CN106783232B - A kind of NiO/NiCo2O4The preparation method of/three-dimensional nitrogen-doped graphene combination electrode material - Google Patents
A kind of NiO/NiCo2O4The preparation method of/three-dimensional nitrogen-doped graphene combination electrode material Download PDFInfo
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Abstract
The present invention provides a kind of NiO/NiCo2O4The preparation method of/three-dimensional nitrogen-doped graphene combination electrode material, includes the following steps：Cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate, hexa and graphene oxide are placed in ultrasonic disperse in water/acetone mixture by step 1, obtain mixed liquor A；Mixed liquor A is transferred to progress incubation water heating reaction in polytetrafluoroethylene (PTFE) water heating kettle by step 2, obtains mixed liquor precursor B after completion of the reaction；Mixed liquor precursor B is filtered, is washed, is dry by step 3, obtains product C；Presoma C is put into microwave reactor by step 4, and microwave heating reaction is carried out under the conditions of power 950W, obtains reaction product NiO/NiCo2O4/ three-dimensional nitrogen-doped graphene combination electrode material.This method has many advantages, such as low reaction cost, technique and simple flow.
Description
Technical field
The present invention relates to the graphene-based field of compound material that ultracapacitor utilizes, and refer in particular to a kind of NiO/NiCo2O4/ tri-
Tie up the preparation method of nitrogen-doped graphene combination electrode material.
Background technology
Since graphene is found, it has been constantly subjected to doting on for scientific researcher, is known as " the strategic material of 21 century ".Stone
Black alkene has huge specific surface area, thermal stability and chemical stability and outstanding leads as two-dimensional layer carbon-based material
Electrical property, therefore have splendid application potential in ultracapacitor field as basis material.However the practical appearance of graphene
It measures and is less than theoretical capacity, and it is very fast to decay, be easy to occur stacking and agglomeration again between lamella, cause it that should have
Standby superior chemical property is difficult to accomplished.N atoms due to have with the approximate atomic radius of C atoms, can be used as electricity
Sub- donor is doped graphene in a manner of replacing, and introducing the hetero atoms such as N in graphene film interlayer can be effectively by stone
Black alkene is transformed into semiconductor from the semimetal of zero band gap, and the graphene for forming n-type or p-doping shows purer graphene more
Mostly excellent performance.(the .Nat.Mater.2011,10,209 such as Meyer J C, Kurasch S；Wu L,Feng H,Liu M,
Equal Nanoscale, 2013,5 (22):10839.) introducing of nitrogen improves graphene surface structure and increases the same of conductive capability
When also cause planar structure defect on the surface of graphene, be conducive to the insertion of external nano-particle, it is mutual to reduce graphene
It stacks.
The NiCo of spinel-type2O4As the electrode material of ultracapacitor, the specific capacitance value, forthright again of superelevation is shown
Energy and good corrosion resistance, by the growing interest of researcher.Ni3+/Ni2+And Co3+/Co2+Ability of the electricity to conversion charge
It is very strong, it, can be by electricity to electronics caused by transmission when redox reaction occurs.Also there is transition metal institute simultaneously
The characteristic having so that NiCo2O4With higher conductivity, simultaneously simultaneously for the diffusional resistance very little of proton and cation
With good electrolyte osmosis ability, Conductivity Ratio single NiO and Co3O4Want the high 1-2 order of magnitude.Due to crystal face knot
The similitude of structure is more conducive to form the nickel oxide nano-crystal of small particle in cobalt acid nickel plane of crystal.By NiO/NiCo2O4With graphite
Olefinic base material progress is compound to make NiO nano-particles growth in situ on cobalt acid nanosized nickel rods, then is interspersed in graphene sheet layer together
Between, ternary contact-type composite material is formed, effectively avoids stacking again between graphene, makes NiO/NiCo2O4High capacitance and stone
The bigger serface advantage of black alkene material be combined with each other, and greatly improves the performance of composite material.The present invention is with six hydration nitre
Sour cobalt, Nickelous nitrate hexahydrate, graphene oxide and hexa are raw material, and NiO/ is prepared by hydro-thermal method-microwave method
NiCo2O4/ three-dimensional nitrogen-doped graphene composite Nano super capacitor material.Utilize NiO, NiCo2O4With nitrogen-doped graphene
Existing synergistic effect is so that NiO, NiCo between three2O4Fake capacitance property and nitrogen-doped graphene electric double layer electricity
Capacitive matter is fully played, and electrochemistry is greatly enhanced.
Invention content
The object of the present invention is to provide it is a kind of it is easy to operate, there is NiO/NiCo2O4/ it is three-dimensional that nitrogen-doped graphene is compound receives
The preparation method of rice material, in current density 1A g-1Under the conditions of, the capacitance of composite material is prepared up to 1971.6F g-1。
The present invention is achieved through the following technical solutions：
A kind of NiO/NiCo2O4The preparation method of/three-dimensional nitrogen-doped graphene combination electrode material, includes the following steps：
Cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate, hexa and graphene oxide are placed in water/acetone by step 1
Ultrasonic disperse in mixed liquor, obtains mixed liquor A；
Mixed liquor A is transferred to progress incubation water heating reaction in polytetrafluoroethylene (PTFE) water heating kettle by step 2, after completion of the reaction
To mixed liquor precursor B；
Mixed liquor precursor B is filtered, is washed, is dry by step 3, obtains product C；
Presoma C is put into microwave reactor by step 4, and microwave heating reaction is carried out under the conditions of power 950W, is obtained
Reaction product NiO/NiCo2O4/ three-dimensional nitrogen-doped graphene combination electrode material.
In step 1, the cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate, hexa, graphene oxide, water/acetone
The amount ratio of mixed liquor is 0.015mol：0.015mol：0.03~0.04mol：80mg：300mL.
In step 1, in the water/acetone mixture, the volume ratio of used water and acetone is 2：1.
In step 2, the temperature of the constant temperature thermal response is 180 DEG C~200 DEG C, reaction time 48h.
In step 4, the microwave reaction temperature is 700 DEG C~900 DEG C, and the reaction time is 15~20min.
In step 1, when preparing solution A, used hexa is as alkali source, nitrogen source and sedimentation agent.
Advantageous effect：
The NiO/NiCo prepared with the method2O4/ three-dimensional nitrogen-doped graphene combination electrode material, grain size is less than 5nm's
NiO is nanocrystalline to be dispersed in NiCo2O4The surface of nanometer sheet, NiCo2O4Surface texture is loose, with three-dimensional nitrogen-doped graphene
It is tightly combined, prepares the capacitance of composite material up to 1971.6F g-1.This method has low reaction cost, technique and simple flow
The advantages that.
Description of the drawings
Fig. 1 is NiO/NiCo2O4The XRD diffraction spectrograms of/three-dimensional nitrogen-doped graphene, diffraction maximum is graphene, oxygen in figure
Change the characteristic diffraction peak of nickel and cobalt acid nickel.
Fig. 2 is NiO/NiCo2O4/ three-dimensional nitrogen-doped graphene transmission electron microscope photo.
Fig. 3 is NiCo2O4, NiCo2O4/ graphene oxide, NiO/NiCo2O4/ three-dimensional nitrogen-doped graphene is in 1A g-1Condition
Under constant current charge-discharge curve graph.
Fig. 4 is NiO/NiCo2O4The constant current charge-discharge curve graph of/three-dimensional nitrogen-doped graphene under different current densities.
Specific implementation mode
With reference to specific implementation example, the present invention will be further described.
Embodiment 1
Weigh 80mg graphene oxides, 4.3660g Co (NO3)2·6H2O(0.015mol)、4.3770g Ni(NO3)2·
6H2O (0.015mol), 4.2059g hexamethylenetetramines (0.03mol) ultrasonic disperse are mixed in 300ml deionized waters and acetone
In liquid (deionized water 200ml, acetone 100ml), mixed solution is transferred in water heating kettle by ultrasonic disperse 1h, 180 DEG C of reactions
48h.Cooled to room temperature after the completion of reaction, absolute ethyl alcohol and deionized water alternating centrifugal wash ten times, then dry in vacuum
36 hours are dried to get cobalt nickel presoma/nitrogen-doped graphene in 60 DEG C in dry case.By cobalt nickel presoma/nitrogen-doped graphene
It is put into microwave reactor, product NiO/NiCo is obtained in power 950W, 700 DEG C of microwave reaction 15min of temperature2O4/ three-dimensional nitrogen is mixed
Miscellaneous graphene, sample are 18.9 °, 31.1 °, 36.7 °, 38.4 °, 44.5 °, 55.3 °, 59.2 ° and 65.0 ° in 2 θ and X occur
The diffraction maximum of ray, difference can be with NiCo2O4(111) of crystal, (220), (311), (222), (400), (422),
(511), (440) crystal face and with NiO (111), (200), (220), (222) respectively it is corresponding with 37.25 °, 43.28 °,
62.86 ° and 79.39 ° corresponding with standard spectrum, such as Fig. 1.Three-dimensional nitrogen-doped graphene has larger specific surface, the doping of nitrogen
Carbon atom adjacent thereto is had activated, the quantity of active site is increased, is conducive to electrolyte ion and occurs instead with active material
It answers.And the NiCo of loose sheet2O4The load for being conducive to small particle NiO substantially increases the fake capacitance of composite material, such as
Fig. 2.The cobalt acid nickel nano material of above-mentioned preparation is subjected to charge-discharge test, current density is 1A g-1When, specific capacity value reaches
1951.2F g-1；Specific capacity remains at 81% or more after 5000 charge-discharge tests.
Embodiment 2
Weigh 80mg graphene oxides, 4.3660g Co (NO3)2·6H2O(0.015mol)、4.3770g Ni(NO3)2·
6H2O (0.015mol), 5.608g hexamethylenetetramines (0.04mol) ultrasonic disperse are mixed in 300ml deionized waters and acetone
In liquid (deionized water 200ml, acetone 100ml), mixed solution is transferred in water heating kettle by ultrasonic disperse 1h, 190 DEG C of reactions
48h.Cooled to room temperature after the completion of reaction, absolute ethyl alcohol and deionized water alternating centrifugal wash ten times, then dry in vacuum
36 hours are dried to get cobalt nickel presoma/nitrogen-doped graphene in 60 DEG C in dry case.By cobalt nickel presoma/nitrogen-doped graphene
It is put into microwave reactor, product NiO/NiCo is obtained in power 950W, 750 DEG C of microwave reaction 18min of temperature2O4/ three-dimensional nitrogen is mixed
There is larger specific surface, the doping of nitrogen to have activated carbon atom adjacent thereto for miscellaneous graphene, three-dimensional nitrogen-doped graphene, increase
The quantity of active site, is conducive to electrolyte ion and reacts with active material.And the NiCo of loose sheet2O4Have
Conducive to the load of small particle NiO, the fake capacitance of composite material is substantially increased.By the cobalt acid nickel nano material of above-mentioned preparation into
Row charge-discharge test, current density are 1A g-1When, specific capacity value has reached 1921.4F g-1, such as Fig. 3, it is more than NiCo2O4
(1000F g-1) and NiCo2O4/ graphene (1675F g-1)；Specific capacity remains at after 5000 charge-discharge tests
83% or more.
Embodiment 3
Weigh 80mg graphene oxides, 4.3660g Co (NO3)2·6H2O(0.015mol)、4.3770g Ni(NO3)2·
6H2O (0.015mol), 4.907g hexamethylenetetramines (0.035mol) ultrasonic disperse are mixed in 300ml deionized waters and acetone
In liquid (deionized water 200ml, acetone 100ml), mixed solution is transferred in water heating kettle by ultrasonic disperse 1h, 190 DEG C of reactions
48h.Cooled to room temperature after the completion of reaction, absolute ethyl alcohol and deionized water alternating centrifugal wash ten times, then dry in vacuum
36 hours are dried to get cobalt nickel presoma/nitrogen-doped graphene in 60 DEG C in dry case.By cobalt nickel presoma/nitrogen-doped graphene
It is put into microwave reactor, product NiO/NiCo is obtained in power 950W, 800 DEG C of microwave reaction 18min of temperature2O4/ three-dimensional nitrogen is mixed
There is larger specific surface, the doping of nitrogen to have activated carbon atom adjacent thereto for miscellaneous graphene, three-dimensional nitrogen-doped graphene, increase
The quantity of active site, is conducive to electrolyte ion and reacts with active material.And the NiCo of loose sheet2O4Have
Conducive to the load of small particle NiO, the fake capacitance of composite material is substantially increased.By the cobalt acid nickel nano material of above-mentioned preparation into
Row charge-discharge test, current density are 1A g-1When, specific capacity value has reached 1940.4F g-1；By 2000 charge-discharge tests
Specific capacity remains at 83% or more later.
Embodiment 4
Weigh 80mg graphene oxides, 4.3660g Co (NO3)2·6H2O(0.015mol)、4.3770g Ni(NO3)2·
6H2O (0.015mol), 4.2059g hexamethylenetetramines (0.03mol) ultrasonic disperse are mixed in 300ml deionized waters and acetone
In liquid (deionized water 200ml, acetone 100ml), mixed solution is transferred in water heating kettle by ultrasonic disperse 1h, 200 DEG C of reactions
48h.Cooled to room temperature after the completion of reaction, absolute ethyl alcohol and deionized water alternating centrifugal wash ten times, then dry in vacuum
36 hours are dried to get cobalt nickel presoma/nitrogen-doped graphene in 60 DEG C in dry case.By cobalt nickel presoma/nitrogen-doped graphene
It is put into microwave reactor, product NiO/NiCo is obtained in power 950W, 850 DEG C of microwave reaction 20min of temperature2O4/ three-dimensional nitrogen is mixed
There is larger specific surface, the doping of nitrogen to have activated carbon atom adjacent thereto for miscellaneous graphene, three-dimensional nitrogen-doped graphene, increase
The quantity of active site, is conducive to electrolyte ion and reacts with active material.And the NiCo of loose sheet2O4Have
Conducive to the load of small particle NiO, the fake capacitance of composite material is substantially increased.By the cobalt acid nickel nano material of above-mentioned preparation into
Row charge-discharge test, current density are 1A g-1When, specific capacity value has reached 1971.6F g-1；By 5000 charge-discharge tests
Specific capacity remains at 85% or more later.Such as Fig. 4, when current density is 1Ag-1、2A·g-1、4A·g-1And 10Ag-1
When, measured specific capacitance value is respectively 1971.6Fg-1、1870.9F·g-1、1769.8F·g-1And 1675.9Fg-1.It can
Work as current density from 1Ag can be clearly seen-1Increase to 10Ag-1When, the specific capacitance value of electric discharge can keep initial value
76%.Its higher specific capacitance value mainly due to prepared three-dimensional nitrogen-doped graphene uniqueness nanostructure, has higher
Specific surface can increase the number of its active site, while loose cobalt acid nickel surface has a large amount of nickel oxide nano-crystal, is conducive to
Electrolyte ion reacts with active material.
Embodiment 5
Weigh 80mg graphene oxides, 4.3660g Co (NO3)2·6H2O(0.015mol)、4.3770g Ni(NO3)2·
6H2O (0.015mol), 5.608g hexamethylenetetramines (0.04mol) ultrasonic disperse are mixed in 300ml deionized waters and acetone
In liquid (deionized water 200ml, acetone 100ml), mixed solution is transferred in water heating kettle by ultrasonic disperse 1h, 200 DEG C of reactions
48h.Cooled to room temperature after the completion of reaction, absolute ethyl alcohol and deionized water alternating centrifugal wash ten times, then dry in vacuum
36 hours are dried to get cobalt nickel presoma/nitrogen-doped graphene in 60 DEG C in dry case.By cobalt nickel presoma/nitrogen-doped graphene
It is put into microwave reactor, product NiO/NiCo is obtained in power 950W, 900 DEG C of microwave reaction 18min of temperature2O4/ three-dimensional nitrogen is mixed
There is larger specific surface, the doping of nitrogen to have activated carbon atom adjacent thereto for miscellaneous graphene, three-dimensional nitrogen-doped graphene, increase
The quantity of active site, is conducive to electrolyte ion and reacts with active material.And the NiCo of loose sheet2O4Have
Conducive to the load of small particle NiO, the fake capacitance of composite material is substantially increased.By the cobalt acid nickel nano material of above-mentioned preparation into
Row charge-discharge test, current density are 1A g-1When, specific capacity value has reached 1948.9F g-1；By 5000 charge-discharge tests
Specific capacity remains at 85% or more later.
Embodiment 6
Weigh 80mg graphene oxides, 4.3660g Co (NO3)2·6H2O(0.015mol)、4.3770g Ni(NO3)2·
6H2O (0.015mol), 5.608g hexamethylenetetramines (0.04mol) ultrasonic disperse are mixed in 300ml deionized waters and acetone
In liquid (deionized water 200ml, acetone 100ml), mixed solution is transferred in water heating kettle by ultrasonic disperse 1h, 200 DEG C of reactions
48h.Cooled to room temperature after the completion of reaction, absolute ethyl alcohol and deionized water alternating centrifugal wash ten times, then dry in vacuum
36 hours are dried to get cobalt nickel presoma/nitrogen-doped graphene in 60 DEG C in dry case.By cobalt nickel presoma/nitrogen-doped graphene
It is put into microwave reactor, product NiO/NiCo is obtained in power 950W, 900 DEG C of microwave reaction 18min of temperature2O4/ three-dimensional nitrogen is mixed
There is larger specific surface, the doping of nitrogen to have activated carbon atom adjacent thereto for miscellaneous graphene, three-dimensional nitrogen-doped graphene, increase
The quantity of active site, is conducive to electrolyte ion and reacts with active material.And the NiCo of loose sheet2O4Have
Conducive to the load of small particle NiO, the fake capacitance of composite material is substantially increased.By the cobalt acid nickel nano material of above-mentioned preparation into
Row charge-discharge test, current density are 1A g-1When, specific capacity value has reached 1993.7F g-1；By 5000 charge-discharge tests
Specific capacity remains at 88% or more later.
Claims (4)
1. a kind of NiO/NiCo2O4The preparation method of/three-dimensional nitrogen-doped graphene combination electrode material, which is characterized in that including such as
Lower step：
Cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate, hexa and graphene oxide are placed in water/acetone mixing by step 1
Ultrasonic disperse in liquid, obtains mixed liquor A；The cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate, hexa, graphite oxide
Alkene, water/acetone mixture amount ratio be 0.015mol：0.015mol：0.03~0.04mol：80mg：300mL；
Mixed liquor A is transferred to progress incubation water heating reaction in polytetrafluoroethylene (PTFE) water heating kettle by step 2, is mixed after completion of the reaction
Close liquid precursor B；
Mixed liquor precursor B is filtered, is washed, is dry by step 3, obtains product C；Presoma C is put into microwave reaction by step 4
In device, microwave heating reaction is carried out under the conditions of power 950W, obtains reaction product NiO/NiCo2O4/ three-dimensional nitrogen-doped graphene
Combination electrode material.
2. a kind of NiO/NiCo according to claim 12O4The preparation side of/three-dimensional nitrogen-doped graphene combination electrode material
Method, which is characterized in that in step 1, in the water/acetone mixture, the volume ratio of used water and acetone is 2：1.
3. a kind of NiO/NiCo according to claim 12O4The preparation side of/three-dimensional nitrogen-doped graphene combination electrode material
Method, which is characterized in that in step 2, the temperature of the incubation water heating reaction is 180 DEG C ~ 200 DEG C, reaction time 48h.
4. a kind of NiO/NiCo according to claim 12O4The preparation side of/three-dimensional nitrogen-doped graphene combination electrode material
Method, which is characterized in that in step 4, the temperature of the microwave heating reaction is 700 DEG C ~ 900 DEG C, and the reaction time is 15 ~ 20min.
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| CN107680831B (en) * | 2017-08-23 | 2019-06-28 | 江苏大学 | A kind of hollow corn shape Co3O4@NiCo2O4The preparation method of/nitrogen-doped graphene flexible electrode material |
| CN108615614A (en) * | 2018-05-25 | 2018-10-02 | 重庆大学 | A kind of N doping TiO2/ MXene composite material and preparation methods and application |
| CN109637830A (en) * | 2018-12-28 | 2019-04-16 | 哈尔滨理工大学 | A kind of preparation method of NiO/ graphene composite nano plate electrode material |
| CN111298822B (en) * | 2020-02-14 | 2022-06-10 | 江苏师范大学 | Nitrogen/sulfur doped carbon coated NiCo2O4Synthetic method of/NiO hollow micron rod |
| CN111250094B (en) * | 2020-03-24 | 2022-06-14 | 辽宁大学 | Double Z type Co3O4/NiCo2O4/NiO photocatalyst and preparation method and application thereof |
| CN114360923B (en) * | 2022-01-18 | 2023-05-30 | 贵州师范学院 | Preparation method of nickel oxide composite electrode material |
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