CN104993143A - Preparation method of self-support lithium ion battery cathode material - Google Patents
Preparation method of self-support lithium ion battery cathode material Download PDFInfo
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- CN104993143A CN104993143A CN201510271384.5A CN201510271384A CN104993143A CN 104993143 A CN104993143 A CN 104993143A CN 201510271384 A CN201510271384 A CN 201510271384A CN 104993143 A CN104993143 A CN 104993143A
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
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- 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
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- 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
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Abstract
The invention relates to a preparation method of a self-support lithium ion battery cathode material. The method includes: making a manganese salt, an oxidant and a solvent into an ultralong one-dimensional manganese dioxide (U-MnO2) nanowire by a hydrothermal technique, dispersing the U-MnO2 in an acidic solution and adding a proper amount of an organic monomer to obtain a U-MnO2@high polymer compound, carrying out cleaning, pumping filtration and drying to obtain a self-support membrane, and carrying out high temperature heat treatment to obtain the self-support carbon coated MnO(MnO@C) electrode material. The MnO@C prepared by the method can be directly used as the cathode material of a lithium ion battery without additional current collector, conductive additive and binder. The material has the characteristics of simple preparation process, high structure stability, self-current collection, excellent electrochemical performance and the like.
Description
Technical field
The invention belongs to lithium ion battery electrode material field, be specifically related to a kind of preparation method of self-supporting lithium ion battery negative material, particularly relate to the complex method of active material and material with carbon element.
Background technology
In the last few years; the a series of energy crises such as fossil energy decays day by day, climate warming, environmental pollution and the environmental problem serious threat survival and development of the mankind; novel energy is due to environmental protection, and the features such as reusable edible, by development and utilization widely.As the representative of novel energy, operating voltage is high, energy density is large, self-discharge rate is low because having for lithium ion battery, have extended cycle life, the advantage such as memory-less effect and environmental protection, be widely used at portable electric appts and electric automobile field, and be expected to be applied in military aerospace field.
Negative material is the important component part of lithium ion battery.At present, commercial negative material is graphite, but, the theoretical specific capacity of graphite is only 372mAh/g, and discharging efficiency is low first, cannot meet the growth requirement of society, therefore, study novel high-capacity negative material and become study hotspot and emphasis.Transition metal oxide has the advantage of high power capacity, wherein Mn oxide (MnO
x) except possessing high theoretical specific capacity (as MnO
2: 1232mAh/g) feature outside, also there is natural rich reserves, cheap, environmental protection, the series of advantages such as charge and discharge platform is low, efficient energy conversion is high.But, MnO
xas the electrode material of lithium ion battery, there is the problem that capacity utilization is low, high rate performance is poor, cyclical stability is poor, main cause is the property led difference and discharge and recharge generation volumetric expansion.
For solving the problem, researcher proposes nanometer and Composite two kinds of means, still there is first the problems such as coulombic efficiency is low, thermodynamic stability is poor, structural instability in the former, and the latter mainly utilizes material with carbon element compound, such as Graphene and carbon nano-tube, but Graphene and carbon nano-tube expensive, limit its further industrialized development.Therefore, a kind of cheap efficient composite preparation process is sought extremely urgent.
Summary of the invention
The technical problem solved
In order to avoid the deficiencies in the prior art part, the present invention proposes a kind of preparation method of self-supporting lithium ion battery negative material, and preparation has strong, the with low cost and eco-friendly self-supporting lithium ion battery negative material of height ratio capacity, long circulation life, high-rate characteristics, process transplanting.
Technical scheme
A preparation method for self-supporting lithium ion battery negative material, is characterized in that step is as follows:
Step 1: by manganese salt and the oxidant raw material mixed in molar ratio according to 0.5 ~ 5 ︰ 1, adopts solvent to make solution, utilizes hydro thermal method to prepare overlength one dimension manganese dioxide U-MnO
2nano wire; The hydrothermal temperature of described hydro thermal method is 110 ~ 260 DEG C, and the hydro-thermal time is >6h;
Step 2: by U-MnO
2, acid and organic monomer according to the mixed in molar ratio of 1 ~ 5 ︰ 1 ︰ 1, be obtained by reacting the coated MnO of high polymer through original position Interface composites
2, be MnO
2@high polymer, obtains MnO through cleaning, drying, suction filtration
2@high-polymer membrane;
Step 3: by MnO
2@high-polymer membrane is placed in atmosphere furnace carbonization, obtains the carbon coated manganese oxide film MnO@C with self-supporting characteristic; Described heat treatment temperature when being placed in atmosphere furnace carbonization is 400 ~ 1500 DEG C, and heat treatment time is 0.5 ~ 12h, and heat-treating atmosphere is inert gas shielding or vacuum protection.
Described manganese salt is manganese sulfate, manganese nitrate, manganese chloride or manganese acetate.
Described oxidant is potassium chlorate, potassium permanganate or persulfate.
Described solvent is ultra-pure water or alcohol.
Described acid is hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, acetic acid, formic acid, benzoic acid or tartaric inorganic and organic acid, and the pH value of acid is 0 ~ 7.
Described organic monomer is the polymer monomer that In-situ reaction can occur.
Described polymer monomer is pyrroles, aniline, thiophene or dopamine.
In described step 3, inert gas is nitrogen, argon gas or helium.
Beneficial effect
The preparation method of a kind of self-supporting lithium ion battery negative material that the present invention proposes, adopts hydro thermal method to prepare overlength one dimension manganese dioxide (U-MnO manganese salt, oxidant and solvent
2) nano wire, by U-MnO
2to be scattered in acid solution and to add appropriate organic monomer, obtained U-MnO
2@High polymer compounds, obtains self-supported membrane through cleaning, suction filtration, drying, obtains the coated MnO of self-supporting carbon (MnO@C) electrode material after high-temperature heat treatment.The MnO@C for preparing of the method can directly as the negative material of lithium ion battery, without the need to extra collector, conductive additive and binding agent.This material has that preparation technology is simple, structural stability is high, from the feature such as afflux, excellent electrochemical performance.
Beneficial effect of the present invention: 1, carbon coated employing in-situ oxidizing-polymerizing technology, can the MnO of even coated different structure
2, technique is simple, technology is by force portable.2, electrode material of the present invention has self-supporting, and electrode production process is simple, without the need to extra collector, conductive additive and binding agent.3, U-MnO@C electrode material of the present invention is overlength one-dimensional nano structure, and mechanical stability is high, and electron conduction ability is strong, has the chemical property advantages such as Large Copacity, high-rate characteristics, long circulation life, have a extensive future as lithium ion cell electrode.
Accompanying drawing explanation
Fig. 1 is inventive method preparation process schematic diagram;
Fig. 2 is the U-MnO that invention step 1 is prepared
2: (a) initial pattern, the pattern after (b) doubling twice;
Fig. 3 is the scanning electron microscopic picture of electrode material in the present invention: (a) U-MnO
2, (b) MnO@C;
Fig. 4 is the chemical property contrast figure of overlength MnO@C and the pure overlength MnO adopting preparation method of the present invention to obtain.Abscissa represents cycle-index, and ordinate represents charge/discharge capacity, and current density is 100mA/g, is lithium metal to electrode.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1
1) taking 4mmol manganese sulfate, 6mmol potassium chlorate, 7mmol potassium acetate and 4mL acetic acid adds in the deionized water of 60mL, after abundant stirring and dissolving, the capacity that proceeded to by solution is in the water heating kettle of 100mL, water heating kettle is put into drying box and be heated to 160 DEG C of insulation 12h, naturally cool to room temperature after hydro-thermal reaction, obtain U-MnO
2, use deionized water and absolute ethyl alcohol respectively to clean 3 times, the U-MnO that suction filtration obtains
2self-supported membrane is dry 24h at 90 DEG C, self-supported membrane picture as shown in Figure 1, wherein (a) for diameter be the self-supported membrane of 50mm, (b) is the picture after self-supported membrane doubling twice, and it has higher mechanical strength and toughness as seen.U-MnO
2scanning electron microscopic picture as shown in accompanying drawing 2 (a);
2) 200mg step 1 is taken) U-MnO for preparing
2, joined in 20mL 0.1M HCl, stirred, added 60 μ L pyrroles subsequently, leave standstill reaction 4h after stirring at room temperature 30min, obtain U-MnO
2@polypyrrole, uses deionized water and absolute ethyl alcohol respectively to clean 3 times, suction filtration film forming and at 60 DEG C vacuumize 12h;
3) by step 2) U-MnO for preparing
2@polypyrrole, puts into tube furnace, under Ar (80sccm) protective atmosphere; 2h is incubated after being warming up to 600 DEG C by the heating rate of 5 DEG C/min; be cooled to room temperature, obtain MnO@C self-supported membrane, corresponding scanning electron microscopic picture is shown in accompanying drawing 2 (b).MnO@C material is directly assembled into lithium ion battery as negative pole, accompanying drawing 3 is the cyclical stability of this material under the current density of 100mA/g after 100 circulations, can see after 100 circulations, the specific capacity of material reaches 860mAh/g, far above pure MnO capacity under the same conditions, also show this material simultaneously and there is excellent cyclical stability.
Embodiment 2
1) 20mmol manganese sulfate is taken and 20mmol ammonium persulfate adds in the deionized water of 80mL, stir, add 50mmol ammonium sulfate subsequently, after stirring 30min, the capacity that proceeded to by solution is in the water heating kettle of 100mL, water heating kettle is put into drying box and be heated to 180 DEG C of insulation 12h, naturally cool to room temperature after hydro-thermal reaction, obtain U-MnO
2.Ultra-pure water and absolute ethyl alcohol is used respectively to clean 3 times, the U-MnO that suction filtration obtains
2self-supported membrane is dry 24h at 90 DEG C;
2) 200mg step 1 is taken) U-MnO for preparing
2, joined in 20mL 0.1M HCl, stirred, added 60 μ L pyrroles subsequently, leave standstill 4h after stirring at room temperature 30min, obtain U-MnO
2@polypyrrole, uses ultra-pure water and washes of absolute alcohol 3 times, suction filtration film forming, vacuumize 12h at 60 DEG C;
3) by step 2) U-MnO for preparing
2@polypyrrole; put into tube furnace; under Ar (80sccm) protective atmosphere; 2h is incubated after being warming up to 600 DEG C by the heating rate of 5 DEG C/min; be cooled to room temperature; obtain MnO@C self-supported membrane, using MnO@C directly as negative material assembling lithium ion battery, under the current density of 500mA/g, after 100 circulations, specific capacity reaches 550mAh/g.
Embodiment 3
1) taking 6mmol manganese nitrate, 8mmol potassium chlorate, 8mmol potassium acetate and 4mL acetic acid adds in the ultra-pure water of 90mL, after abundant stirring and dissolving, the capacity that proceeded to by solution is in the water heating kettle of 100mL, water heating kettle is proceeded in drying box and be heated to 160 DEG C of insulation 16h, naturally cool to room temperature after hydro-thermal reaction, obtain U-MnO
2, use ultra-pure water and absolute ethyl alcohol respectively to clean 3 times, the U-MnO that suction filtration obtains
2self-supported membrane is forced air drying 48h at 90 DEG C;
2) 200mg step 1 is taken) U-MnO for preparing
2, joined 40mL 0.1M HNO
3in, stir, add 80 μ L thiophene subsequently, leave standstill reaction 4h after stirring at room temperature 60min, obtain U-MnO
2@polythiophene, uses ultra-pure water and washes of absolute alcohol 3 times, suction filtration film forming and at 60 DEG C vacuumize 24h;
3) by step 2) U-MnO for preparing
2@polythiophene, puts into tube furnace, at N
2(120sccm) in atmosphere, 2h is incubated after being warming up to 700 DEG C by the heating rate of 5 DEG C/min, be cooled to room temperature, obtain MnO@C self-supported membrane, using MnO@C directly as negative material assembling lithium ion battery, under the current density of 500mA/g, after 100 circulations, specific capacity reaches 650mAh/g.
Embodiment 4
1) taking 4mmol manganese sulfate, 8mmol potassium chlorate, 8mmol potassium acetate and 6mL acetic acid adds in 80mL ultra-pure water, after abundant stirring and dissolving, the capacity that proceeded to by solution is in the water heating kettle of 100mL, water heating kettle is proceeded in drying box and be heated to 160 DEG C of insulation 16h, naturally cool to room temperature after hydro-thermal reaction, obtain U-MnO
2, use ultra-pure water and absolute ethyl alcohol respectively to clean 3 times, the U-MnO that suction filtration obtains
2self-supported membrane is forced air drying 24h at 90 DEG C;
2) 200mg step 1 is taken) U-MnO for preparing
2, joined in 20mL 0.5M HCl, stirred, added 60 μ L aniline subsequently, leave standstill reaction 2h after stirring at room temperature 30min, obtain U-MnO
2@polyaniline, uses ultra-pure water and washes of absolute alcohol 3 times, suction filtration film forming, vacuumize 24h at 60 DEG C;
3) by step 2) U-MnO for preparing
2@polyaniline, put into tube furnace, in vacuum atmosphere, 2h is incubated after being warming up to 500 DEG C by the heating rate of 5 DEG C/min, be cooled to room temperature, obtain MnO@C self-supported membrane, using MnO@C directly as negative material assembling lithium ion battery, under 500mA/g current density, after 100 circulations, specific capacity reaches 520mAh/g.
Embodiment 5
1) taking 4mmol manganese chloride, 6mmol potassium chlorate, 10mmol potassium acetate and 2mL concentrated hydrochloric acid adds in 80mL ultra-pure water, after abundant stirring and dissolving, the capacity that proceeded to by solution is in the water heating kettle of 100mL, water heating kettle is proceeded in drying box and be heated to 160 DEG C of insulation 24h, naturally cool to room temperature after hydro-thermal reaction, obtain U-MnO
2, use ultra-pure water and absolute ethyl alcohol respectively to clean 3 times, take out the U-MnO obtained
2self-supported membrane is forced air drying 24h at 90 DEG C;
2) 200mg step 1 is taken) U-MnO for preparing
2, joined in 20mL 1M HCl, stir, add 60 μ L pyrroles subsequently, low temperature (5 ~ 10 DEG C) stirs 60min, leaves standstill reaction 2h, obtains U-MnO
2@polypyrrole, uses ultra-pure water and washes of absolute alcohol 3 times, suction filtration film forming, vacuumize 12h at 60 DEG C;
3) by step 2) U-MnO for preparing
2@polypyrrole, put into tube furnace, in Ar (80sccm) atmosphere, 2h is incubated after being warming up to 500 DEG C by the heating rate of 5 DEG C/min, be cooled to room temperature, obtain MnO@C self-supported membrane, using MnO@C directly as negative material assembling lithium ion battery, under 500mA/g current density, after 100 circulations, specific capacity reaches 608mAh/g.
Claims (8)
1. a preparation method for self-supporting lithium ion battery negative material, is characterized in that step is as follows:
Step 1: by manganese salt and the oxidant raw material mixed in molar ratio according to 0.5 ~ 5 ︰ 1, adopts solvent to make solution, utilizes hydro thermal method to prepare overlength one dimension manganese dioxide U-MnO
2nano wire; The hydrothermal temperature of described hydro thermal method is 110 ~ 260 DEG C, and the hydro-thermal time is >6h;
Step 2: by U-MnO
2, acid and organic monomer according to the mixed in molar ratio of 1 ~ 5 ︰ 1 ︰ 1, be obtained by reacting the coated MnO of high polymer through original position Interface composites
2, be MnO
2@high polymer, obtains MnO through cleaning, drying, suction filtration
2@high-polymer membrane;
Step 3: by MnO
2@high-polymer membrane is placed in atmosphere furnace carbonization, obtains the carbon coated manganese oxide film MnO@C with self-supporting characteristic; Described heat treatment temperature when being placed in atmosphere furnace carbonization is 400 ~ 1500 DEG C, and heat treatment time is 0.5 ~ 12h, and heat-treating atmosphere is inert gas shielding or vacuum protection.
2. the preparation method of self-supporting lithium ion battery negative material according to claim 1, is characterized in that: described manganese salt is manganese sulfate, manganese nitrate, manganese chloride or manganese acetate.
3. the preparation method of self-supporting lithium ion battery negative material according to claim 1, is characterized in that: described oxidant is potassium chlorate, potassium permanganate or persulfate.
4. the preparation method of self-supporting lithium ion battery negative material according to claim 1, is characterized in that: described solvent is ultra-pure water or alcohol.
5. the preparation method of self-supporting lithium ion battery negative material according to claim 1, is characterized in that: described acid is hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, acetic acid, formic acid, benzoic acid or tartaric inorganic and organic acid, and the pH value of acid is 0 ~ 7.
6. the preparation method of self-supporting lithium ion battery negative material according to claim 1, is characterized in that: described organic monomer is the polymer monomer that In-situ reaction can occur.
7. the preparation method of self-supporting lithium ion battery negative material according to claim 1, is characterized in that: described polymer monomer is pyrroles, aniline, thiophene or dopamine.
8. the preparation method of self-supporting lithium ion battery negative material according to claim 1, is characterized in that: in described step 3, inert gas is nitrogen, argon gas or helium.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105355893A (en) * | 2015-12-16 | 2016-02-24 | 西北工业大学 | Preparation method of flexible lithium ion battery negative material |
| CN105470481A (en) * | 2015-11-30 | 2016-04-06 | 武汉理工大学 | Nitrogen-doped carbon-coated manganese monoxide composite material with one-dimensional porous core-shell structure and preparation method of nitrogen-doped carbon-coated manganese monoxide composite material |
| CN105552342A (en) * | 2016-02-18 | 2016-05-04 | 长春理工大学 | Flexible negative electrode with MnO2 attached onto carbon fiber of lithium ion battery and preparation method of flexible negative electrode |
| CN106206065A (en) * | 2016-09-14 | 2016-12-07 | 安徽师范大学 | A kind of electrode material for super capacitor MnO2the preparation method of@PDA nano composite material |
| CN106672935A (en) * | 2016-12-26 | 2017-05-17 | 西北工业大学 | Preparation method of nitrogen-doped hollow porous carbon |
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| CN107492648A (en) * | 2017-08-18 | 2017-12-19 | 湖北文理学院 | Cotton base carbon fibre/MnO/C materials, preparation method and application |
| CN108134057A (en) * | 2017-12-05 | 2018-06-08 | 西北工业大学 | A kind of preparation method of high-tap density MnO/C negative materials |
| CN110061209A (en) * | 2019-04-03 | 2019-07-26 | 合肥国轩高科动力能源有限公司 | A kind of MnO2@V2O5Core-shell nano material and preparation method thereof, application |
| CN113086967A (en) * | 2021-04-12 | 2021-07-09 | 北京化工大学 | Preparation method of uniform carbon-manganese oxide composite aerogel electrode material |
| CN113823777A (en) * | 2021-08-11 | 2021-12-21 | 中国地质大学（武汉） | Porous nitrogen-doped carbon coaxial coating manganese dioxide nanotube and preparation method and application thereof |
| CN114639819A (en) * | 2022-03-24 | 2022-06-17 | 中南大学 | Sodium-rich manganese-based oxide composite substrate metal oxide self-supporting binary anode material and preparation method thereof |
| RU2790818C1 (en) * | 2022-05-12 | 2023-02-28 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method for producing a manganese monoxide/carbon composite |
| WO2024087567A1 (en) * | 2022-10-28 | 2024-05-02 | 安徽科技学院 | Nitrogen-doped carbon-film-coated manganese monoxide nanowire lithium battery material and preparation method therefor |
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| CN105470481A (en) * | 2015-11-30 | 2016-04-06 | 武汉理工大学 | Nitrogen-doped carbon-coated manganese monoxide composite material with one-dimensional porous core-shell structure and preparation method of nitrogen-doped carbon-coated manganese monoxide composite material |
| CN105355893A (en) * | 2015-12-16 | 2016-02-24 | 西北工业大学 | Preparation method of flexible lithium ion battery negative material |
| CN105552342A (en) * | 2016-02-18 | 2016-05-04 | 长春理工大学 | Flexible negative electrode with MnO2 attached onto carbon fiber of lithium ion battery and preparation method of flexible negative electrode |
| CN106206065B (en) * | 2016-09-14 | 2018-11-13 | 安徽师范大学 | A kind of electrode material for super capacitor MnO2The preparation method of@PDA nanocomposites |
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| CN106672935A (en) * | 2016-12-26 | 2017-05-17 | 西北工业大学 | Preparation method of nitrogen-doped hollow porous carbon |
| CN106824290A (en) * | 2017-03-03 | 2017-06-13 | 哈尔滨工业大学 | A kind of preparation method of overstable self-supporting manganese dioxide membrane for water treatment |
| CN106824290B (en) * | 2017-03-03 | 2020-08-21 | 哈尔滨工业大学 | Preparation method of ultra-stable self-supporting manganese dioxide water treatment membrane |
| CN107492648A (en) * | 2017-08-18 | 2017-12-19 | 湖北文理学院 | Cotton base carbon fibre/MnO/C materials, preparation method and application |
| CN108134057A (en) * | 2017-12-05 | 2018-06-08 | 西北工业大学 | A kind of preparation method of high-tap density MnO/C negative materials |
| CN110061209A (en) * | 2019-04-03 | 2019-07-26 | 合肥国轩高科动力能源有限公司 | A kind of MnO2@V2O5Core-shell nano material and preparation method thereof, application |
| CN110061209B (en) * | 2019-04-03 | 2022-03-04 | 合肥国轩高科动力能源有限公司 | MnO (MnO)2@V2O5Core-shell nano material and preparation method and application thereof |
| CN113086967A (en) * | 2021-04-12 | 2021-07-09 | 北京化工大学 | Preparation method of uniform carbon-manganese oxide composite aerogel electrode material |
| CN113823777A (en) * | 2021-08-11 | 2021-12-21 | 中国地质大学（武汉） | Porous nitrogen-doped carbon coaxial coating manganese dioxide nanotube and preparation method and application thereof |
| CN114639819A (en) * | 2022-03-24 | 2022-06-17 | 中南大学 | Sodium-rich manganese-based oxide composite substrate metal oxide self-supporting binary anode material and preparation method thereof |
| CN114639819B (en) * | 2022-03-24 | 2024-01-30 | 中南大学 | Sodium-rich manganese-based oxide composite substrate metal oxide self-supporting binary anode material and preparation method thereof |
| RU2790818C1 (en) * | 2022-05-12 | 2023-02-28 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method for producing a manganese monoxide/carbon composite |
| WO2024087567A1 (en) * | 2022-10-28 | 2024-05-02 | 安徽科技学院 | Nitrogen-doped carbon-film-coated manganese monoxide nanowire lithium battery material and preparation method therefor |
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