CN104600261B - Graphite/Mn3O4 composite material and preparation method and application thereof - Google Patents
Graphite/Mn3O4 composite material and preparation method and application thereof Download PDFInfo
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- CN104600261B CN104600261B CN201410853670.8A CN201410853670A CN104600261B CN 104600261 B CN104600261 B CN 104600261B CN 201410853670 A CN201410853670 A CN 201410853670A CN 104600261 B CN104600261 B CN 104600261B
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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
- H01M4/364—Composites as mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
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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
- H01M4/62—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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- 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
The invention discloses a graphite/Mn3O4 composite material and a preparation method and application thereof. The method comprises the following steps: (1) dissolving potassium permanganate and sodium sulfate in a mixed solvent consisting of water and ethanol, thereby obtaining a chemical plating solution; (2) adding artificial graphite into the chemical plating solution, stirring for 0.1-1 hour, standing and soaking for 0.1-2 hours, so that potassium permanganate is reduced into manganous-manganic oxide which is uniformly loaded on the surface of non-hydrophilic artificial graphite; filtering, washing, and drying, thereby obtaining the product; and (3) heating the obtained product to the temperature of 400-800 DEG C in a protective atmosphere, preserving the temperature for 2-8 hours, and cooling, thereby obtaining the graphite/Mn3O4 composite material. The prepared graphite/Mn3O4 composite material has the characteristics of high capacity, high conductivity, high cycling stability and the like and can serve as a lithium ion battery negative pole electrode to be applied to the field of high-capacity lithium ion batteries.
Description
Technical field
The present invention relates to cathode material of lithium ion battery field and in particular to a kind of graphite/Mn3O4 composite and its
Preparation method and the application as lithium ion battery negative material.
Background technology
Mangano-manganic oxide, as a kind of manganese series oxides material, has abundance, environmental friendliness, cheap, electrochemical
The features such as performance is good.It has higher theoretical specific capacity (936mAh/g) it is considered to be the most potential high power capacity
One of lithium ion battery negative material.However, mangano-manganic oxide is in actual applications, it mainly faces two problems：On the one hand,
The electrical conductivity of mangano-manganic oxide is low, leads to its high rate performance poor；On the other hand, during embedding lithium ionic insertion/deinsertion repeatedly, can go out
Now violent Volume Changes, thus causing material serious agglomeration and efflorescence, lead to its capacity rapid decay.These problems are seriously made
About commercial applications as lithium ion battery negative material for the mangano-manganic oxide.
Lithium ion battery negative mainly adopts graphite material.Although native graphite capacity is high, be easy to compacting, in circulation
During occur that lamella comes off, lead to cycle performance difference and safety problem.And Delanium has Stability Analysis of Structures, cycle performance
The features such as get well and have a safety feature, the always first-selection of lithium ion battery negative material.Delanium, also reduces specific surface
Long-pending, improve capacity, be a kind of preferable carbon negative pole material.But in actual use, carbon negative pole material because itself
Theoretical capacity is relatively low, and the space of lifting is very limited, is difficult to meet the high-energy-density density of a new generation, the lithium of high-specific-power density
The requirement of ion battery.
In recent years, domestic and international researcher finds to be combined preferable for electric conductivity material with carbon element with mangano-manganic oxide, can be effective
In conjunction with the advantage of mangano-manganic oxide high power capacity and material with carbon element high conductivity, solve mangano-manganic oxide capacity exhaustion and hold with material with carbon element soon
The not enough problem of amount.
Content of the invention
It is an object of the invention to provide a kind of graphite/Mn preparing high power capacity and good circulation stability3O4Composite
Method；And preparation cost is low, process is simple, suitable industrialized production.
The present invention first using adding a certain proportion of absolute ethyl alcohol to be made into solvent in water, using solution dipping method,
Ensure to overcome its hydrophobic problem while graphite-structure.This method process is simple, cost is relatively low, it is easy to accomplish industrial metaplasia
Produce.
For achieving the above object, the present invention adopts the following technical scheme that.
A kind of graphite/Mn3O4The preparation method of composite, comprises the following steps：
(1) potassium permanganate and sodium sulphate are dissolved in the mixed solvent being made up of water and ethanol, form chemical plating fluid；
(2) Delanium is added in chemical plating fluid, stir 0.1～1h, be standing and soak for 0.1～2h, make potassium permanganate also
Former become mangano-manganic oxide and uniform load is on the Delanium surface of non-hydrophilic, through filtering, washing, be dried after produced
Thing；
(3) product obtaining is warming up under protective atmosphere 400 DEG C～800 DEG C, is incubated 2～8h, cooling afterwards obtains
Graphite/Mn3O4Composite.
In step (1), in the described mixed solvent being made up of water and ethanol, the volume ratio of water and ethanol is 1～10：1,
Preferably 3～6：1.
In step (1), the mol ratio of described potassium permanganate and sodium sulphate is 2～0.2：1, preferably 1.2～0.8:1, institute
In the chemical plating fluid stated, the total concentration of potassium permanganate and sodium sulphate is 0.1～5mol/L.
In step (2), described Delanium is 0.1～3 with the mass ratio that feeds intake of potassium permanganate：1, preferably 0.2～1：
1.
In step (2), described protective atmosphere adopts nitrogen.
In step (3), it is warming up to 400～800 DEG C with the heating rate of 5～20 DEG C/min and is incubated 2～8h.Excellent further
Choosing, is warming up to 600 DEG C with the heating rate of 5 DEG C/min and is incubated 4～8h.
Present invention also offers graphite/Mn3O4Composite is as the application of lithium ion battery negative material.
By graphite/Mn3O4Composite can prepare lithium-ion electric as the negative material of lithium ion battery using existing method
The negative pole in pond, then obtains lithium ion battery by existing method assembling again.
Compared with prior art, the beneficial effects of the present invention is：
First, raw materials wide material sources, cheap it is easy to industrializing implementation；
2nd, mangano-manganic oxide is supported on graphite matrix the composite that the present invention is obtained, four oxidations not only improving
The electric conductivity of three manganese, introduces mangano-manganic oxide on graphite simultaneously, improves its reversible capacity.Obtained graphite/Mn3O4Multiple
Condensation material has the characteristics such as capacity height, good conductivity, cyclical stability height, particularly has preferable charging and discharging capacity and relatively
Good cycle performance, can apply in high-capacity lithium ion cell field as lithium ion battery negative material.
Brief description
Fig. 1 is the graphite/Mn prepared by embodiment 13O4The XRD diffraction pattern of composite；
Fig. 2 is the graphite/Mn prepared by embodiment 13O4The SEM photograph of composite；
Fig. 3 is the graphite/Mn prepared by embodiment 13O4The charging and discharging curve of composite；
Fig. 4 is the graphite/Mn prepared by embodiment 13O4The cycle performance curve of composite；
Fig. 5 is the graphite/Mn prepared by embodiment 13O4The high rate performance curve of composite；
Fig. 6 is the graphite/Mn prepared by embodiment 13O4The cyclic voltammetry curve of composite.
Specific embodiment
With specific embodiment, technical scheme is described further below, but protection scope of the present invention does not limit
In this.
Embodiment 1
By 4gKMnO4And 3.6gNa2SO4It is dissolved in the mixed solvent that 20ml absolute ethyl alcohol and 80ml deionized water are formed,
Subsequently 1.5g Delanium (FSNC-4, FSNC-4 also normal abbreviation FSN-4, Shanghai Shanshan Science and Technology Co., Ltd) is added above-mentioned molten
In liquid, stir 0.1h, stand 0.5h.By the liquid suction filtration of above-mentioned standing, it is placed in 80 DEG C of air dry ovens dry after cyclic washing
Dry 24h.Take the above-mentioned dried powder of 1g, in N2It is warming up to 500 DEG C with the speed of 5 DEG C/min under protective atmosphere, be incubated 6h, cold
But obtain product afterwards, i.e. graphite/Mn3O4Composite.Fig. 1 is this graphite/Mn3O4The XRD diffraction pattern of composite, to sighting target
Quasi- card understands, products therefrom is mangano-manganic oxide.Fig. 2 is this graphite/Mn3O4The corresponding SEM photograph of composite.
Make electrode with the composite obtained by embodiment 1 as follows.
With 80:10:10 mass ratio weighs graphite/Mn respectively3O4Composite, acetylene black, polytetrafluoroethylene (PTFE), grind all
It is coated in after even on Copper Foil and makes negative electrode, electrolyte is 1mol/L LiPF6(volume ratio is 1 to/EC DMC:1:1), poly- third
Alkene microporous membrane (Celgard 2300) is barrier film, is assembled into simulation lithium ion battery.Fig. 3 is battery in 100mAg-1Discharge and recharge
Curve, it can be seen that first charge-discharge specific capacity is very high, reaches 1450mAhg-1And in 0.3～0.5V about have stable filling
Discharge platform.Fig. 4 is 100mAg-1Cyclic curve that discharge and recharge is 80 times it can be seen that after 80 times capacity still remain in
600mAhg-1.Fig. 5 is curve of double curvature figure, and as can be seen from the figure this material still also has certain appearance under high current density
Amount, when current density returns to 50mAg-1, its capacity is stably in 600mAhg-1Left and right.Fig. 6 is the cyclic voltammogram of this material.
Embodiment 2
By 4gKMnO4And 3.6gNa2SO4It is dissolved in the mixed solvent that 20ml absolute ethyl alcohol and 80ml deionized water are formed
In, subsequently 1.5g Delanium (FSNC-4, Shanghai Shanshan Science and Technology Co., Ltd) is added in above-mentioned solution, stir 0.1h, quiet
Set to 0 .5h.By the liquid suction filtration of above-mentioned standing, it is placed in after cyclic washing in 80 DEG C of air dry ovens and 24h is dried.Take 1g above-mentioned dry
Powder after dry, in N2It is warming up to 500 DEG C with the speed of 15 DEG C/min under protective atmosphere, be incubated 6h, obtain product after cooling, that is,
Graphite/Mn3O4Composite.
100mAg-1Cyclic curve that discharge and recharge is 80 times it can be seen that after 80 times capacity still remain in 500mAhg-1.
Different from embodiment 1 be heating rate different it is seen that under 5 DEG C/min Elevated Temperature Conditions, can have preferably
Electric property.
Embodiment 3
By 4gKMnO4And 3.6gNa2SO4It is dissolved in the mixed solvent that 20ml absolute ethyl alcohol and 80ml deionized water are formed,
Subsequently 1.5g Delanium (FSNC-4, Shanghai Shanshan Science and Technology Co., Ltd) is added in above-mentioned solution, stir 0.1h, standing
0.5h.By the liquid suction filtration of above-mentioned standing, it is placed in after cyclic washing in 80 DEG C of air dry ovens and 24h is dried.Take the above-mentioned drying of 1g
Powder afterwards, in N2It is warming up to 600 DEG C with the speed of 5 DEG C/min under protective atmosphere, be incubated 6h, obtain product after cooling, i.e. stone
Ink/Mn3O4Composite.Fig. 1 is this graphite/Mn3O4The XRD diffraction pattern of composite, reference standard card understands, gained produces
Thing is mangano-manganic oxide.Fig. 2 is this graphite/Mn3O4The corresponding SEM photograph of composite.
100mAg-1Cyclic curve that discharge and recharge is 80 times it can be seen that after 80 times capacity still remain in 500mAhg-1.
The final temperatures that are be warmed up to different from embodiment 1 different it is seen that at 500 DEG C, can have more preferable electricity
Learn performance.
Embodiment 4
By 2gKMnO4And 1.8Na2SO4It is dissolved in the mixed solvent that 30ml absolute ethyl alcohol and 70ml deionized water are formed,
Subsequently 2g Delanium (FSNC-4, Shanghai Shanshan Science and Technology Co., Ltd) is added in above-mentioned solution, stir 0.2h, stand 1h.
By the liquid suction filtration of above-mentioned standing, it is placed in after cyclic washing in 80 DEG C of air dry ovens and 24h is dried.Take the above-mentioned dried powder of 1g
End, in N2Be warming up to 550 DEG C with the speed of 15 DEG C/min under protective atmosphere, be incubated 5h, obtain product after cooling, that is, graphite/
Mn3O4Composite.
With obtained graphite/Mn3O4Composite makes electrode as described in Example 1, is assembled into simulation lithium ion
Battery, first charge-discharge capacity about 1000mAhg-1, 100mAg-1Discharge capacity close to 400mAhg-1.
Embodiment 5
By 3gKMnO4And 2.7Na2SO4It is dissolved in the mixed solvent that 40ml absolute ethyl alcohol and 60ml deionized water are formed,
Subsequently 1g Delanium (FSNC-4, Shanghai Shanshan Science and Technology Co., Ltd) is added in above-mentioned solution, stir 0.5h, stand 1h.
By the liquid suction filtration of above-mentioned standing, it is placed in after cyclic washing in 80 DEG C of air dry ovens and 24h is dried.Take 2.5g above-mentioned dried
Powder, in N2Be warming up to 450 DEG C with the speed of 10 DEG C/min under protective atmosphere, be incubated 5h, obtain product after cooling, that is, graphite/
Mn3O4Composite.
With obtained graphite/Mn3O4Composite makes electrode as described in Example 1, is assembled into simulation lithium-ion electric
Pond, first charge-discharge capacity about 1100mAhg-1, 100mAg-1Discharge capacity close to 450mAhg-1.
Embodiment 6
By 6gKMnO4And 5.4Na2SO4It is dissolved in the mixed liquor that 10ml absolute ethyl alcohol and 90ml deionized water are formed, with
Afterwards 4g Delanium (FSNC-4, Shanghai Shanshan Science and Technology Co., Ltd) is added in above-mentioned solution, stir 0.5h, stand 2h.Will
The liquid suction filtration of above-mentioned standing, is placed in after cyclic washing in 80 DEG C of air dry ovens and 24h is dried.Take the above-mentioned dried powder of 3g
End, in N2Be warming up to 600 DEG C with the speed of 20 DEG C/min under protective atmosphere, be incubated 4h, obtain product after cooling, that is, graphite/
Mn3O4Composite.
With obtained graphite/Mn3O4Composite makes electrode as described in Example 1, is assembled into simulation lithium-ion electric
Pond, first charge-discharge capacity about 1200mAhg-1, 100mAg-1Discharge capacity close to 480mAhg-1.
Claims (7)
1. a kind of graphite/Mn3O4The preparation method of composite is it is characterised in that comprise the following steps：
(1) potassium permanganate and sodium sulphate are dissolved in the mixed solvent being made up of water and ethanol, form chemical plating fluid；
In the described mixed solvent being made up of water and ethanol, the volume ratio of water and ethanol is 1～10：1；
The mol ratio of described potassium permanganate and sodium sulphate is 2～0.2：1, potassium permanganate and sodium sulphate in described chemical plating fluid
Total concentration be 0.1～5mol/L；
(2) Delanium is added in chemical plating fluid, stir 0.1～1h, be standing and soak for 0.1～2h, so that potassium permanganate is reduced into
For mangano-manganic oxide and uniform load on the Delanium surface of non-hydrophilic, through filtering, washing, be dried after obtain product；
Described Delanium is 0.1～3 with the mass ratio that feeds intake of potassium permanganate：1；
(3) product obtaining is warming up under protective atmosphere 400 DEG C～800 DEG C, be incubated 2～8h, afterwards cooling obtain graphite/
Mn3O4Composite.
2. graphite/Mn according to claim 13O4The preparation method of composite it is characterised in that in step (1), institute
In the mixed solvent being made up of water and ethanol stated, the volume ratio of water and ethanol is 3～6：1.
3. graphite/Mn according to claim 13O4The preparation method of composite it is characterised in that in step (3), institute
The protective atmosphere stated adopts nitrogen.
4. graphite/Mn according to claim 13O4The preparation method of composite it is characterised in that in step (3), with 5
The heating rate of～20 DEG C/min is warming up to 400～800 DEG C and is incubated 2～8h.
5. graphite/Mn according to claim 43O4The preparation method of composite it is characterised in that in step (3), with 5
DEG C/heating rate of min is warming up to 600 DEG C and is incubated 4～8h.
6. graphite/the Mn of the preparation method preparation according to any one of Claims 1 to 53O4Composite.
7. graphite/Mn according to claim 63O4Composite is in the application as lithium ion battery negative material.
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| CN114634206B (en) * | 2020-12-16 | 2023-11-17 | 中国计量大学 | Preparation method of manganous-manganic oxide |
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| CN103022463B (en) * | 2012-12-20 | 2015-03-25 | 中国东方电气集团有限公司 | Manganese-based compound cathode material of lithium battery and preparation method of material |
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Effective date of registration: 20201202 Address after: 214266, No. 82, new middle road, Xinzhuang Industrial Complex, Wuxi, Jiangsu, Yixing Patentee after: Yixing Xinchi Energy Technology Co., Ltd Address before: 214266, Jiangsu, Wuxi province Yixing Xinzhuang Street industrial concentration zone Patentee before: JIANGSU FENGCHI GREEN POWER SUPPLY Co.,Ltd. |