CN106299271A - A kind of nano nickel cobalt oxide/graphene composite material and preparation method thereof - Google Patents
A kind of nano nickel cobalt oxide/graphene composite material and preparation method thereof Download PDFInfo
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- CN106299271A CN106299271A CN201610706998.6A CN201610706998A CN106299271A CN 106299271 A CN106299271 A CN 106299271A CN 201610706998 A CN201610706998 A CN 201610706998A CN 106299271 A CN106299271 A CN 106299271A
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- composite material
- graphene composite
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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
- H01M4/364—Composites as mixtures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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 a kind of nano nickel cobalt oxide/graphene composite material and preparation method thereof；The steps include: to be placed in graphene oxide ultrasonic disperse in dehydrated alcohol, cobalt nitrate and nickel nitrate join stirring and dissolving in dehydrated alcohol, sodium hydroxide aqueous slkali is dripped after the two system mixing and stirring, after continuing to stir, put in water heating kettle and react, it is washed out, lyophilization, it is thus achieved that Folium Bambusae shape nano nickel cobalt oxide/graphene composite material.The present invention uses hydro-thermal method with graphene oxide for base material, is prepared for Folium Bambusae shape nano nickel cobalt oxide/graphene composite material.Folium Bambusae shape nano nickel cobalt oxide/graphene composite material prepared by the application present invention has preferable application prospect and economic benefit as lithium ion battery negative.
Description
Technical field
The present invention relates to a kind of nano nickel cobalt oxide/graphene composite material and preparation method thereof, belong to nano material and prepare
Field.
Background technology
In recent years, due to the in short supply of fossil energy and the lifting of people's environmental consciousness, the mankind were to cleaning sustainable energy
Development and utilization constantly make progress, wherein lithium ion battery because of its high voltage, big energy density, excellent cycle performance and
(mobile phone, notebook computer, electric automobile, satellite in the remarkable advantages such as memory-less effect, all trades and professions in life
And Aero-Space etc.) extensively applied and produce certain economic benefit.At present, lithium ion battery has become as this century pair
One of people's lives and the significant new high-tech industry of national economy.Lithium ion battery is mainly made up of four parts,
Being respectively positive pole, negative pole, electrolyte and barrier film, wherein the characteristic of positive and negative pole material greatly affects the property of lithium ion battery
Can, such as reversible capacity, energy density, cycle performance and high rate performance etc..And binary metal oxide cobalt acid nickel (NiCo2O4) with
Unique advantage is had in the application of lithium ion battery negative material by means of its preferable electric conductivity and electro-chemical activity.The most several
Nian Lai, the cobalt acid nickel that scientists has different structure and pattern by different method control synthesis promotes its dependency
Energy.Sun etc. use the three-dimensional porous cobalt acid nickel of Template synthesis [Yang Bai, Ranran Wang, Xiaoyu Lu,
Jing Sun, and Lian Sun. Template method to controllable synthesis 3D porous
NiCo2O4 with enhanced capacitance and stability for supercapacitors[J].
Journal of colloid and interface science, 2016,468:1-9.], Liu etc. uses electrodeposition process
By porous cobalt acid nickel nanowire growth on carbon fiber paper [Liang Huang, Dongchang Chen, Yong Ding,
Shi Feng, Zhonglin Wang, and Meilin Liu. Nickel–cobalt hydroxide nanosheets
coated on NiCo2O4 nanowires grown on carbon fiber paper for high-performance
pseudocapacitors[J]. Nano letters, 2013, 13(7): 3135-3139.].Lou etc. use heat treatment
Cobalt acid nickel nanoneedle is deposited on nickel foam surface [Gen Qiang Zhang, Hao Bin Wu, Harry E. by method
Hoster, Mary B. Chan-Park, and Xiong Wen (David) Lou. Single-crystalline
NiCo2O4 nanoneedle arrays grown on conductive substrates as binder-free
electrodes for high-performance supercapacitors[J]. Energy & Environmental
Science, 2012, 5(11): 9453-9456.]。
The negative material of commercial li-ion battery is graphite at present, and its reversible capacity only has 330 mAhg-1, relatively low；
It addition, for different structure and the preparation of pattern cobalt acid nickel, current majority all needs to add reducing agent and preparation process is numerous and diverse.
Summary of the invention
It is an object of the invention to provide a kind of nano nickel cobalt oxide/graphene composite material and preparation method thereof.
The technical solution realizing the object of the invention is: a kind of nano nickel cobalt oxide/graphene composite material, described compound
Material is bamboo foliation structure.
Wherein, Graphene and the mass ratio of composite are not less than 40%.
Above-mentioned nano nickel cobalt oxide/graphene composite material uses following steps to prepare:
The first step, by graphite oxide ultrasonic disperse in dehydrated alcohol；
Second step, by nickel salt and cobalt salt according to mol ratio 1:2 stirring and dissolving in dehydrated alcohol；
3rd step, mixes the graphene oxide dispersion of first step gained with the mixed solution of second step gained, and stirs；
4th step, then be added dropwise over sodium hydroxide solution regulation pH value to 13 ± 0.1, continue stirring；
5th step, carries out hydro-thermal reaction 16-24h at the 4th step resultant bulk is lain in 160-180 DEG C；
6th step, separates the 5th step product sucking filtration, respectively with deionized water and absolute ethanol washing；
7th step, after the 6th step products therefrom lyophilization, it is thus achieved that the composite of described Folium Bambusae shape.
In the first step, described graphite oxide uses hummer method to prepare, and the ultrasonic disperse time is 30-120 minute.
In second step, the stirring and dissolving time is 20-60 minute.
In 3rd step, mixing time is 30-60 minute.
In 4th step, mixing time is 30-60 minute.
The present invention compared with prior art, has an advantage in that: (1) uses ethanol to be solvent, by hydro-thermal reaction, aoxidizes stone
Ink is reduced into Graphene, it is to avoid use other reducing agents, environmentally safe；(2) using graphene oxide is substrate, system
For Folium Bambusae shape nano nickel cobalt oxide/graphene composite material；Using graphene oxide is Folium Bambusae shape nanometer cobalt acid prepared by substrate
Nickel/graphene composite material has preferable chemical property as lithium ion battery negative, its first charge-discharge reversible capacity
Can up to 1318 mAhg-1, it is expected to be applied in energy storage field.
Accompanying drawing explanation
Fig. 1 is the preparation flow schematic diagram of Folium Bambusae shape nano nickel cobalt oxide/graphene composite material of the present invention.
Fig. 2 is that TEM figure (a) and SEM of Folium Bambusae shape nano nickel cobalt oxide/graphene composite material obtained by case study on implementation 2 scheme
(b).
Fig. 3 is the XRD figure of Folium Bambusae shape nano nickel cobalt oxide/graphene composite material obtained by case study on implementation 2.
Detailed description of the invention
Such as Fig. 1, the Folium Bambusae shape nano nickel cobalt oxide/graphene composite material of the present invention is prepared by following steps:
The first step, by graphite oxide ultrasonic disperse 30-120 minute in dehydrated alcohol；
Second step, stirs nickel salt and cobalt salt 20-60 minute according to mol ratio 1:2 in dehydrated alcohol；
3rd step, mixes the graphene oxide dispersion of first step gained with the mixed solution of second step gained, and stirs 30-
60 minutes；
4th step, then be added dropwise over sodium hydroxide solution regulation pH value to 13 ± 0.1, continue stirring 30-60 minute；
5th step, carries out hydro-thermal reaction 16-24h at the 4th step resultant bulk is lain in 160-180 DEG C；
6th step, separates the 5th step product sucking filtration, respectively with deionized water and absolute ethanol washing；
7th step, after the 6th step products therefrom lyophilization, it is thus achieved that Folium Bambusae shape nano nickel cobalt oxide/graphene composite material.
Case study on implementation 1:
The first step, carries out ultrasonic disperse in dehydrated alcohol 60 minutes by 0.321 g graphite oxide, obtains graphene oxide and divide
Dissipate liquid；
Second step, is dissolved in 40 mL dehydrated alcohol stirring 30 minutes by 0.582 g nickel nitrate and 1.164 g cobalt nitrates；
3rd step, mixes first two steps gained system, and stirs 30 minutes；
4th step, 0.64 g NaOH is dissolved in 10 mL water, is added drop-wise in the 3rd step system after stirring, and continues stirring 30 points
Clock；
5th step, is transferred in water heating kettle hydro-thermal reaction 24 hours at 160 DEG C by the 4th step gained system；
6th step, separates the 5th step product sucking filtration, uses deionized water and absolute ethanol washing for several times respectively；
7th step, after the 6th step products therefrom lyophilization, it is thus achieved that Folium Bambusae shape nano nickel cobalt oxide/graphene composite material.
The Folium Bambusae shape nano nickel cobalt oxide/graphene composite material of preparation is carried out electrification as lithium ion battery negative material
Learning performance test, first charge-discharge reversible capacity is 1287 mAhg-1。
Case study on implementation 2:
The first step, carries out ultrasonic disperse in dehydrated alcohol 60 minutes by 0.321 g graphite oxide, obtains graphene oxide and divide
Dissipate liquid；
Second step, is dissolved in 40 mL dehydrated alcohol stirring 30 minutes by 0.582 g nickel nitrate and 1.164 g cobalt nitrates；
3rd step, mixes first two steps gained system, and stirs 30 minutes；
4th step, 0.64 g NaOH is dissolved in 10 mL water, is added drop-wise in the 3rd step system after stirring, and continues stirring 30 points
Clock；
5th step, is transferred in water heating kettle hydro-thermal reaction 20 hours at 180 DEG C by the 4th step gained system；
6th step, separates the 5th step product sucking filtration, uses deionized water and absolute ethanol washing for several times respectively；
7th step, after the 6th step products therefrom lyophilization, it is thus achieved that Folium Bambusae shape nano nickel cobalt oxide/graphene composite material.
The Folium Bambusae shape nano nickel cobalt oxide/graphene composite material prepared, its transmission electron microscope and scanning electron microscope are respectively such as Fig. 2 a
Shown in Fig. 2 b；Fig. 3 is Folium Bambusae shape nano nickel cobalt oxide/graphene composite material XRD spectra；By the Folium Bambusae shape nanometer cobalt acid of preparation
Nickel/graphene composite material carries out electrochemical property test, first charge-discharge reversible capacity as lithium ion battery negative material
It is 1318 mAhg-1。
Case study on implementation 3:
The first step, carries out ultrasonic disperse in dehydrated alcohol 60 minutes by 0.321 g graphite oxide, obtains graphene oxide and divide
Dissipate liquid；
Second step, is dissolved in 40 mL dehydrated alcohol stirring 30 minutes by 0.582 g nickel nitrate and 1.164 g cobalt nitrates；
3rd step, mixes first two steps gained system, and stirs 30 minutes；
4th step, 0.64 g NaOH is dissolved in 10 mL water, is added drop-wise in the 3rd step system after stirring, and continues stirring 30 points
Clock；
5th step, is transferred in water heating kettle hydro-thermal reaction 16 hours at 200 DEG C by the 4th step gained system；
6th step, separates the 5th step product sucking filtration, uses deionized water and absolute ethanol washing for several times respectively；
7th step, after the 6th step products therefrom lyophilization, it is thus achieved that product.
The Folium Bambusae shape nano nickel cobalt oxide/graphene composite material of preparation is carried out electrification as lithium ion battery negative material
Learning performance test, first charge-discharge reversible capacity is 1135 mAhg-1。
Claims (7)
1. nano nickel cobalt oxide/graphene composite material, it is characterised in that described composite is bamboo foliation structure, graphite
Alkene is not less than 40% with the mass ratio of composite.
2. nano nickel cobalt oxide/graphene composite material as claimed in claim 1, it is characterised in that use following steps to prepare:
The first step, by graphite oxide ultrasonic disperse in dehydrated alcohol；
Second step, by nickel salt and cobalt salt according to mol ratio 1:2 stirring and dissolving in dehydrated alcohol；
3rd step, mixes the graphene oxide dispersion of first step gained with the mixed solution of second step gained, and stirs；
4th step, then be added dropwise over sodium hydroxide solution regulation pH value to 13 ± 0.1, continue stirring；
5th step, carries out hydro-thermal reaction 16-24h at the 4th step resultant bulk is lain in 160-180 DEG C；
6th step, separates the 5th step product sucking filtration, respectively with deionized water and absolute ethanol washing；
7th step, after the 6th step products therefrom lyophilization, it is thus achieved that the composite of described Folium Bambusae shape.
3. nano nickel cobalt oxide/graphene composite material as claimed in claim 2, it is characterised in that in the first step, graphite oxide
Using hummer method to prepare, the ultrasonic disperse time is 30-120 minute.
4. nano nickel cobalt oxide/graphene composite material as claimed in claim 2, it is characterised in that in second step, stirring and dissolving
Time is 20-60 minute.
5. nano nickel cobalt oxide/graphene composite material as claimed in claim 2, it is characterised in that in the 3rd step, mixing time
For 30-60 minute.
6. nano nickel cobalt oxide/graphene composite material as claimed in claim 2, it is characterised in that in the 4th step, mixing time
For 30-60 minute.
7. the preparation method of the nano nickel cobalt oxide/graphene composite material as described in claim 1-6 is arbitrary.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107293413A (en) * | 2017-07-03 | 2017-10-24 | 大连理工大学 | A kind of Ni of the Co doping of graphene coated3(NO3)2(OH)4The preparation method of combination electrode material |
| CN108031427A (en) * | 2017-11-13 | 2018-05-15 | 温州大学 | A kind of technique and application that cobalt acid nickel/graphene composite material is prepared using micro- impact flow reactor |
| CN108387631A (en) * | 2018-01-22 | 2018-08-10 | 中国科学院兰州化学物理研究所 | A kind of graphene-supported cobalt acid nanosized nickel rods compound and its application |
| CN108520827A (en) * | 2018-01-29 | 2018-09-11 | 江苏大学 | Carbon fiber/NiCo2O4The preparation method of/graphene composite material |
| CN109841812A (en) * | 2019-01-25 | 2019-06-04 | 四川师范大学 | A kind of ternary cobalt acid nickel lithium ion battery negative material of sandwich structure and preparation method thereof |
| CN110102304A (en) * | 2019-04-03 | 2019-08-09 | 江苏载驰科技股份有限公司 | A kind of preparation method and application of ferrous acid Raney nickel |
| CN110189921A (en) * | 2019-05-31 | 2019-08-30 | 上海应用技术大学 | A kind of preparation method of nickel cobalt oxide/nitrogen-doped graphene composite material |
| CN110212181A (en) * | 2019-05-22 | 2019-09-06 | 南京理工大学 | Graphene/cobalt-based complex lithium cell negative pole material and preparation method thereof |
| CN110729134A (en) * | 2019-10-25 | 2020-01-24 | 陕西科技大学 | Nano NiCo2O4/rGO/ANF composite film and preparation method and application thereof |
| CN111816867A (en) * | 2020-07-01 | 2020-10-23 | 广西壮族自治区分析测试研究中心 | Sea urchin-shaped NiCo with mesoporous structure2O4Preparation method and application of three-dimensional construction graphene microsphere composite material |
| CN114551892A (en) * | 2022-04-27 | 2022-05-27 | 浙江清华柔性电子技术研究院 | Cobalt niobate oxide-loaded graphene composite material and preparation method and application thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107293413A (en) * | 2017-07-03 | 2017-10-24 | 大连理工大学 | A kind of Ni of the Co doping of graphene coated3(NO3)2(OH)4The preparation method of combination electrode material |
| CN108031427A (en) * | 2017-11-13 | 2018-05-15 | 温州大学 | A kind of technique and application that cobalt acid nickel/graphene composite material is prepared using micro- impact flow reactor |
| CN108387631A (en) * | 2018-01-22 | 2018-08-10 | 中国科学院兰州化学物理研究所 | A kind of graphene-supported cobalt acid nanosized nickel rods compound and its application |
| CN108520827A (en) * | 2018-01-29 | 2018-09-11 | 江苏大学 | Carbon fiber/NiCo2O4The preparation method of/graphene composite material |
| CN109841812A (en) * | 2019-01-25 | 2019-06-04 | 四川师范大学 | A kind of ternary cobalt acid nickel lithium ion battery negative material of sandwich structure and preparation method thereof |
| CN110102304A (en) * | 2019-04-03 | 2019-08-09 | 江苏载驰科技股份有限公司 | A kind of preparation method and application of ferrous acid Raney nickel |
| CN110212181A (en) * | 2019-05-22 | 2019-09-06 | 南京理工大学 | Graphene/cobalt-based complex lithium cell negative pole material and preparation method thereof |
| CN110189921A (en) * | 2019-05-31 | 2019-08-30 | 上海应用技术大学 | A kind of preparation method of nickel cobalt oxide/nitrogen-doped graphene composite material |
| CN110729134A (en) * | 2019-10-25 | 2020-01-24 | 陕西科技大学 | Nano NiCo2O4/rGO/ANF composite film and preparation method and application thereof |
| CN110729134B (en) * | 2019-10-25 | 2021-07-23 | 陕西科技大学 | Nano NiCo2O4/rGO/ANF composite film and preparation method and application thereof |
| CN111816867A (en) * | 2020-07-01 | 2020-10-23 | 广西壮族自治区分析测试研究中心 | Sea urchin-shaped NiCo with mesoporous structure2O4Preparation method and application of three-dimensional construction graphene microsphere composite material |
| CN111816867B (en) * | 2020-07-01 | 2022-11-18 | 广西壮族自治区分析测试研究中心 | Sea urchin-shaped NiCo with mesoporous structure 2 O 4 Preparation method and application of three-dimensional construction graphene microsphere composite material |
| CN114551892A (en) * | 2022-04-27 | 2022-05-27 | 浙江清华柔性电子技术研究院 | Cobalt niobate oxide-loaded graphene composite material and preparation method and application thereof |
| CN114551892B (en) * | 2022-04-27 | 2022-08-02 | 浙江清华柔性电子技术研究院 | Cobalt niobate oxide-loaded graphene composite material and preparation method and application thereof |
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