CN107123794B - 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 PDF

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CN107123794B
CN107123794B CN201710318940.9A CN201710318940A CN107123794B CN 107123794 B CN107123794 B CN 107123794B CN 201710318940 A CN201710318940 A CN 201710318940A CN 107123794 B CN107123794 B CN 107123794B
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graphene
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lithium ion
mno
carbon coating
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CN107123794A (en
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曹丽云
王瑞谊
许占位
李嘉胤
黄剑锋
李瑞梓
李康
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Shaanxi University of Science and Technology
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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
    • 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
    • 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
    • H01M4/502—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese for non-aqueous cells
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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

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 in redox graphene on 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 is improved to the electric conductivity of the difference of MnO in this synthetic method, and MnO particle is uniformly dispersed on the surface of graphene, second of hydro-thermal is evenly coated ground carbon-coating in MnO particle surface, carbon shell is as an elasticity limitation body, it can prevent the aggregation and dusting of MnO particle in charge and discharge process, the buffer area of one volume expansion is provided, its cyclical stability as lithium ion battery is largely improved.

Description

A kind of carbon coating manganese monoxide/N doping redox graphene lithium ion battery is negative The preparation method of pole material
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 electrode material.
Background technique
In order to meet growing high energy consumption and high power density requirements, transition metal oxide Fe3O4、CoO、 Due to high theoretical specific capacity, advantages of environment protection is widely investigated as the negative of lithium ion battery by NiO, CuO and ZnO etc. Pole material.Wherein, manganese monoxide has suitable electromotive force (< 0.8V) and high energy density, it is considered to be most prospect One of negative electrode material.But correspondingly there is also some disadvantages, such as poorly conductive, volume expansion is big, structural instability etc.. Correspondingly there is also some measures, for example preparing the Mn oxide of porous structure includes: the nano stick of 1D, hollow nanometer Pipe, 2D nanometer sheet, the nanostructure substance etc. of the porous layering of 3D, or prepare oxide/C compound or doping；Because The elastic property of carbon-based material can provide a buffering effect to cope with the variation of volume, and can increase composite material 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.]。
Doping type manganese monoxide/carbon complex method for preparing common at present is two-step method.Wherein the first step includes water Thermal method, water-bath/bath oiling and low-temperature co-precipitation method.Second step is then mostly heat treatment process.Zhao et al. with potassium permanganate and Graphene oxide is raw material, brings it about the compound that redox reaction is prepared for manganese dioxide and graphene oxide first, Then heat treatment has obtained the compound of manganese monoxide and graphene oxide under an argon atmosphere.The product is in 100mA g-1Electric current Under density, 90 circle specific discharge capacity of circulation is 900mA h g-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 restores Mn using the reproducibility of graphene oxide4+, the amount consumption of graphene oxide is compared Greatly, a degree of waste is caused.
Summary of the invention
The object of the present invention is to provide a kind of short preparation period, safety and stability, and the combination electrode material prepared is significantly The electric conductivity for improving MnO improves the excellent carbon coating manganese monoxide/N doping of its large volume bulking effect cycle performance The preparation method of redox graphene lithium ion battery negative material.
For achieving the above object, specific technical solution is as follows:
1) manganese acetate is added to the water stir evenly at room temperature be configured to mass fraction be 2.5%-8.5% manganese acetate it is molten Liquid；
2) graphene oxide of 30-100mg is taken to be added in the acetic acid manganese solution of 40-70ml, stirring, ultrasonic disperse are uniform Obtain mixture；
3) the resulting mixture of step 2) is transferred in reaction kettle, carries out microwave hydrothermal reaction；
4) product by the resulting microwave hydrothermal reaction of step 3) is uniformly mixed with 1.2-3.5g sucrose, is transferred to polytetrafluoro Hydro-thermal reaction in ethylene reaction kettle；
5) hydro-thermal reaction product obtained by step 4) is filtered, washed, dried；
6) pattern that solid is obtained after being heat-treated the resulting product of step 5) in atmosphere furnace is graininess, and size is The MnO of 100nm has been supported on graphene film, and the surface MnO has coated equably carbon-coating.
The stirring of the step 2) and ultrasound are alternately.
Step 2) the ultrasonic power is 60-100W, and ultrasonic number is 3-7 times, and ultrasonic time is each 1h.
Step 3) the microwave hydrothermal reaction temperature is 120 DEG C -200 DEG C, reaction time 1-3h.
The temperature of hydro-thermal reaction in the step 4) is 150-180 DEG C, reaction time 12-24h.
Washing in the step 5) is alternately washed using deionized water, dehydrated alcohol and acetone.
Atmosphere in the step 6) is the mixed atmosphere that argon gas and ammonia are mixed by the volume ratio of 95:5.
Step 6) the heat treatment temperature is 500-800 DEG C, time 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 Object is closed, it is heat-treated in atmosphere furnace after, carbon coating manganese monoxide particulate load has been prepared and has restored Graphene oxide on piece, while N doping is realized to graphene, it can be used as high performance lithium ionic cell cathode material.This synthesis First time hydro-thermal introduces graphene and is improved to the electric conductivity of the difference of MnO in method, and makes MnO particle in graphene table Face is uniformly dispersed, and second of hydro-thermal is evenly coated ground carbon-coating in MnO particle surface, and carbon shell, can be with as an elasticity limitation body The aggregation and dusting for preventing MnO particle in charge and discharge process, provide the buffer area of a volume expansion, largely improve Its cyclical stability as lithium ion battery.
Detailed description of the invention
Fig. 1 is SEM (scanning electron microscope) figure (times magnification of C@MnO/NRGO lithium ion battery negative material prepared by the present invention 50,000 times of number).
Fig. 2 is TEM (transmission electron microscope) figure (times magnification of C@MnO/NRGO lithium ion battery negative material prepared by the present invention Number 500nm).
Fig. 3 is XRD (X-ray diffraction) figure of C@MnO/NRGO lithium ion battery negative material prepared by the present invention.
Fig. 4 is the cyclical stability figure of C@MnO/NRGO negative electrode of lithium ion battery material prepared by the present invention.
Specific embodiment
Embodiment 1:
1) manganese acetate is added to the water to stir evenly at room temperature and is configured to the acetic acid manganese solution that mass fraction is 2.5%；
2) graphene oxide of 30mg is taken to be added in the acetic acid manganese solution of 40ml, ultrasound 1h is handed under stirring and 60W power For progress 3 times, it is uniformly dispersed；
3) the resulting mixture of step 2) is transferred in reaction kettle, 120 DEG C of progress microwave hydrothermals react 1h；
4) product by the resulting microwave hydrothermal reaction of step 3) is uniformly mixed with 1.2g sucrose, is transferred to polytetrafluoroethylene (PTFE) 150 DEG C of hydro-thermal reaction 12h in reaction kettle；
5) hydro-thermal reaction product obtained by step 4) is filtered, is alternately washed using ethyl alcohol, deionized water, acetone, is dry It is dry；
6) by the resulting product of step 5) 500 DEG C in the mixed atmosphere furnace that argon gas and ammonia are mixed by the volume ratio of 95:5 The pattern that solid is obtained after heat treatment 2h heat treatment is that graininess MnO has been supported on graphene film, and size is the MnO of 100nm It has been supported on graphene film, and the surface MnO has coated 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 particle is grown on graphene film, and MnO particle surface has 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 is preferable as illustrating for lithium ion battery negative material Cyclical stability, first discharge specific capacity are 1022mAh g-1, 30 circle after reversible specific capacity be 899mAh g-1, decaying is slowly.
Embodiment 2:
1) manganese acetate is added to the water to stir evenly at room temperature and is configured to the acetic acid manganese solution that mass fraction is 3.5%；
2) graphene oxide of 30mg is taken to be added in the acetic acid manganese solution of 50ml, ultrasound 1h is handed under stirring and 70W power For progress 4 times, it is uniformly dispersed；
3) the resulting mixture of step 2) is transferred in reaction kettle, 150 DEG C of progress microwave hydrothermals react 2h；
4) product by the resulting microwave hydrothermal reaction of step 3) is uniformly mixed with 2.0g sucrose, is transferred to polytetrafluoroethylene (PTFE) 180 DEG C of hydro-thermal reaction 16h in reaction kettle；
5) hydro-thermal reaction product obtained by step 4) is filtered, is alternately washed using ethyl alcohol, deionized water, acetone, is dry It is dry；
6) by the resulting product of step 5) 600 DEG C in the mixed atmosphere furnace that argon gas and ammonia are mixed by the volume ratio of 95:5 The pattern that solid is obtained after heat treatment 1h heat treatment is that graininess MnO has been supported on graphene film, and size is the MnO of 100nm It has been supported on graphene film, and the surface MnO has coated equably carbon-coating.
Embodiment 3:
1) manganese acetate is added to the water to stir evenly at room temperature and is configured to the acetic acid manganese solution that mass fraction is 4.5%；
2) graphene oxide of 50mg is taken to be added in the acetic acid manganese solution of 45ml, ultrasound 1h is handed under stirring and 80W power For progress 5 times, it is uniformly dispersed；
3) the resulting mixture of step 2) is transferred in reaction kettle, 180 DEG C of progress microwave hydrothermals react 3h；
4) product by the resulting microwave hydrothermal reaction of step 3) is uniformly mixed with 2.5g sucrose, is transferred to polytetrafluoroethylene (PTFE) 180 DEG C of hydro-thermal reaction 18h in reaction kettle；
5) hydro-thermal reaction product obtained by step 4) is filtered, is alternately washed using ethyl alcohol, deionized water, acetone, is dry It is dry；
6) by the resulting product of step 5) 700 DEG C in the mixed atmosphere furnace that argon gas and ammonia are mixed by the volume ratio of 95:5 The pattern that solid is obtained after heat treatment 3h heat treatment is that graininess MnO has been supported on graphene film, and size is the MnO of 100nm It has been supported on graphene film, and the surface MnO has coated equably carbon-coating.
Embodiment 4:
1) manganese acetate is added to the water to stir evenly at room temperature and is configured to the acetic acid manganese solution that mass fraction is 5.5%；
2) graphene oxide of 80mg is taken to be added in the acetic acid manganese solution of 65ml, ultrasound 1h is handed under stirring and 90W power For progress 6 times, it is uniformly dispersed；
3) the resulting mixture of step 2) is transferred in reaction kettle, 200 DEG C of progress microwave hydrothermals react 2h；
4) product by the resulting microwave hydrothermal reaction of step 3) is uniformly mixed with 3g sucrose, and it is anti-to be transferred to polytetrafluoroethylene (PTFE) Answer 190 DEG C of hydro-thermal reaction 20h in kettle；
5) hydro-thermal reaction product obtained by step 4) is filtered, is alternately washed using ethyl alcohol, deionized water, acetone, is dry It is dry；
6) by the resulting product of step 5) 800 DEG C in the mixed atmosphere furnace that argon gas and ammonia are mixed by the volume ratio of 95:5 The pattern that solid is obtained after heat treatment 2h heat treatment is that graininess MnO has been supported on graphene film, and size is the MnO of 100nm It has been supported on graphene film, and the surface MnO has coated equably carbon-coating.
Embodiment 5:
1) manganese acetate is added to the water to stir evenly at room temperature and is configured to the acetic acid manganese solution that mass fraction is 7.5%；
2) graphene oxide of 70mg is taken to be added in the acetic acid manganese solution of 60ml, ultrasound 1h is handed under stirring and 100W power For progress 7 times, it is uniformly dispersed；
3) the resulting mixture of step 2) is transferred in reaction kettle, 120 DEG C of progress microwave hydrothermals react 1h；
4) product by the resulting microwave hydrothermal reaction of step 3) is uniformly mixed with 3.5g sucrose, is transferred to polytetrafluoroethylene (PTFE) 150 DEG C of hydro-thermal reactions are for 24 hours in reaction kettle；
5) hydro-thermal reaction product obtained by step 4) is filtered, is alternately washed using ethyl alcohol, deionized water, acetone, is dry It is dry；
6) by the resulting product of step 5) 600 DEG C in the mixed atmosphere furnace that argon gas and ammonia are mixed by the volume ratio of 95:5 The pattern that solid is obtained after heat treatment 4h heat treatment is that graininess MnO has been supported on graphene film, and size is the MnO of 100nm It has been supported on graphene film, and the surface MnO has coated equably carbon-coating.
Embodiment 6:
1) manganese acetate is added to the water to stir evenly at room temperature and is configured to the acetic acid manganese solution that mass fraction is 8.5%；
2) graphene oxide of 100mg is taken to be added in the acetic acid manganese solution of 70ml, ultrasound 1h is handed under stirring and 70W power For progress 5 times, it is uniformly dispersed；
3) the resulting mixture of step 2) is transferred in reaction kettle, 150 DEG C of progress microwave hydrothermals react 2h；
4) product by the resulting microwave hydrothermal reaction of step 3) is uniformly mixed with 2.0g sucrose, is transferred to polytetrafluoroethylene (PTFE) 180 DEG C of hydro-thermal reaction 15h in reaction kettle；
5) hydro-thermal reaction product obtained by step 4) is filtered, is alternately washed using ethyl alcohol, deionized water, acetone, is dry It is dry；
6) by the resulting product of step 5) 700 DEG C in the mixed atmosphere furnace that argon gas and ammonia are mixed by the volume ratio of 95:5 The pattern that solid is obtained after heat treatment 5h heat treatment is that graininess MnO has been supported on graphene film, and size is the MnO of 100nm It has been supported on graphene film, and the surface MnO has coated equably carbon-coating.

Claims (5)

1. a kind of carbon coating manganese monoxide/N doping redox graphene lithium ion battery negative material preparation method, It is characterized in that specific step is as follows:
1) manganese acetate is added to the water to the acetic acid manganese solution for stirring evenly be configured to that mass fraction is 2.5%-8.5% at room temperature；
2) graphene oxide of 30-100mg is taken to be added in the acetic acid manganese solution of 40-70ml, stirring, ultrasonic disperse is uniform to mix Close object；
3) the resulting mixture of step 2) is transferred in reaction kettle, carries out microwave hydrothermal reaction；
4) product by the resulting microwave hydrothermal reaction of step 3) is uniformly mixed with 1.2-3.5g sucrose, is transferred to polytetrafluoroethylene (PTFE) Hydro-thermal reaction in reaction kettle；
5) hydro-thermal reaction product obtained by step 4) is filtered, washed, dried；
6) pattern that solid is obtained after being heat-treated the resulting product of step 5) in atmosphere furnace is graininess, size 100nm MnO be supported on graphene film, and the surface MnO has coated uniform carbon-coating；
Washing in the step 5) is alternately washed using deionized water, dehydrated alcohol and acetone；
Atmosphere in the step 6) is the mixed atmosphere that argon gas and ammonia are mixed by the volume ratio of 95:5；
Step 6) the heat treatment temperature is 500-800 DEG C, time 1-5h.
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 stirring of the step 2) and ultrasound are 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 is 60-100 W, and ultrasonic number is 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: step 3) the microwave hydrothermal reaction temperature is 120 DEG C -200 DEG C, reaction time 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 temperature of the hydro-thermal reaction in the step 4) is 150-180 DEG C, reaction time 12- 24h。
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IT201800010540A1 (en) 2018-11-23 2020-05-23 Torino Politecnico Reduced and doped graphene oxide, and its production method
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
CN110237835B (en) * 2019-06-12 2020-06-19 西安交通大学 Titanium dioxide-tin dioxide-graphene composite photocatalyst and preparation method thereof
CN110783539B (en) * 2019-09-30 2022-06-07 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
CN114976062B (en) * 2020-10-15 2024-01-26 昆明理工大学 Preparation method of nitrogen-doped rGO loaded MnO nanoparticle catalyst
CN113097484B (en) * 2021-04-01 2023-04-28 陕西科技大学 Carbon-coated sandwich-like structure SnSe/r-GO@C compound and preparation method and application thereof

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