CN108023071A - Preparation method of foamy graphite alkene nickel-loaded cobalt oxide negative material and products thereof and application - Google Patents
Preparation method of foamy graphite alkene nickel-loaded cobalt oxide negative material and products thereof and application Download PDFInfo
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- CN108023071A CN108023071A CN201711214847.XA CN201711214847A CN108023071A CN 108023071 A CN108023071 A CN 108023071A CN 201711214847 A CN201711214847 A CN 201711214847A CN 108023071 A CN108023071 A CN 108023071A
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- nickel
- graphite alkene
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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
- H01M4/366—Composites as layered products
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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
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative 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
- Y02E60/10—Energy storage using batteries
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Abstract
The present invention provides a kind of preparation method of foamy graphite alkene nickel-loaded cobalt oxide negative material and products thereof and application, nickel foam is handled, and be immersed in graphene oxide solution, electronation is carried out with reducing agent to the graphene oxide being coated in nickel foam in the solution；The nickel foam for being coated with graphene is placed in solution, by acid corrosion nickel foam, while adds corresponding cobalt salt, it is 1 to make the mole of nickel salt and cobalt salt:2；The solution is transferred in 100 mL hydrothermal reaction kettles, 160~180 DEG C of 3~5 h of reaction；It is cooled to room temperature, sediment is filtered by vacuum, then washed for several times with water and ethanol, then 60~80 DEG C of 10~15 h of drying of vacuum drying oven；By above-mentioned sediment in 500~600 DEG C of 3~5 h of temperature lower calcination, foamy graphite alkene nickel-loaded cobalt oxide is obtained.The material has larger specific surface area, is further conducive to improve the chemical property of material.The preparation process is relatively easy, easy to operate.
Description
Technical field
The present invention relates to a kind of preparation method of lithium cell negative pole material, and nickel cobalt is loaded more particularly to a kind of foamy graphite alkene
Preparation method of oxygen negative material and products thereof and application.
Background technology
With the development of society, lithium ion battery receives much concern.Lithium ion battery be it is ideal in the world at present can
Rechargeable battery, it not only has the advantages that energy density is big, has extended cycle life, memory-less effect and pollution are small.With technology
Progressive, lithium ion battery will be widely used in the fields such as electric automobile, aerospace and biological medicine, therefore, research and development
Power is of great significance with lithium ion battery and associated materials.For power lithium ion battery, its key is to carry
High power density and energy density, and what power density and energy density improved is electrode material at all, is particularly negative material
Improvement.
From the beginning of the nineties in last century, Japanese scientific worker have developed the carbon material of layer structure, and carbon material is most
It is early to be studied by people and be applied to the material of lithium ion battery commercialization, be still everybody concern so far and the emphasis studied it
One, but there are some defects for carbon negative pole material：During Battery formation, react to form SEI films with electrolyte, cause disappearing for electrolyte
Consumption and relatively low coulombic efficiency first；During over-charging of battery, it may form Li dendrite at carbon electrodes precipitating metal lithium and cause
Short circuit, causes temperature to raise, battery explosion；In addition, diffusion coefficient of the lithium ion in carbon material is smaller, cause battery real
Existing high current charge-discharge, so as to limit the application range of lithium ion battery.
Nickel cobalt oxygen（NiCo2O4）It is a kind of composite oxides of spinel structure, is a kind of widely applied magnetic material,
Fuel cell material is commonly used for, lithium ion battery negative material can also be used as at present, is had by conversion and alloying reaction
Higher Li+Storage volume.The material is considered as a kind of promising ion cathode material lithium.
The content of the invention
For overcome the deficiencies in the prior art, present invention aims at：A kind of foamy graphite alkene nickel-loaded cobalt oxide anode is provided
The preparation method of material.
Still a further object of the present invention is：The product that a kind of above-mentioned preparation method obtains is provided.
Another object of the present invention is：A kind of application of the said goods is provided.
The object of the invention is realized by following proposal：A kind of preparation side of foamy graphite alkene nickel-loaded cobalt oxide negative material
Method, comprises the following steps：
（1）Nickel foam is handled, and is immersed in graphene oxide solution, in the solution the oxygen to being coated in nickel foam
Graphite alkene carries out electronation with reducing agent；
（2）The nickel foam for being coated with graphene is placed in solution, by acid corrosion nickel foam, while adds corresponding cobalt salt,
It is 1 to make the mole of nickel salt and cobalt salt:2；
（3）The solution is transferred in 100 mL hydrothermal reaction kettles, 160~180 DEG C of 3~5 h of reaction；
（4）It is cooled to room temperature, sediment is filtered by vacuum, is then washed for several times with water and ethanol, then vacuum drying oven 60~80
DEG C dry 10~15 h；
（5）By above-mentioned sediment in 500~600 DEG C of 3~5 h of temperature lower calcination, foamy graphite alkene nickel-loaded cobalt oxide is obtained.
The reducing agent is one kind or its combination in hydrazine hydrate, hydroiodic acid or ascorbic acid.
The acid is one kind or its combination in hydrochloric acid, acetic acid or nitric acid.
The cobalt salt is one kind or its combination in cobalt chloride, cobalt acetate or cobalt nitrate.
The present invention provides a kind of foamy graphite alkene nickel-loaded cobalt oxide negative material, is prepared into according to any of the above-described the method
Arrive.
The present invention provides a kind of application of foamy graphite alkene nickel-loaded cobalt oxide negative material in lithium ion battery.
The present invention is that template prepares foamy graphite alkene, by original raw material of the template nickel salt of dissolving, preparation is steeped using nickel foam
The graphene-supported nickel cobalt oxygen of foam, the material have larger specific surface area, are further conducive to improve the chemical property of material.
Preparation method of the present invention is relatively easy with technique, easy-operating feature.Its product first discharge specific capacity is 1211 mAh/g,
Second of specific discharge capacity is 689 mAh/g, and specific discharge capacity is 385 mAh/g after 50 circulations.
Brief description of the drawings
Fig. 1 is the cycle life figure of 1 foamy graphite alkene nickel-loaded cobalt oxide of embodiment.
Embodiment
The present invention is described in detail by following instantiation, but protection scope of the present invention is not only restricted to these
Examples of implementation.
Embodiment 1
Nickel foam is handled, and is immersed in graphene oxide solution, in the solution the oxidation to being coated in nickel foam
Graphene carries out electronation with ascorbic acid；The nickel foam for being coated with graphene is placed in solution, is steeped by hcl corrosion
Foam nickel, while cobalt chloride is added, it is 1 to make the mole of nickel chloride and cobalt chloride:2；The solution is transferred to 100 mL hydro-thermal reactions
In kettle, 160 DEG C of 5 h of reaction；It is cooled to room temperature, sediment is filtered by vacuum, is then washed for several times with water and ethanol, Ran Houzhen
Empty 80 DEG C of 10 h of drying of baking oven；By above-mentioned sediment in 500 DEG C of 5 h of temperature lower calcination, foamy graphite alkene load nickel cobalt is obtained
Oxygen.The cycle life figure of foamy graphite alkene nickel-loaded cobalt oxide is as shown in Figure 1, first discharge specific capacity is 1211 mAh/g, second
Secondary specific discharge capacity is 689 mAh/g, and specific discharge capacity is 385 mAh/g after 50 circulations.
Embodiment 2
Nickel foam is handled, and is immersed in graphene oxide solution, in the solution the oxidation to being coated in nickel foam
Graphene carries out electronation with hydroiodic acid；The nickel foam for being coated with graphene is placed in solution, foam is corroded by nitric acid
Nickel, while cobalt nitrate is added, it is 1 to make the mole of nickel nitrate and cobalt nitrate:2；The solution is transferred to 100 mL hydrothermal reaction kettles
In, 180 DEG C of 3 h of reaction；It is cooled to room temperature, sediment is filtered by vacuum, is then washed for several times with water and ethanol, then vacuum
80 DEG C of 10 h of drying of baking oven；By above-mentioned sediment in 600 DEG C of 3 h of temperature lower calcination, foamy graphite alkene nickel-loaded cobalt oxide is obtained.
Embodiment 3
Nickel foam is handled, and is immersed in graphene oxide solution, in the solution the oxidation to being coated in nickel foam
Graphene carries out electronation with hydrazine hydrate；The nickel foam for being coated with graphene is placed in solution, foam is corroded by nitric acid
Nickel, while cobalt nitrate is added, it is 1 to make the mole of nickel nitrate and cobalt nitrate:2；The solution is transferred to 100 mL hydrothermal reaction kettles
In, 180 DEG C of 3 h of reaction；It is cooled to room temperature, sediment is filtered by vacuum, is then washed for several times with water and ethanol, then vacuum
80 DEG C of 10 h of drying of baking oven；By above-mentioned sediment in 600 DEG C of 3 h of temperature lower calcination, foamy graphite alkene nickel-loaded cobalt oxide is obtained.
Claims (6)
1. a kind of preparation method of foamy graphite alkene nickel-loaded cobalt oxide negative material, it is characterised in that comprise the following steps：
（1）Nickel foam is handled, and is immersed in graphene oxide solution, in the solution the oxygen to being coated in nickel foam
Graphite alkene carries out electronation with reducing agent；
（2）The nickel foam for being coated with graphene is placed in solution, by acid corrosion nickel foam, while adds corresponding cobalt salt,
It is 1 to make the mole of nickel salt and cobalt salt:2；
（3）The solution is transferred in 100 mL hydrothermal reaction kettles, 160~180 DEG C of 3~5 h of reaction；
（4）It is cooled to room temperature, sediment is filtered by vacuum, is then washed for several times with water and ethanol, then vacuum drying oven 60~80
DEG C dry 10~15 h；
（5）By above-mentioned sediment in 500~600 DEG C of 3~5 h of temperature lower calcination, foamy graphite alkene nickel-loaded cobalt oxide is obtained.
2. the preparation method of foamy graphite alkene nickel-loaded cobalt oxide negative material according to claim 1, it is characterised in that described
Reducing agent be one kind in hydrazine hydrate, hydroiodic acid or ascorbic acid or its combination.
3. the preparation method of foamy graphite alkene nickel-loaded cobalt oxide negative material according to claim 1, it is characterised in that described
Acid be hydrochloric acid, acetic acid or nitric acid in one kind or its combination.
4. the preparation method of foamy graphite alkene nickel-loaded cobalt oxide negative material according to claim 1, it is characterised in that described
Cobalt salt be cobalt chloride, cobalt acetate or cobalt nitrate in one kind or its combination.
5. a kind of foamy graphite alkene nickel-loaded cobalt oxide negative material, it is characterised in that according to any the methods of claim 1-4
It is prepared.
6. application of the foamy graphite alkene nickel-loaded cobalt oxide negative material in lithium ion battery according to claim 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711214847.XA CN108023071A (en) | 2017-11-28 | 2017-11-28 | Preparation method of foamy graphite alkene nickel-loaded cobalt oxide negative material and products thereof and application |
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| CN201711214847.XA CN108023071A (en) | 2017-11-28 | 2017-11-28 | Preparation method of foamy graphite alkene nickel-loaded cobalt oxide negative material and products thereof and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108899501A (en) * | 2018-06-28 | 2018-11-27 | 肇庆市华师大光电产业研究院 | A kind of preparation method of foamy graphite alkene composite sulfuration indium Zinc material |
| CN112435859A (en) * | 2020-11-12 | 2021-03-02 | 西北工业大学 | Super capacitor adopting superstructure graphene foam and preparation method thereof |
| CN114214634A (en) * | 2021-11-05 | 2022-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of graphite plate loaded porous nanosheet cobalt nitride-zinc oxide, product and application |
| CN116779830A (en) * | 2023-08-22 | 2023-09-19 | 浙江煌能新能源科技有限公司 | Lithium battery positive electrode material with coating structure, preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104291324A (en) * | 2014-09-09 | 2015-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene foams |
| CN106938859A (en) * | 2017-04-01 | 2017-07-11 | 吉林大学 | One step hydro thermal method prepares cathode of lithium battery tubular material NiCo2O4Method |
-
2017
- 2017-11-28 CN CN201711214847.XA patent/CN108023071A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104291324A (en) * | 2014-09-09 | 2015-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene foams |
| CN106938859A (en) * | 2017-04-01 | 2017-07-11 | 吉林大学 | One step hydro thermal method prepares cathode of lithium battery tubular material NiCo2O4Method |
Non-Patent Citations (4)
| Title |
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| PINJARI SYEDVALI等: "In situ fabrication of graphene decorated microstructured globe artichokes of partial molar nickel cobaltite anchored on a Ni foam as a high－performance supercapacitor electrode", 《THE ROYAL SOCIETY OF CHEMISTRY》 * |
| SHUMIN SUN等: "Asymmetric supercapacitors based on a NiCo2O4/three dimensional graphene composite and three dimensional graphene with high energy density", 《THE ROYAL SOCIETY OF CHEMISTRY》 * |
| YUEXING JIANG等: "Needle-like NiCo2O4 Coated on Graphene Foam as a Flexible Cathode for Lithium-Oxygen Batteries", 《CHEMELECTROCHEM》 * |
| 祁永东: "三维石墨烯基Co-Ni 双氢氧化物复合材料", 《应用化工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108899501A (en) * | 2018-06-28 | 2018-11-27 | 肇庆市华师大光电产业研究院 | A kind of preparation method of foamy graphite alkene composite sulfuration indium Zinc material |
| CN112435859A (en) * | 2020-11-12 | 2021-03-02 | 西北工业大学 | Super capacitor adopting superstructure graphene foam and preparation method thereof |
| CN114214634A (en) * | 2021-11-05 | 2022-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of graphite plate loaded porous nanosheet cobalt nitride-zinc oxide, product and application |
| CN114214634B (en) * | 2021-11-05 | 2023-11-24 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation, product and application of graphite plate loaded porous nano-sheet cobalt nitride-zinc oxide |
| CN116779830A (en) * | 2023-08-22 | 2023-09-19 | 浙江煌能新能源科技有限公司 | Lithium battery positive electrode material with coating structure, preparation method and application thereof |
| CN116779830B (en) * | 2023-08-22 | 2023-12-05 | 浙江煌能新能源科技有限公司 | Lithium battery positive electrode material with coating structure, preparation method and application thereof |
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Application publication date: 20180511 |