ultracapacitor well known to those skilled in the art, and it is that electrode material is this Shen
Graphene/nickel hydroxide composite that please be described, other parts all do not change.
Graphene/nickel hydroxide composite that the application provides, can suppress the reunion of Graphene and nickel hydroxide simultaneously,
Effectively improve the chemical stability of nickel hydroxide, and gather the electrochemical double layer electric capacity of Graphene and quasi- faraday's electric capacity, by
This improves the chemical property of composite；Further, Graphene has the physical property such as intensity, tough of uniqueness in itself
Property, can be nanometer ni (oh)2Particulate provides support system and skeleton so that rgo/ni (oh)2Composite entirety mechanicalness
Can be excellent.
For a further understanding of the present invention, it is combined with reference to Graphene/nickel hydroxide that embodiment provides to the present invention
The preparation method of material is described in detail, and protection scope of the present invention is not limited by the following examples.
Raw material in following examples is commercially available prod.
Embodiment 1
0.1g graphene oxide is taken to be distributed in the middle of the 100ml aqueous solution, with the ultrasonic 1h of the ultrasonic device of 1000w power, then
Add a certain amount of nickel sulfate (niso4·6h2O) with hexamethylenetetramine ((ch2)6n4) all it is configured to 0.5mol/l, magnetic force stirs
Mix 30min, ultrasonic good uniform solution is poured in ptfe autoclave, airtight good hydro-thermal tank, it is heated to 180 DEG C of insulations
20h；Take out product, freeze-drying after massive laundering after container cooling, obtain final product.
As shown in figure 1, Fig. 1 is the tem photo of Graphene manufactured in the present embodiment/nickel hydroxide composite, in figure stone
Black alkene (at arrow) is the big tissue layer of specific surface area, and nano-sized nickel hydroxide is attached on graphene layer, forms Graphene/hydrogen-oxygen
Change nickel composite construction；Fig. 3 and Fig. 4 is respectively single-phase ni (oh)2, rgo and rgo/ni (oh)2Composite is in koh electrolyte
Cyclic voltammetry curve figure (cv) and its constant current discharge curve map (gcd)；From the figure 3, it may be seen that the cv scanning of composite all occurs
A pair of redox peaks, oxidation peak characterizes ni (oh)2+oh-→niooh+h2o+e-Reaction, ion good dispersion, be conducive to reacting
To bulk diffusion, material use reduction peak then corresponds to its inverse process to thing；As can be seen that rgo/ni (oh)2Composite presents
Broader redox peaks and bigger peak current density, this is because this ni (oh)2Nanoparticle rate its oxidation rate of height is very fast,
Interface resistance is little.As can be seen here, Graphene is to ni (oh)2The chemical property of super capacitor material truly has and is obviously improved.By
Fig. 4 can be seen that, under identical discharge current density, rgo/ni (oh)2The discharge time of composite is than single-phase ni (oh)2
With rgo length, i.e. rgo/ni (oh)2Higher than capacitance, thus showing rgo/ni (oh)2Composite electro-chemical activity is preferable；By
Charging and discharging curve can calculate the specific capacity of electrode, shown in the following formula of calculating process,
Cs=it/ δ v, m；
Wherein, cs refers to charging and discharging currents；T is discharge time；δ v is potential difference；M is the quality of active material；
In the present embodiment, known by figure, t is 450s, δ v is 0.4v, current density i/m takes 0.8a/g.Thus can calculate
Go out Graphene/nickel hydroxide composite cs under the current density of 1a/g, it is up to 1000f/g than electric capacity.Further knot
Fruit shows, its charge and discharge cycles still can reach 94% 500 times.
Embodiment 2
0.05g graphene oxide is taken to be distributed in the middle of the 100ml aqueous solution, with the ultrasonic 1h of the ultrasonic device of 1000w power, then
Add a certain amount of nickel sulfate (niso4·6h2O) with hexamethylenetetramine ((ch2)6n4) all it is configured to 0.4mol/l, magnetic force stirs
Mix 30min, ultrasonic good uniform solution is poured in ptfe autoclave, airtight good hydro-thermal tank, it is heated to 180 DEG C of insulations
18h；Take out product, freeze-drying after massive laundering after container cooling, obtain final product.
Embodiment 3
1g graphene oxide is taken to be distributed in the middle of the 100ml aqueous solution, with the ultrasonic 1h of the ultrasonic device of 1000w power, then plus
Enter a certain amount of nickel sulfate (niso4·6h2O) with hexamethylenetetramine ((ch2)6n4) all it is configured to finite concentration 0.5mol/l,
Magnetic agitation 30min, ultrasonic good uniform solution is poured in ptfe autoclave, airtight good hydro-thermal tank, is heated to 160
DEG C insulation 20h；Take out product, freeze-drying after massive laundering after container cooling, obtain final product.
Embodiment 4
2g graphene oxide is taken to be distributed in the middle of the 100ml aqueous solution, with the ultrasonic 1h of the ultrasonic device of 1000w power, then plus
Enter a certain amount of nickel sulfate (niso4·6h2O) with hexamethylenetetramine ((ch2)6n4) all it is configured to 0.5mol/l, magnetic agitation
30min, ultrasonic good uniform solution is poured in ptfe autoclave, airtight good hydro-thermal tank, is heated to 200 DEG C of insulations
24h；Take out product, massive laundering, rear freeze-drying after container cooling, obtain final product.
Comparative example
0.1g graphene oxide is taken to be distributed in the middle of the 100ml aqueous solution, with the ultrasonic 1h of the ultrasonic device of 1000w power, then
Add a certain amount of nickel sulfate (niso4·6h2O) and NaOH (naoh) is all configured to 0.5mol/l, magnetic agitation 30min,
Ultrasonic good uniform solution is poured in ptfe autoclave, airtight good hydro-thermal tank, it is heated to 180 DEG C of insulation 20h.Wait to hold
Take out product, massive laundering, rear freeze-drying after device cooling, obtain final product.
In the present embodiment preparation process, naoh degree of ionization is high, and direct ionization goes out substantial amounts of oh-, lead to oh-Concentration excessive,
Be combined rapidly with ni, generate substantial amounts of particle diameter distribution heterogeneity and the serious ni of agglomeration (oh)2Particulate, its specific surface area
Little, charge transfer path is long, and chemical property is bad.
The explanation of above example is only intended to help and understands the method for the present invention and its core concept.It should be pointed out that it is right
For those skilled in the art, under the premise without departing from the principles of the invention, the present invention can also be carried out
Some improvement and modification, these improve and modify and also fall in the protection domain of the claims in the present invention.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention.
Multiple modifications to these embodiments will be apparent from for those skilled in the art, as defined herein
General Principle can be realized without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention
It is not intended to be limited to the embodiments shown herein, and be to fit to and principles disclosed herein and features of novelty phase one
The scope the widest causing.
Claims (10)
1. the preparation method of a kind of Graphene/nickel hydroxide composite, comprising:
Graphene oxide, water, hexamethylenetetramine are mixed with nickel source, heating, obtain Graphene/nickel hydroxide after reaction and be combined
Material；Described nickel source is to ionize out ni in water2+Nickel source.
2. preparation method according to claim 1 is it is characterised in that also include after described reaction:
Freeze-drying after the product obtaining is washed.
3. preparation method according to claim 1 and 2 it is characterised in that described heating temperature be 140～200 DEG C, institute
The temperature retention time stating heating is 16～24h.
4. preparation method according to claim 1 and 2 is it is characterised in that in described mixed mixed liquor, described pregnancy
The concentration of urotropine is 0.1～2mol/l, and the concentration of described nickel source is 0.1～2mol/l.
5. preparation method according to claim 1 and 2 is it is characterised in that the ratio of described graphene oxide and described water
For (0.01～2) g:100ml.
6. preparation method according to claim 1 and 2 is it is characterised in that described nickel source is in nickel sulfate and nickel nitrate
One or two.
7. a kind of Graphene/nickel hydroxide composite is it is characterised in that including Graphene and being compound in described graphenic surface
Nickel hydroxide.
8. Graphene according to claim 7/nickel hydroxide composite is it is characterised in that described nickel hydroxide and stone
The mass ratio of black alkene is (3～5): 1.
9. Graphene according to claim 7/nickel hydroxide composite it is characterised in that described nickel hydroxide be α-
ni(oh)2.
10. a kind of electrode material is it is characterised in that described electrode material is the preparation method described in any one of claim 1～6
Graphene/nickel hydroxide composite described in prepared or any one of claim 7～9.
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| CN108878161A (en) * | 2018-06-28 | 2018-11-23 | 陕西科技大学 | Rose-shaped Ni (OH)2/ rGO combination electrode material and its preparation method and application |
| CN108922792A (en) * | 2018-07-13 | 2018-11-30 | 黑龙江省科学院高技术研究院 | A kind of preparation method of graphene/ZnO/NiO composite material |
| CN109142475A (en) * | 2018-07-27 | 2019-01-04 | 哈尔滨理工大学 | Preparation and application without oxydasis nickel redox graphene composite electrode |
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| CN109659516B (en) * | 2018-11-26 | 2021-07-23 | 国宏中晶集团有限公司 | Preparation method of electrode positive electrode material containing graphene |
| CN113371752A (en) * | 2021-05-31 | 2021-09-10 | 江汉大学 | Ni (OH) applied to super capacitor2/KCu7S4Composite electrode material and preparation method thereof |
| CN113371752B (en) * | 2021-05-31 | 2022-11-22 | 江汉大学 | Ni (OH) applied to super capacitor 2 /CuO@Cu 7 S 4 Composite electrode material and preparation method thereof |
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