CN105355893B - The preparation method of flexible lithium ion battery negative material - Google Patents
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- CN105355893B CN105355893B CN201510945159.5A CN201510945159A CN105355893B CN 105355893 B CN105355893 B CN 105355893B CN 201510945159 A CN201510945159 A CN 201510945159A CN 105355893 B CN105355893 B CN 105355893B
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/502—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese for non-aqueous cells
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention discloses a kind of preparation method of flexible lithium ion battery negative material, for solving the technical problem of the flexible difference of the lithium ion battery negative material of the preparation method of existing lithium ion battery negative material preparation.Technical scheme is using length as 100 μm or so of overlength MnO2Nano wire is matrix, adds graphene oxide solution, the Mn using secondary water hot preparation with flexible self-supporting3O4/ rGO electrode materials, prepared electrode material are used directly for the negative material of lithium ion battery, without additionally using conductive additive and binding agent.Wherein, the ratio shared by redox graphene is 20% 60%.Due to the manganese dioxide nanowire that the matrix utilized is overlength, therefore the lithium ion battery negative material prepared has self-supporting, improves the flexible characteristic of lithium ion battery negative material.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material, more particularly to a kind of flexible lithium ion battery
The preparation method of negative material.
Background technology
Since 21 century, as the increasingly exhaustion of the non-renewable resources such as coal, oil, natural gas, and its combustion zone come
Environmental pollution, the energy and environment two large problems have become the bottleneck problem for hindering world today's sustainable development.In order to
Solve this world-famous puzzle, seek the renewable green energy resource for substituting conventional fossil fuel and the harmonious development for seeking human and environment
Seem particularly urgent.The representative lithium ion battery of novel energy has energy density height, had extended cycle life and memory-less effect etc.
Advantage and be widely used in portable electric appts.In recent years, with the development of flexibility/foldable electronic, exploitation
Flexible lithium ion battery with flexural property is as one of forward position direction of current energy storage area research.
In terms of negative material, theoretical capacity (the 372mAh g of current commercialized graphite as anode material for lithium-ion battery-1) relatively low, the raising of lithium ion battery chemical property is limited, therefore design and prepare high performance lithium ionic cell cathode material
Material is to meet the key factor that lithium ion battery develops to electrical equipment.Transition metal oxide has the advantages of high power capacity, its
Middle Mn oxide (MnOx) in addition to possessing the characteristics of high theoretical specific capacity, also with natural rich reserves, cheap, green ring
Protect, the series of advantages such as charge and discharge platform is low, efficient energy conversion is high.But MnOxAs the electrode material of lithium ion battery,
There is the problem of capacity utilization is low, high rate performance is poor, cyclical stability is poor, its poorly conductive and lithium ion are primarily due to
Volumetric expansion occurs during embedded and abjection.Can be above-mentioned to improve by building specific appearance structure and preparing composite
Capacity attenuation caused by problem etc..Wherein graphene is because of its excellent electric conductivity, mechanical stability and 2630m2g-1Ratio table
Area and be widely used in preparing transition metal oxide/graphene composite material, for improving the property of negative electrode of lithium ion battery
Energy.
Document " Li L, Guo Z, Du A, et al.Rapid microwave-assisted synthesis of
Mn3O4–graphene nanocomposite and its lithium storage properties[J].Journal of
Materials Chemistry,2012,22(8):3600-3605. " disclose a kind of preparation of lithium ion battery negative material
Method.This method successfully synthesizes Mn using microwave-hydrothermal method3O4With the nano composite material of graphene and be successfully applied to lithium from
Sub- cell negative electrode material, but the product form of its synthesis is nanometer powder, and conductive addition has been used in the assembling process of electrode
Agent and binding agent, and the electrode material prepared does not possess the characteristic of flexible bendable.
The content of the invention
In order to overcome lithium ion battery negative material prepared by the preparation method of existing lithium ion battery negative material flexible
The deficiency of difference, the present invention provide a kind of preparation method of flexible lithium ion battery negative material.This method is using length as 100 μm of left sides
Right overlength MnO2Nano wire is matrix, adds graphene oxide solution, has flexible self-supporting using secondary water hot preparation
Mn3O4/ rGO electrode materials, prepared electrode material are used directly for the negative material of lithium ion battery, without additionally making
With conductive additive and binding agent.Wherein, the ratio shared by redox graphene is 20%-60%.Due to the matrix utilized
Lithium ion battery negative material for the manganese dioxide nanowire of overlength, therefore preparation has self-supporting, improves lithium-ion electric
The flexible characteristic of pond negative material.
The technical solution adopted for the present invention to solve the technical problems：A kind of preparation of flexible lithium ion battery negative material
Method, it is characterized in comprising the following steps：
Step 1: the mixed solution of the manganese salt prepared, oxidant and acid is moved into hydrothermal reaction kettle, 110~260
At a temperature of DEG C, hydro-thermal reaction 12-96h, the manganese dioxide nanowire that hydro-thermal is obtained is rushed repeatedly using ultra-pure water and absolute ethyl alcohol
Wash more than 3 times, forced air drying or vacuum drying more than 4h are then carried out at a temperature of 60~150 DEG C；
Step 2: the manganese dioxide nanowire that step 1 is prepared is distributed in deionized water, graphite oxide is added
Alkene solution, 0.25~8h of ultrasonic disperse, obtain well mixed MnO2/ GO suspensions；
Step 3: the MnO that step 2 is prepared2/ GO mixing suspensions are moved into hydrothermal reaction kettle, 100~220
At a temperature of DEG C, hydro-thermal reaction 8-48h, Mn is obtained3O4/rGO；
Step 4: the Mn that step 3 is prepared3O4/ rGO is scattered in deionized water and absolute ethyl alcohol, utilizes vacuum
Filter and obtain flexible Mn3O4/ rGO films, it is subsequently placed in 60~90 DEG C of vacuum drying chamber and dries；
Step 5: the flexible Mn that step 4 is prepared3O4Negative material of/rGO the films directly as lithium ion battery
Assemble lithium ion battery.
The manganese salt, oxidant and acid are to analyze pure, ultra-pure water resistivity >=25 DEG C of 18.2M Ω .cm@.
The manganese salt is any of manganese sulfate, manganese chloride, manganese nitrate or manganese acetate.
The oxidant is any of potassium chlorate, ammonium sulfate, ammonium persulfate, potassium permanganate or ammonium fluoride or appointed several.
The acid is any of acetic acid, hydrochloric acid or nitric acid.
The beneficial effects of the invention are as follows：This method is using length as 100 μm or so of overlength MnO2Nano wire is matrix, addition
Graphene oxide solution, there is the Mn of flexible self-supporting using secondary water hot preparation3O4/ rGO electrode materials, prepared electrode
Material is used directly for the negative material of lithium ion battery, without additionally using conductive additive and binding agent.Wherein, reduce
Ratio shared by graphene oxide is 20%-60%.Because the matrix utilized is the manganese dioxide nanowire of overlength, therefore prepare
Lithium ion battery negative material has self-supporting, improves the flexible characteristic of lithium ion battery negative material.
The present invention is elaborated with reference to the accompanying drawings and detailed description.
Brief description of the drawings
Fig. 1 is the preparation method flow chart of flexible lithium ion battery negative material of the present invention.
Fig. 2 is the stereoscan photograph that the inventive method embodiment 1 prepares flexible lithium ion battery negative material.
Fig. 3 is that the inventive method embodiment 1 prepares flexible lithium ion battery negative material, GO and pure MnO2X ray spread out
Penetrate collection of illustrative plates.
Fig. 4 is the chemical property figure that the inventive method embodiment 1 prepares flexible lithium ion battery negative material.
Embodiment
Following examples reference picture 1-4.
Embodiment 1.
1) deionized water that 4mmol manganese nitrates, 6mmol potassium chlorate, 7mmol sodium acetates and 4mL acetic acid add 60mL is weighed
In, after being sufficiently stirred dissolving, solution is transferred in the water heating kettle that capacity is 100mL, water heating kettle is put into drying box and is heated to
110 DEG C are incubated 96h, naturally cool to room temperature after hydro-thermal reaction, obtain MnO2, respectively rushed using deionized water and absolute ethyl alcohol
Wash 3 times, filter obtained MnO2Self-supported membrane dries 10h at 60 DEG C；
2) MnO of 80mg steps 1) preparation is weighed2, it is dissolved in 40mL deionized waters, is uniformly mixing to obtain MnO2,
Then weigh 80mg GO to be dissolved in 40mL deionized waters, ultrasonic disperse 8h, form uniform GO dispersion liquids, will be obtained above
Two kinds of solution mixing, are stirred at room temperature 2h, obtain uniform MnO2/ GO mixing suspensions；
3) MnO for preparing step 2)2/ GO mixing suspensions are moved into water heating kettle, and water heating kettle is put into drying box
160 DEG C of insulation 12h are heated to, room temperature is naturally cooled to after hydro-thermal reaction, obtains Mn3O4/ rGO, uses deionized water and nothing
Water-ethanol is respectively rinsed 3 times, filters, and the Mn that 24h is obtained is dried at 80 DEG C3O4/ rGO flexible membranes.Figure it is seen that the present embodiment
The lithium ion battery negative material of preparation has self-supporting, improves the flexible characteristic of lithium ion battery negative material.From Fig. 3
As can be seen that the thing phase composition of lithium ion battery negative material manufactured in the present embodiment is Mn3O4@rGO.Pass through as seen from Figure 4
After crossing 100 circulations, the specific capacity of lithium ion battery negative material manufactured in the present embodiment is stable in 700mAh/g.
Embodiment 2.
1) deionized water that 2mmol manganese acetates, 3mmol potassium chlorate, 5mmol potassium acetates and 2mL acetic acid add 30mL is weighed
In, after being sufficiently stirred dissolving, solution is transferred in the water heating kettle that capacity is 50mL, water heating kettle is put into drying box and is heated to
140 DEG C are incubated 70h, naturally cool to room temperature after hydro-thermal reaction, obtain MnO2, respectively rushed using deionized water and absolute ethyl alcohol
Wash 3 times, filter obtained U-MnO2Self-supported membrane dries 24h at 90 DEG C；
2) MnO of 40mg steps 1) preparation is weighed2, it is dissolved in 40mL deionized waters, is uniformly mixing to obtain MnO2,
Then weigh 40mg GO to be dissolved in 40mL deionized waters, ultrasonic disperse 3h, form uniform GO dispersion liquids, will be obtained above
Two kinds of solution mixing, are stirred at room temperature 2h, obtain uniform MnO2/ GO mixing suspensions；
3) MnO for preparing step 2)2/ GO mixing suspensions are moved into water heating kettle, and water heating kettle is put into drying box
180 DEG C of insulation 10h are heated to, room temperature is naturally cooled to after hydro-thermal reaction, obtains Mn3O4/ rGO, uses deionized water and nothing
Water-ethanol is respectively rinsed 3 times, filters, and the Mn that 24h is obtained is dried at 70 DEG C3O4@rGO flexible membranes.By Mn3O4/ rGO materials are directly made
Lithium ion battery is assembled into for negative pole, specific capacity can reach 650mAh/g after 100 circulations.
Embodiment 3.
1) deionized water that 4mmol manganese chlorides, 6mmol potassium chlorate, 7mmol potassium acetates and 4mL nitric acid add 70mL is weighed
In, after being sufficiently stirred dissolving, solution is transferred in the water heating kettle that capacity is 100mL, water heating kettle is put into drying box and is heated to
200 DEG C are incubated 40h, naturally cool to room temperature after hydro-thermal reaction, obtain MnO2, respectively rushed using deionized water and absolute ethyl alcohol
Wash 3 times, filter obtained MnO2Self-supported membrane dries 40h at 120 DEG C；
2) MnO of 160mg steps 1) preparation is weighed2, it is dissolved in 40mL deionized waters, is uniformly mixing to obtain MnO2,
Then weigh 80mg GO to be dissolved in 40mL deionized waters, ultrasonic disperse 6h, form uniform GO dispersion liquids, will be obtained above
Two kinds of solution mixing, are stirred at room temperature 2h, obtain uniform MnO2/ GO mixing suspensions；
3) MnO for preparing step 2)2/ GO mixing suspensions are moved into water heating kettle, and water heating kettle is put into drying box
180 DEG C of insulation 18h are heated to, room temperature is naturally cooled to after the completion of hydro-thermal reaction, obtains Mn3O4/@rGO, using deionized water and
Absolute ethyl alcohol is respectively rinsed 3 times, filters, and the Mn that 24h is obtained is dried at 90 DEG C3O4/ rGO flexible membranes.By Mn3O4/ rGO materials are direct
Lithium ion battery is assembled into as negative pole.Specific capacity may remain in more than 550mAh/g after 200 circulations.
Embodiment 4.
1) weigh 3mmol potassium permanganate and 3mmol ammonium fluorides are added in 40mL deionized water, after being sufficiently stirred dissolving,
Solution is transferred in the water heating kettle that capacity is 50mL, water heating kettle is put into drying box and is heated to 260 DEG C of insulation 12h, hydro-thermal is anti-
Room temperature is naturally cooled to after answering, obtains MnO2, respectively rinsed 3 times using deionized water and absolute ethyl alcohol, filter obtained MnO2
Self-supported membrane dries 24h at 100 DEG C；
2) MnO of 90mg steps 1) preparation is weighed2, it is dissolved in 40mL deionized waters, is uniformly mixing to obtain MnO2,
Then weigh 50mg GO to be dissolved in 50mL deionized waters, ultrasonic disperse 0.25h, form uniform GO dispersion liquids, obtained above-mentioned
Two kinds of solution mixing, 2h is stirred at room temperature, obtains uniform MnO2/ GO mixing suspensions；
3) MnO for preparing step 2)2/ GO mixing suspensions are moved into water heating kettle, and water heating kettle is put into drying box
220 DEG C of insulation 8h are heated to, room temperature is naturally cooled to after the completion of hydro-thermal reaction, obtains Mn3O4/ rGO, uses deionized water and nothing
Water-ethanol is respectively rinsed 3 times, filters, and the Mn that 24h is obtained is dried at 60 DEG C3O4/ rGO flexible membranes.By Mn3O4/ rGO materials are directly made
Lithium ion battery is assembled into for negative pole.Specific capacity may remain in more than 600mAh/g after 100 circulations.
Inventor is also by the oxidant including the manganese salt including manganese sulfate, with ammonium sulfate, ammonium persulfate, and including hydrochloric acid
Sour various combination be applied to above example in tested, achieve good effect.
Claims (3)
1. a kind of preparation method of flexible lithium ion battery negative material, it is characterised in that comprise the following steps：
Step 1: the mixed solution of the manganese salt prepared, oxidant and acid is moved into hydrothermal reaction kettle, in 110~260 DEG C of temperature
Under degree, hydro-thermal reaction 12-96h, the manganese dioxide nanowire that hydro-thermal is obtained is rinsed 3 times repeatedly using ultra-pure water and absolute ethyl alcohol
More than, forced air drying or vacuum drying more than 4h are then carried out at a temperature of 60~150 DEG C；
Step 2: the manganese dioxide nanowire that step 1 is prepared is distributed in deionized water, it is molten to add graphene oxide
Liquid, 0.25~8h of ultrasonic disperse, obtain well mixed MnO2/ GO suspensions；
Step 3: the MnO that step 2 is prepared2/ GO mixing suspensions are moved into hydrothermal reaction kettle, in 100~220 DEG C of temperature
Under degree, hydro-thermal reaction 8-48h, Mn is obtained3O4/rGO；
Step 4: the Mn that step 3 is prepared3O4/ rGO is scattered in deionized water and absolute ethyl alcohol, utilizes vacuum filtration
Obtain flexible Mn3O4/ rGO films, it is subsequently placed in 60~90 DEG C of vacuum drying chamber and dries；
Step 5: the flexible Mn that step 4 is prepared3O4/ rGO films assemble directly as the negative material of lithium ion battery
Lithium ion battery；
The oxidant is any of potassium chlorate, ammonium sulfate, ammonium persulfate, potassium permanganate or ammonium fluoride or appointed several；
The acid is any of acetic acid, hydrochloric acid or nitric acid.
2. the preparation method of flexible lithium ion battery negative material according to claim 1, it is characterised in that：The manganese
Salt, oxidant and acid are to analyze pure, ultra-pure water resistivity >=18.2M Ω .cm at 25 DEG C.
3. the preparation method of flexible lithium ion battery negative material according to claim 1, it is characterised in that：The manganese salt
It is any of manganese sulfate, manganese chloride, manganese nitrate or manganese acetate.
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| CN105514398B (en) * | 2016-03-04 | 2017-11-10 | 中国石油大学(华东) | A kind of graphite oxide/manganese oxide controllable nano composite for electrode of lithium cell |
| CN105870399A (en) * | 2016-04-15 | 2016-08-17 | 厦门大学 | Preparation method of transition metal oxide@ linear carbon negative electrode with porous mesh structure |
| KR101896040B1 (en) * | 2016-11-09 | 2018-09-06 | 한국화학연구원 | Fiber electrode containing active materials with controlled morphology and preparation method thereof |
| CN106672935B (en) * | 2016-12-26 | 2019-01-11 | 西北工业大学 | A kind of preparation method of the hollow porous carbon materials of N doping |
| CN108258334B (en) * | 2018-01-19 | 2020-11-24 | 北京大学深圳研究生院 | Composite flexible electrode, preparation method and application thereof |
| CN109713263A (en) * | 2018-12-19 | 2019-05-03 | 华电电力科学研究院有限公司 | A kind of anode material for lithium-ion batteries stratiform δ-MnO2The preparation method of/rGO |
| CN111180715B (en) * | 2020-02-16 | 2021-04-06 | 深圳市艾维普思科技有限公司 | Lithium battery flexible negative electrode material for wearable electronic equipment and preparation method |
| CN112701295B (en) * | 2020-12-29 | 2022-02-22 | 蜂巢能源科技有限公司 | Graphite fibrofelt flexible current collector, preparation method thereof and flexible battery |
| CN113054175A (en) * | 2021-03-15 | 2021-06-29 | 西北工业大学 | Flexible zinc ion battery anode material MnO2Preparation method of/C film |
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| KR101459736B1 (en) * | 2013-04-25 | 2014-11-20 | 주식회사 포스코 | Manufacturing method for cathode active material for lithium second battery |
| CN103700815A (en) * | 2013-12-11 | 2014-04-02 | 中山大学 | Flexible transparent lithium ion battery electrode material and preparation method thereof |
| CN104022262A (en) * | 2014-06-03 | 2014-09-03 | 浙江工业大学 | Preparation method of manganous-manganic oxide/graphene composite material |
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