CN107968191A - Ni(OH)2The preparation method of-carbon nano tube reduction graphene oxide composite material - Google Patents
Ni(OH)2The preparation method of-carbon nano tube reduction graphene oxide composite material Download PDFInfo
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- CN107968191A CN107968191A CN201711148707.7A CN201711148707A CN107968191A CN 107968191 A CN107968191 A CN 107968191A CN 201711148707 A CN201711148707 A CN 201711148707A CN 107968191 A CN107968191 A CN 107968191A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/24—Alkaline accumulators
- H01M10/30—Nickel accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses Ni (OH)2The preparation method of carbon nano tube reduction graphene oxide composite material, it is characterised in that：Specifically include following steps：Step S1：Prepare GO/CNTs mixed solutions；Step S2：Specifically refer to：According to mass ratio GO:Ni(OH)2=1：8 weigh a certain amount of nickel nitrate (Ni (NO3)2·6H2O) it is dissolved in 10mL deionized waters, which is slowly dropped in above-mentioned GO/CNTs mixed solutions, stirs 3 4h；Step S3：Hydro-thermal reaction；Step S4：Vacuum drying, obtains Ni (OH)2CNTs/RGO composite materials.The beneficial effects of the invention are as follows：Material prepared by the present invention has height ratio capacity and the electrode material of good circulation stability, and the optimization preparation for nickel radical battery high-performance, inexpensive electrode material provides facility.
Description
Technical field
The present invention relates to technical field of graphene, is Ni (OH) specifically2- carbon nano tube reduction graphene oxide is answered
The preparation method of condensation material.
Background technology
Ni(OH)2It is a kind of P-type semiconductor, improves Ni (OH)2One of effective ways of structural stability and electric conductivity be to
Wherein add carbon material.As the carbon nanotubes (CNTs) and graphene since the advent of the world of carbon material, due to its excellent chemistry
The very big concern of researcher is caused with physical property.CNTs is a kind of one-dimensional material with special construction, unique structure
Assign its excellent physicochemical characteristics.
Graphene is a kind of two-dimentional new carbon, is the monoatomic layer that carbon atom is formed by connecting by sp2 hydridization, its is basic
Structure is a kind of benzene six-membered ring structure of stabilization, and stable regular hexagon structure ensure that itself highly stable property.Therefore
Ni (OH) 2 is compound with CNTs, graphene, obtained Ni (OH)2- CNTs/ graphene composite structures can maintain electrode steady
It is qualitative, so as to improve its cycle performance, with the compound electric conductivity that can also significantly improve electrode material of carbon-based material, lift it
High rate performance.
Graphene/SWCNTs/Ni (OH) is prepared for using chemical precipitation method2Composite material, have studied graphene and CNTs
Different quality compare the influence of composite structure and performance, it is used for ultracapacitor and shows good cycle performance.
Nickel aluminium layered double-hydroxide/graphene/CNTs composite materials are synthesized by the hot method of alcohol solvent, its structure has
Beneficial to the chemical property for improving electrode material, high specific capacitance (5mA/cm is possessed as electrode material2When 1562F/g), it is excellent
Good high rate performance and cyclical stability.
Carbon nanotubes-α-Ni (OH) are prepared for by hydro-thermal method2/ graphene composite material, the electricity as ultracapacitor
Pole material, in the case where current density is 15A/g, specific capacity remains to reach 1008F/g after 1000 circulations.Prepared by CVD method
Contain Ni (OH)2Nanometer sheet, CNTs, the composite material of graphene, when current density is 10A/g, by 500 times circulation after its
Specific capacitance remains to holding 80%, is demonstrated by high capacity retention ratio.
The content of the invention
It is an object of the invention to provide Ni (OH)2The preparation method of-carbon nano tube reduction graphene oxide composite material,
The present invention effectively increases the electric conductivity of electrode material using the effect of the collaboration of CNTs and RGO, and particularly CNTs prevents graphite
Alkene lamella it is overlapping, the structure of electrode material is stabilized in charge and discharge process, outstanding high rate performance is shown and circulation is steady
It is qualitative.
CNTs is as flexible support material, it is suppressed that volumetric expansion of the electrode material in charge and discharge process, is quickly filling
Be conducive to the diffusion of electrolyte ion in electric discharge, be conducive to increase the contact surface area of electrolyte and active material, so that electric
Pole material has higher specific discharge capacity and preferable stability.
Material prepared by the present invention has height ratio capacity and the electrode material of good circulation stability, is that nickel radical battery is high
Prepared by the optimization of performance, inexpensive electrode material provides facility.
Ni(OH)2The preparation method of-carbon nano tube reduction graphene oxide composite material, specifically includes following steps：
Step S1：Prepare GO/CNTs mixed solutions；
Step S2：Specifically refer to：According to mass ratio GO:Ni(OH)2=1：8 weigh a certain amount of nickel nitrate (Ni (NO3)2·
6H2O) it is dissolved in 10mL deionized waters, which is slowly dropped in above-mentioned GO/CNTs mixed solutions, stirs 3-4h；
Step S3：Hydro-thermal reaction；
Step S4：Vacuum drying, obtains Ni (OH)2- CNTs/RGO composite materials.
Further, in order to preferably realize the present invention, the step S1 is specifically referred to：Weigh what 100mg had been prepared
GO and 30mgCNTs is dissolved in 100mL deionized waters, and stirring is ultrasonically treated 4-8h, and it is molten to obtain well dispersed GO/CNTs mixing
Liquid；
Further, in order to preferably realize the present invention, the step S3 is specifically referred to：By a certain amount of NaOH aqueous solutions
Add in above-mentioned solution and add 0.5mL hydrazine hydrates after stirring 2h, stir 0.5-1h；Solution is then moved into polytetrafluoroethylene (PTFE)
In the reaction kettle of liner, hydro-thermal reaction is carried out in thermostatic drying chamber；
Further, in order to preferably realize the present invention, the step S4 is specifically referred to；After question response, stand
24h, then filtered, washed repeatedly for several times with deionized water and absolute ethyl alcohol, be then dried in vacuo 12-24h at 80 DEG C, obtain
To Ni (OH)2- CNTs/RGO composite materials.
Ni(OH)2- carbon nano tube reduction graphene oxide composite material, includes the raw material of following components by weight percent：Graphite powder
50-100 parts, 5-16 parts of the concentrated sulfuric acid, KMnO43-5 parts, NaNO32-4 parts, H2O270-90 parts, 5-20 parts of carbon nanotubes, nickel nitrate
(Ni(NO3)2·6H2O) 12-15 parts, NaOH0.3-0.8 parts, 2-6 parts of 1-3 parts of hydrazine hydrate, absolute ethyl alcohol parts.
Further, in order to preferably realize the present invention, the particle diameter of the graphite powder is 30-40 μm.
Further, in order to preferably realize the present invention, the concentration of the concentrated sulfuric acid is more than 98%.
Further, in order to preferably realize the present invention, the thickness of the nickel foam is 1mm, surface density 320g/cm2、
Porosity is 95%.
Further, in order to preferably realize the present invention, the outside diameter of the carbon nanotubes is 30~50nm, length for 10~
20 μm of multi-walled carbon nanotube or single-walled carbon nanotube.
Compared with prior art, the present invention haing the following advantages and beneficial effect：
The present invention effectively increases the electric conductivity of electrode material, particularly CNTs using the effect of the collaboration of CNTs and RGO
The overlapping of graphene sheet layer is prevented, the structure of electrode material is stabilized in charge and discharge process, shows outstanding high rate performance
And cyclical stability.
CNTs is as flexible support material, it is suppressed that volumetric expansion of the electrode material in charge and discharge process, is quickly filling
Be conducive to the diffusion of electrolyte ion in electric discharge, be conducive to increase the contact surface area of electrolyte and active material, so that electric
Pole material has higher specific discharge capacity and preferable stability.
Embodiment
The present invention is described in further detail with reference to embodiment, but the implementation of the present invention is not limited to this.
Embodiment 1：
The present invention is achieved through the following technical solutions, Ni (OH)2- carbon nano tube reduction graphene oxide composite material, bag
Include the raw material of following components by weight percent：50-100 parts of graphite powder, 5-16 parts of the concentrated sulfuric acid, KMnO43-5 parts, NaNO32-4 parts, H2O270-
90 parts, 5-20 parts of carbon nanotubes, nickel nitrate (Ni (NO3)2·6H2O) 12-15 parts, NaOH0.3-0.8 parts, 1-3 parts of hydrazine hydrate,
2-6 parts of absolute ethyl alcohol.
It should be noted that by above-mentioned improvement, CNTs prevents the overlapping of graphene sheet layer, stablizes in charge and discharge process
The structure of electrode material, shows outstanding high rate performance and cyclical stability.
CNTs is as flexible support material, it is suppressed that volumetric expansion of the electrode material in charge and discharge process, is quickly filling
Be conducive to the diffusion of electrolyte ion in electric discharge, be conducive to increase the contact surface area of electrolyte and active material, so that electric
Pole material has higher specific discharge capacity and preferable stability.
Material prepared by the present invention has height ratio capacity and the electrode material of good circulation stability, is that nickel radical battery is high
Prepared by the optimization of performance, inexpensive electrode material provides facility.
The other parts of the present embodiment are same as the previously described embodiments, and so it will not be repeated.
Embodiment 2：
The present embodiment does further optimization on the basis of above-described embodiment, further, in order to preferably realize this hair
Bright, the particle diameter of the graphite powder is 30-40 μm.
Further, in order to preferably realize the present invention, the concentration of the concentrated sulfuric acid is more than 98%.
In order to preferably realize the present invention, the thickness of the nickel foam is 1mm, surface density 320g/cm2, porosity are
95%.
Further, in order to preferably realize the present invention, the outside diameter of the carbon nanotubes is 30~50nm, length for 10~
20 μm of multi-walled carbon nanotube or single-walled carbon nanotube.
It should be noted that by above-mentioned improvement,
The other parts of the present embodiment are same as the previously described embodiments, and so it will not be repeated.
Embodiment 3：
The present embodiment does further optimization on the basis of above-described embodiment, by the sample obtained by embodiment 1- embodiments 2
Product are tested；Active material, conductive agent acetylene black and binding agent PTFE emulsion in mass ratio 85:10:5 fill in agate mortar
Divide mixing, then paste is tuned into absolute ethyl alcohol, be uniformly applied in the nickel foam of area 10mm × 10mm, smear quality
In the range of 2mg~4mg, vacuum drying (60 DEG C) 3h removes the moisture in electrode, pushes flakiness in 10MPa pressure, and count
The quality for the active material that each nickel foam on piece is smeared is calculated, as subsequent electrochemical performance test when is used.Chemical property
Test uses three-electrode system, the platinum plate electrode of auxiliary electrode 10mm × 10mm, and reference electrode is saturated calomel electrode (SCE),
Electrolyte is 6mol/LKOH solution.Cyclic voltammetric (CV) and electrochemical AC impedance (EIS) test, CV tests are carried out to material
Scanning voltage scope is 0.1-0.7V, and EIS test frequencies scope is 0.01-100000Hz.Constant current charge-discharge is carried out to material
Test.
As hydrothermal temperature raises, the diffraction peak intensity increase of Ni (OH) 2-CNTs/RGO composite materials, works as temperature
During rise, favourable condition is provided for the nucleating growth of crystal grain, the size of crystal grain can increase with the rise of reaction temperature.
With relatively low crystallinity and less lattice rigidity, the crystallite dimension of generation is smaller, is conducive to the diffusion of electrolyte ion
And infiltration.
Therefore：By test of many times, hydrothermal temperature is 120 DEG C, the sample of 150 DEG C, 180 DEG C preparations is respectively labeled as
NCR-120、NCR-150、NCR-180.When without CNTs, Ni (OH) is prepared with above-mentioned same method2/ RGO, without GO and
During CNTs, Ni (OH) is prepared2, NR-120 and N-120 are respectively labeled as, (1) uses differential responses temperature, passes through a simple step
Hydro-thermal method is prepared for nickel hydroxide/carbon nano tube/redox graphene (Ni (OH)2- CNTs/RGO) composite material.
When hydrothermal temperature is 120 DEG C, the Ni (OH) in prepared composite material2For hexagonal β-Ni (OH)2Nanometer
Piece, it is dispersed in RGO sheet surfaces with CNTs, effectively prevents the reunion of RGO, and forms three-dimensional net structure.
When hydrothermal temperature is 120 DEG C, Ni (OH)2Specific discharge capacity is most in 0.2C for-CNTs/RGO electrode materials
Greatly 362.8mAh/g, far above Ni (OH)2、Ni(OH)2The specific discharge capacity of/RGO, specific discharge capacity is 286.2mAh/ during 5C
G, still greater than Ni (OH)2Specific discharge capacity in 0.2C, shows good high rate performance, illustrates the collaboration of CNTs and RGO
Effect effectively increase the electric conductivity of electrode material, particularly CNTs prevents the overlapping of graphene sheet layer, in charge and discharge process
In stabilize the structure of electrode material, show outstanding high rate performance and cyclical stability.
The other parts of the present embodiment are same as the previously described embodiments, and so it will not be repeated.
Embodiment 4：
The present embodiment is further optimization, Ni (OH) on the basis of above-described embodiment2- carbon nano tube reduction graphite oxide
The preparation method of alkene composite material, specifically includes following steps：
Step S1：Prepare GO/CNTs mixed solutions；Specifically refer to：Weigh GO that 100mg prepared and 30mgCNTs is molten
In 100mL deionized waters, stirring is ultrasonically treated 4-8h, obtains well dispersed GO/CNTs mixed solutions；
Step S2：Specifically refer to：According to mass ratio GO:Ni(OH)2=1：8 weigh a certain amount of nickel nitrate (Ni (NO3)2·
6H2O) it is dissolved in 10mL deionized waters, which is slowly dropped in above-mentioned GO/CNTs mixed solutions, stirs 3-4h；
Step S3：Hydro-thermal reaction；Specifically refer to：After adding in above-mentioned solution by a certain amount of NaOH aqueous solutions and stir 2h
0.5mL hydrazine hydrates are added, stir 0.5-1h；Then solution is moved in the reaction kettle of polytetrafluoroethyllining lining, done in constant temperature
Hydro-thermal reaction is carried out in dry case；
Step S4：Vacuum drying, obtains Ni (OH)2- CNTs/RGO composite materials.Specifically refer to；It is quiet after question response
24h is put, then is filtered, is washed repeatedly for several times with deionized water and absolute ethyl alcohol, is then dried in vacuo 12-24h at 80 DEG C,
Obtain Ni (OH)2- CNTs/RGO composite materials.
The other parts of the present embodiment are same as the previously described embodiments, and so it will not be repeated.
The above, is only presently preferred embodiments of the present invention, not does limitation in any form to the present invention, it is every according to
Any simply modification, the equivalent variations made according to the technical spirit of the present invention to above example, each fall within the protection of the present invention
Within the scope of.
Claims (4)
1.Ni(OH)2The preparation method of-carbon nano tube reduction graphene oxide composite material, it is characterised in that：Specifically include following
Step：
Step S1：Prepare GO/CNTs mixed solutions；
Step S2：Specifically refer to：According to mass ratio GO:Ni(OH)2=1：8 weigh a certain amount of nickel nitrate (Ni (NO3)2·6H2O)
It is dissolved in 10mL deionized waters, which is slowly dropped in above-mentioned GO/CNTs mixed solutions, stirs 3-4h；
Step S3：Hydro-thermal reaction；
Step S4：Vacuum drying, obtains Ni (OH)2- CNTs/RGO composite materials.
2. Ni (OH) according to claim 62The preparation method of-carbon nano tube reduction graphene oxide composite material, it is special
Sign is：The step S1 is specifically referred to：Weigh GO that 100mg prepared and 30mgCNTs be dissolved in 100mL deionized waters,
Stirring is ultrasonically treated 4-8h, obtains well dispersed GO/CNTs mixed solutions.
3. Ni (OH) according to claim 62The preparation method of-carbon nano tube reduction graphene oxide composite material, it is special
Sign is：The step S3 is specifically referred to：A certain amount of NaOH aqueous solutions are added in above-mentioned solution and are added after stirring 2h
0.5mL hydrazine hydrates, stir 0.5-1h；Then solution is moved in the reaction kettle of polytetrafluoroethyllining lining, in thermostatic drying chamber
Middle carry out hydro-thermal reaction.
4. Ni (OH) according to claim 62The preparation method of-carbon nano tube reduction graphene oxide composite material, it is special
Sign is：The step S4 is specifically referred to；After question response, 24h is stood, then is filtered, with deionized water and anhydrous second
Alcohol washs for several times repeatedly, is then dried in vacuo 12-24h at 80 DEG C, obtains Ni (OH)2- CNTs/RGO composite materials.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113488639A (en) * | 2021-07-01 | 2021-10-08 | 肇庆市华师大光电产业研究院 | Preparation method of high-sulfur-content lithium-sulfur battery positive electrode material |
| CN114105224A (en) * | 2021-11-23 | 2022-03-01 | 黑龙江工程学院 | Preparation method and application of nickel hydroxide/carbon nano tube composite nanosheet |
| CN114695854A (en) * | 2022-03-23 | 2022-07-01 | 西安建筑科技大学 | CNTs-SnS-SnS2@ GO heterostructure composite material and preparation method and application thereof |
-
2017
- 2017-11-17 CN CN201711148707.7A patent/CN107968191A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113488639A (en) * | 2021-07-01 | 2021-10-08 | 肇庆市华师大光电产业研究院 | Preparation method of high-sulfur-content lithium-sulfur battery positive electrode material |
| CN113488639B (en) * | 2021-07-01 | 2022-08-26 | 肇庆市华师大光电产业研究院 | Preparation method of high-sulfur-content lithium-sulfur battery positive electrode material |
| CN114105224A (en) * | 2021-11-23 | 2022-03-01 | 黑龙江工程学院 | Preparation method and application of nickel hydroxide/carbon nano tube composite nanosheet |
| CN114695854A (en) * | 2022-03-23 | 2022-07-01 | 西安建筑科技大学 | CNTs-SnS-SnS2@ GO heterostructure composite material and preparation method and application thereof |
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