CN107123794A - A kind of preparation method of carbon coating manganese monoxide/N doping redox graphene lithium ion battery negative material - Google Patents
A kind of preparation method of carbon coating manganese monoxide/N doping redox graphene lithium ion battery negative material Download PDFInfo
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- CN107123794A CN107123794A CN201710318940.9A CN201710318940A CN107123794A CN 107123794 A CN107123794 A CN 107123794A CN 201710318940 A CN201710318940 A CN 201710318940A CN 107123794 A CN107123794 A CN 107123794A
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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
- H01M4/36—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
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- 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
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- 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
- 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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- H—ELECTRICITY
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- 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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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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Abstract
A kind of preparation method of carbon coating manganese monoxide/N doping redox graphene lithium ion battery negative material.The present invention is using manganese acetate, graphene and sucrose as primary raw material, the compound of manganese carbonate and redox graphene is prepared using microwave-hydrothermal method first, then the compound of carbon coating manganese carbonate and redox graphene is made by conventional hydrothermal, it is heat-treated in atmosphere furnace after, carbon coating manganese monoxide particulate load has been prepared on redox graphene piece, N doping is realized to graphene simultaneously, can be used as high performance lithium ionic cell cathode material.First time hydro-thermal introduces graphene and MnO poor electric conductivity is improved in this synthetic method, and MnO particles are uniformly dispersed in graphenic surface, second of hydro-thermal is evenly coated ground carbon-coating in MnO particle surfaces, carbon shell limits body as an elasticity, the aggregation and efflorescence of MnO particles in charge and discharge process can be prevented, the buffer area of one volumetric expansion is provided, it is largely improved as the cyclical stability of lithium ion battery.
Description
Technical field
The invention belongs to field of lithium ion battery, and in particular to a kind of carbon coating manganese monoxide/N doping oxygen reduction fossil
The preparation method of black alkene (MnO/NRGO) negative material.
Background technology
In order to meet growing high energy consumption and high power density requirements, transition metal oxide Fe3O4、CoO、
NiO, CuO and ZnO etc. are due to high theoretical specific capacity, and advantages of environment protection is widely investigated as the negative of lithium ion battery
Pole material.Wherein, manganese monoxide have suitable electromotive force (<0.8V) and high energy density, it is considered to be most prospect
One of negative material.But correspondingly there is also some shortcomings, such as poorly conductive, volumetric expansion is big, structural instability etc..
Correspondingly there is also some measures, such as preparing the Mn oxide of loose structure includes：1D nano stick, hollow nanometer
Pipe, 2D nanometer sheets, the nanostructured material of the porous layerings of 3D etc., or prepare oxide/C compounds or doping；Because
The elastic performance of carbon-based material can provide a buffering effect to tackle the change of volume, and can also increase composite
Electric conductivity.[Qiu T,Wang J,Lu Y,et al.Facile fabrication of Chinese lantern-like
MnO@N-C:a high-performance anode material for lithium-ion batteries[J].Rsc
Advances,2014,4(44):23027-23035.]。
The method for preparing doping type manganese monoxide/carbon complex common at present is two-step method.Wherein the first step includes water
Hot method, water-bath/bath oiling and low-temperature co-precipitation method.Second step is mostly then heat treatment process.Zhao et al. with potassium permanganate and
Graphene oxide is raw material, and the compound that redox reaction is prepared for manganese dioxide and graphene oxide is brought it about first,
The compound of manganese monoxide and graphene oxide has then been thermally treated resulting under an argon atmosphere.The product is in 100mA g-1Electric current
Under density, it is 900mA h g that specific discharge capacity is enclosed in circulation 90-1。[Zhao G,Huang X,Wang X,et al.Synthesis
and lithium-storage properties of MnO/reduced graphene oxide composites
derived from graphene oxide plus the transformation of Mn(VI)to Mn(II)by the
reducing power of graphene oxide[J].Journal of Materials Chemistry A,2014,3
(1):297-303.].The system reduces Mn using the reproducibility of graphene oxide4+, the consumption of the amount of graphene oxide is compared
Greatly, a certain degree of waste is caused.
The content of the invention
It is an object of the invention to provide a kind of short preparation period, safety and stability, and the combination electrode material prepared is significantly
MnO electric conductivity is improved, the excellent carbon coating manganese monoxide/N doping of its large volume bulking effect cycle performance is improved
The preparation method of redox graphene lithium ion battery negative material.
For achieving the above object, its specific technical scheme is as follows：
1) manganese acetate is added to the water stir at room temperature be configured to mass fraction be 2.5%-8.5% manganese acetate it is molten
Liquid；
2) 30-100mg graphene oxide is taken to be added in 40-70ml acetic acid manganese solution, stirring, ultrasonic disperse are uniform
Obtain mixture；
3) by step 2) obtained by mixture be transferred in reactor, carry out microwave hydrothermal reaction；
4) by step 3) obtained by microwave hydrothermal reaction product be well mixed with 1.2-3.5g sucrose, be transferred to polytetrafluoro
Hydro-thermal reaction in ethylene reaction kettle；
5) by step 4) gained hydro-thermal reaction product filtered, washed, drying；
6) by step 5) obtained by product be heat-treated in atmosphere furnace after to obtain the pattern of solid be graininess, size is
100nm MnO has been supported on graphene film, and MnO Surface coatings equably carbon-coating.
The step 2) stirring and ultrasound alternately.
The step 2) ultrasonic power be 60-100W, ultrasonic number of times be 3-7 time, ultrasonic time be each 1h.
The step 3) microwave hydrothermal reaction temperature be 120 DEG C -200 DEG C, the reaction time is 1-3h.
The step 4) in hydro-thermal reaction temperature be 150-180 DEG C, the reaction time is 12-24h.
The step 5) in washing alternately washed using deionized water, absolute ethyl alcohol and acetone.
The step 6) in atmosphere press 95 for argon gas and ammonia：The mixed atmosphere of 5 volume ratio mixing.
The step 6) heat treatment temperature be 500-800 DEG C, the time is 1-5h.
The present invention prepares manganese carbonate using microwave-hydrothermal method first using manganese acetate, graphene and sucrose as primary raw material
With the compound of redox graphene, answering for carbon coating manganese carbonate and redox graphene is then made by conventional hydrothermal
It, is heat-treated by compound after in atmosphere furnace, has prepared carbon coating manganese monoxide particulate load in reduction
On graphene oxide sheet, while realizing N doping to graphene, it can be used as high performance lithium ionic cell cathode material.This synthesis
First time hydro-thermal introduces graphene and MnO poor electric conductivity is improved in method, and causes MnO particles in graphene table
Face is uniformly dispersed, and second of hydro-thermal is evenly coated ground carbon-coating in MnO particle surfaces, and carbon shell limits body as an elasticity, can be with
Prevent the aggregation and efflorescence of MnO particles in charge and discharge process there is provided the buffer area of a volumetric expansion, largely improve
Its as lithium ion battery cyclical stability.
Brief description of the drawings
SEM (ESEM) figure (times magnification for the C@MnO/NRGO lithium ion battery negative materials that Fig. 1 is prepared for the present invention
50,000 times of number).
TEM (transmission electron microscope) figure (times magnification for the C@MnO/NRGO lithium ion battery negative materials that Fig. 2 is prepared for the present invention
Number 500nm).
XRD (X-ray diffraction) figure for the C@MnO/NRGO lithium ion battery negative materials that Fig. 3 is prepared for the present invention.
The cyclical stability figure for the C@MnO/NRGO negative electrode of lithium ion battery material that Fig. 4 is prepared for the present invention.
Embodiment
Embodiment 1：
1) manganese acetate is added to the water to the acetic acid manganese solution for stirring be configured to that mass fraction is 2.5% at room temperature；
2) 30mg graphene oxide is taken to be added in 40ml acetic acid manganese solution, ultrasound 1h is handed under stirring and 60W power
For carrying out 3 times, it is uniformly dispersed；
3) by step 2) obtained by mixture be transferred in reactor, 120 DEG C carry out microwave hydrothermals reaction 1h；
4) by step 3) obtained by microwave hydrothermal reaction product be well mixed with 1.2g sucrose, be transferred to polytetrafluoroethylene (PTFE)
150 DEG C of hydro-thermal reaction 12h in reactor；
5) by step 4) gained hydro-thermal reaction product filtered, using ethanol, deionized water, acetone alternately washing, do
It is dry；
6) by step 5) obtained by product press 95 in argon gas and ammonia：500 DEG C in the mixed atmosphere stove of 5 volume ratio mixing
The pattern of solid is obtained after heat treatment 2h heat treatments to be supported on graphene film for graininess MnO, size is 100nm MnO
It has been supported on graphene film, and MnO Surface coatings equably carbon-coating.
It will be seen from figure 1 that preparing prepared product is presented graphene laminated structure.
Figure it is seen that MnO particles length is on graphene film, and MnO particle surfaces have coated carbon-coating, MnO
The size about 100nm. of grain
From figure 3, it can be seen that successfully having been prepared by the process of this two one-step hydrothermal and Post isothermal treatment pure
The MnO of hexagonal phase.
It can be seen from figure 4 that prepared C@MnO/NRGO illustrating preferably as lithium ion battery negative material
Cyclical stability, first discharge specific capacity is 1022mAh g-1, 30 circle after reversible specific capacity be 899mAh g-1, decay is slowly.
Embodiment 2：
1) manganese acetate is added to the water to the acetic acid manganese solution for stirring be configured to that mass fraction is 3.5% at room temperature；
2) 30mg graphene oxide is taken to be added in 50ml acetic acid manganese solution, ultrasound 1h is handed under stirring and 70W power
For carrying out 4 times, it is uniformly dispersed；
3) by step 2) obtained by mixture be transferred in reactor, 150 DEG C carry out microwave hydrothermals reaction 2h；
4) by step 3) obtained by microwave hydrothermal reaction product be well mixed with 2.0g sucrose, be transferred to polytetrafluoroethylene (PTFE)
180 DEG C of hydro-thermal reaction 16h in reactor；
5) by step 4) gained hydro-thermal reaction product filtered, using ethanol, deionized water, acetone alternately washing, do
It is dry；
6) by step 5) obtained by product press 95 in argon gas and ammonia：600 DEG C in the mixed atmosphere stove of 5 volume ratio mixing
The pattern of solid is obtained after heat treatment 1h heat treatments to be supported on graphene film for graininess MnO, size is 100nm MnO
It has been supported on graphene film, and MnO Surface coatings equably carbon-coating.
Embodiment 3：
1) manganese acetate is added to the water to the acetic acid manganese solution for stirring be configured to that mass fraction is 4.5% at room temperature；
2) 50mg graphene oxide is taken to be added in 45ml acetic acid manganese solution, ultrasound 1h is handed under stirring and 80W power
For carrying out 5 times, it is uniformly dispersed；
3) by step 2) obtained by mixture be transferred in reactor, 180 DEG C carry out microwave hydrothermals reaction 3h；
4) by step 3) obtained by microwave hydrothermal reaction product be well mixed with 2.5g sucrose, be transferred to polytetrafluoroethylene (PTFE)
180 DEG C of hydro-thermal reaction 18h in reactor；
5) by step 4) gained hydro-thermal reaction product filtered, using ethanol, deionized water, acetone alternately washing, do
It is dry；
6) by step 5) obtained by product press 95 in argon gas and ammonia：700 DEG C in the mixed atmosphere stove of 5 volume ratio mixing
The pattern of solid is obtained after heat treatment 3h heat treatments to be supported on graphene film for graininess MnO, size is 100nm MnO
It has been supported on graphene film, and MnO Surface coatings equably carbon-coating.
Embodiment 4：
1) manganese acetate is added to the water to the acetic acid manganese solution for stirring be configured to that mass fraction is 5.5% at room temperature；
2) 80mg graphene oxide is taken to be added in 65ml acetic acid manganese solution, ultrasound 1h is handed under stirring and 90W power
For carrying out 6 times, it is uniformly dispersed；
3) by step 2) obtained by mixture be transferred in reactor, 200 DEG C carry out microwave hydrothermals reaction 2h；
4) by step 3) obtained by microwave hydrothermal reaction product be well mixed with 3g sucrose, be transferred to polytetrafluoroethylene (PTFE) anti-
Answer 190 DEG C of hydro-thermal reaction 20h in kettle；
5) by step 4) gained hydro-thermal reaction product filtered, using ethanol, deionized water, acetone alternately washing, do
It is dry；
6) by step 5) obtained by product press 95 in argon gas and ammonia：800 DEG C in the mixed atmosphere stove of 5 volume ratio mixing
The pattern of solid is obtained after heat treatment 2h heat treatments to be supported on graphene film for graininess MnO, size is 100nm MnO
It has been supported on graphene film, and MnO Surface coatings equably carbon-coating.
Embodiment 5：
1) manganese acetate is added to the water to the acetic acid manganese solution for stirring be configured to that mass fraction is 7.5% at room temperature；
2) 70mg graphene oxide is taken to be added in 60ml acetic acid manganese solution, ultrasound 1h is handed under stirring and 100W power
For carrying out 7 times, it is uniformly dispersed；
3) by step 2) obtained by mixture be transferred in reactor, 120 DEG C carry out microwave hydrothermals reaction 1h；
4) by step 3) obtained by microwave hydrothermal reaction product be well mixed with 3.5g sucrose, be transferred to polytetrafluoroethylene (PTFE)
150 DEG C of hydro-thermal reaction 24h in reactor；
5) by step 4) gained hydro-thermal reaction product filtered, using ethanol, deionized water, acetone alternately washing, do
It is dry；
6) by step 5) obtained by product press 95 in argon gas and ammonia：600 DEG C in the mixed atmosphere stove of 5 volume ratio mixing
The pattern of solid is obtained after heat treatment 4h heat treatments to be supported on graphene film for graininess MnO, size is 100nm MnO
It has been supported on graphene film, and MnO Surface coatings equably carbon-coating.
Embodiment 6：
1) manganese acetate is added to the water to the acetic acid manganese solution for stirring be configured to that mass fraction is 8.5% at room temperature；
2) 100mg graphene oxide is taken to be added in 70ml acetic acid manganese solution, ultrasound 1h is handed under stirring and 70W power
For carrying out 5 times, it is uniformly dispersed；
3) by step 2) obtained by mixture be transferred in reactor, 150 DEG C carry out microwave hydrothermals reaction 2h；
4) by step 3) obtained by microwave hydrothermal reaction product be well mixed with 2.0g sucrose, be transferred to polytetrafluoroethylene (PTFE)
180 DEG C of hydro-thermal reaction 15h in reactor；
5) by step 4) gained hydro-thermal reaction product filtered, using ethanol, deionized water, acetone alternately washing, do
It is dry；
6) by step 5) obtained by product press 95 in argon gas and ammonia：700 DEG C in the mixed atmosphere stove of 5 volume ratio mixing
The pattern of solid is obtained after heat treatment 5h heat treatments to be supported on graphene film for graininess MnO, size is 100nm MnO
It has been supported on graphene film, and MnO Surface coatings equably carbon-coating.
Claims (8)
1. a kind of preparation method of carbon coating manganese monoxide/N doping redox graphene lithium ion battery negative material, its
It is characterised by comprising the following steps that：
1) manganese acetate is added to the water to the acetic acid manganese solution for stirring be configured to that mass fraction is 2.5%-8.5% at room temperature；
2) 30-100mg graphene oxide is taken to be added in 40-70ml acetic acid manganese solution, stirring, ultrasonic disperse is uniform to mix
Compound；
3) by step 2) obtained by mixture be transferred in reactor, carry out microwave hydrothermal reaction；
4) by step 3) obtained by microwave hydrothermal reaction product be well mixed with 1.2-3.5g sucrose, be transferred to polytetrafluoroethylene (PTFE)
Hydro-thermal reaction in reactor；
5) by step 4) gained hydro-thermal reaction product filtered, washed, drying；
6) by step 5) obtained by product be heat-treated in atmosphere furnace after obtain solid pattern be graininess, size is 100nm
MnO be supported on graphene film, and graininess MnO Surface coatings equably carbon-coating.
2. carbon coating manganese monoxide according to claim 1/N doping redox graphene negative electrode of lithium ion battery material
The preparation method of material, it is characterised in that：The step 2) stirring and ultrasound alternately.
3. carbon coating manganese monoxide according to claim 1/N doping redox graphene negative electrode of lithium ion battery material
The preparation method of material, it is characterised in that：The step 2) ultrasonic power be 60-100W, ultrasonic number of times be 3-7 times, ultrasonic time
For each 1h.
4. carbon coating manganese monoxide according to claim 1/N doping redox graphene negative electrode of lithium ion battery material
The preparation method of material, it is characterised in that：The step 3) microwave hydrothermal reaction temperature be 120 DEG C -200 DEG C, the reaction time is 1-
3h。
5. carbon coating manganese monoxide according to claim 1/N doping redox graphene negative electrode of lithium ion battery material
The preparation method of material, it is characterised in that：The step 4) in hydro-thermal reaction temperature be 150-180 DEG C, the reaction time is 12-
24h。
6. carbon coating manganese monoxide according to claim 1/N doping redox graphene negative electrode of lithium ion battery material
The preparation method of material, it is characterised in that：The step 5) in washing alternately washed using deionized water, absolute ethyl alcohol and acetone
Wash.
7. carbon coating manganese monoxide according to claim 1/N doping redox graphene negative electrode of lithium ion battery material
The preparation method of material, it is characterised in that：The step 6) in atmosphere press 95 for argon gas and ammonia：It is mixed that 5 volume ratio is mixed
Close atmosphere.
8. carbon coating manganese monoxide according to claim 1/N doping redox graphene negative electrode of lithium ion battery material
The preparation method of material, it is characterised in that：The step 6) heat treatment temperature be 500-800 DEG C, the time is 1-5h.
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Cited By (6)
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| CN109817948A (en) * | 2019-03-04 | 2019-05-28 | 河南师范大学 | A kind of preparation method of lithium ion battery carbon coating MnO/ crystalline flake graphite combination electrode material |
| CN110237835A (en) * | 2019-06-12 | 2019-09-17 | 西安交通大学 | A kind of titania-silica tin-graphite alkene composite photo-catalyst and preparation method thereof |
| CN110783539A (en) * | 2019-09-30 | 2020-02-11 | 合肥国轩高科动力能源有限公司 | Manganese oxide composite material of lithium ion battery and preparation method and application thereof |
| IT201800010540A1 (en) | 2018-11-23 | 2020-05-23 | Torino Politecnico | Reduced and doped graphene oxide, and its production method |
| CN113097484A (en) * | 2021-04-01 | 2021-07-09 | 陕西科技大学 | Carbon-coated sandwich structure SnSe/r-GO @ C compound and preparation method and application thereof |
| CN114976062A (en) * | 2020-10-15 | 2022-08-30 | 昆明理工大学 | Preparation method of nitrogen-doped rGO-supported MnO nanoparticle catalyst |
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| IT201800010540A1 (en) | 2018-11-23 | 2020-05-23 | Torino Politecnico | Reduced and doped graphene oxide, and its production method |
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| CN114976062A (en) * | 2020-10-15 | 2022-08-30 | 昆明理工大学 | Preparation method of nitrogen-doped rGO-supported MnO nanoparticle catalyst |
| CN114976062B (en) * | 2020-10-15 | 2024-01-26 | 昆明理工大学 | Preparation method of nitrogen-doped rGO loaded MnO nanoparticle catalyst |
| CN113097484A (en) * | 2021-04-01 | 2021-07-09 | 陕西科技大学 | Carbon-coated sandwich structure SnSe/r-GO @ C compound and preparation method and application thereof |
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