CN104600261A - Graphite/Mn3O4 composite material and preparation method and application thereof - Google Patents

Graphite/Mn3O4 composite material and preparation method and application thereof Download PDF

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Publication number
CN104600261A
CN104600261A CN201410853670.8A CN201410853670A CN104600261A CN 104600261 A CN104600261 A CN 104600261A CN 201410853670 A CN201410853670 A CN 201410853670A CN 104600261 A CN104600261 A CN 104600261A
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graphite
composite material
preparation
potassium permanganate
ethanol
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CN104600261B (en
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史雪锋
陈鹏
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Yixing Xinchi Energy Technology Co., Ltd
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Sharp Point Of Jiangsu Speeds In Green Power Co Ltd
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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
    • 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
    • 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
    • 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

A kind of graphite/Mn 3o 4composite material and its preparation method and application
Technical field
The present invention relates to cathode material of lithium ion battery field, be specifically related to a kind of graphite/Mn3O4 composite material and preparation method thereof and the application as lithium ion battery negative material.
Background technology
Mangano-manganic oxide as a kind of manganese series oxides material, the feature such as there is abundance, environmental friendliness, cheap, chemical property is good.It has higher theoretical specific capacity (936mAh/g), is considered to one of the most potential cathode material for high capacity lithium ion battery.But in actual applications, it mainly faces two problems to mangano-manganic oxide: on the one hand, and the conductivity of mangano-manganic oxide is low, cause its high rate performance poor; On the other hand, in the process of doff lithium ion repeatedly, there will be violent change in volume, thus cause material serious agglomeration and efflorescence, cause its capacity rapid decay.These problems seriously constrain the commercial applications of mangano-manganic oxide as lithium ion battery negative material.
Lithium ion battery negative mainly adopts graphite material.Although native graphite capacity is high, be easy to compacting, in cyclic process, there will be lamella come off, cause cycle performance difference and safety problem.And Delanium has Stability Analysis of Structures, good cycle and the feature such as security performance is good are the first-selections of lithium ion battery negative material always.Delanium, also reduces specific area, improves capacity, is a kind of carbon negative pole material preferably.But in actual use, carbon negative pole material is because the theoretical capacity of itself is lower, and the space of lifting is very limited, be difficult to the high-energy-density density meeting a new generation, the requirement of the lithium ion battery of high-specific-power density.
In recent years, domestic and international researcher finds good for conductivity material with carbon element and mangano-manganic oxide compound, can effectively in conjunction with the advantage of mangano-manganic oxide high power capacity and material with carbon element high conductivity, solves the exhaustion of mangano-manganic oxide capacity soon and the problem of material with carbon element off-capacity.
Summary of the invention
The object of this invention is to provide a kind of graphite/Mn preparing high power capacity and good circulation stability 3o 4the method of composite material; And preparation cost is low, simple, the applicable suitability for industrialized production of technique.
The present invention adopts first and in water, adds a certain proportion of absolute ethyl alcohol be made into solvent, utilizes solution dipping method, while guarantee graphite-structure, overcome its thin water problem.This method technique is simple, and cost is lower, is easy to realize suitability for industrialized production.
For achieving the above object, the present invention adopts following technical scheme.
A kind of graphite/Mn 3o 4the preparation method of composite material, comprises the following steps:
(1) potassium permanganate and sodium sulphate are dissolved in the mixed solvent be made up of water and ethanol, form chemical plating fluid;
(2) Delanium is added in chemical plating fluid, stirs 0.1 ~ 1h, leave standstill immersion 0.1 ~ 2h, potassium permanganate is reduced become mangano-manganic oxide and uniform load on the Delanium surface of non-hydrophilic, after filtration, washing, obtain product after drying;
(3) product obtained is warming up to 400 DEG C ~ 800 DEG C under protective atmosphere, insulation 2 ~ 8h, cooling afterwards obtains graphite/Mn 3o 4composite material.
In step (1), in the described mixed solvent be made up of water and ethanol, the volume ratio of water and ethanol is 1 ~ 10:1, preferably 3 ~ 6:1.
In step (1), described potassium permanganate and the mol ratio of sodium sulphate are 2 ~ 0.2:1, preferably 1.2 ~ 0.8:1, and in described chemical plating fluid, the total concentration of potassium permanganate and sodium sulphate is 0.1 ~ 5mol/L.
In step (2), the mass ratio that feeds intake of described Delanium and potassium permanganate is 0.1 ~ 3:1, preferably 0.2 ~ 1:1.
In step (2), described protective atmosphere adopts nitrogen.
In step (3), be warming up to 400 ~ 800 DEG C with the heating rate of 5 ~ 20 DEG C/min and be incubated 2 ~ 8h.Further preferably, be warming up to 600 DEG C with the heating rate of 5 DEG C/min and be incubated 4 ~ 8h.
Present invention also offers graphite/Mn 3o 4composite material is as the application of lithium ion battery negative material.
By graphite/Mn 3o 4the negative material that composite material can be used as lithium ion battery adopts existing method to prepare the negative pole of lithium ion battery, and then obtains lithium ion battery by existing method assembling.
Compared with prior art, beneficial effect of the present invention is:
One, raw materials wide material sources, cheap, are easy to industrializing implementation;
Two, the composite material that obtains of the present invention is by mangano-manganic oxide load on graphite matrix, and the conductivity of the mangano-manganic oxide not only improved, introduces mangano-manganic oxide simultaneously, improve its reversible capacity on graphite.Obtained graphite/Mn 3o 4composite material has the characteristics such as capacity is high, good conductivity, cyclical stability are high, particularly has good charging and discharging capacity and good cycle performance, can be used as lithium ion battery negative material and be applied in high-capacity lithium ion cell field.
Accompanying drawing explanation
Fig. 1 is the graphite/Mn prepared by embodiment 1 3o 4the XRD diffraction pattern of composite material;
Fig. 2 is the graphite/Mn prepared by embodiment 1 3o 4the SEM photo of composite material;
Fig. 3 is the graphite/Mn prepared by embodiment 1 3o 4the charging and discharging curve of composite material;
Fig. 4 is the graphite/Mn prepared by embodiment 1 3o 4the cycle performance curve of composite material;
Fig. 5 is the graphite/Mn prepared by embodiment 1 3o 4the high rate performance curve of composite material;
Fig. 6 is the graphite/Mn prepared by embodiment 1 3o 4the cyclic voltammetry curve of composite material.
Embodiment
With specific embodiment, technical scheme of the present invention is described further below, but protection scope of the present invention is not limited thereto.
Embodiment 1
By 4gKMnO 4and 3.6gNa 2sO 4be dissolved in the mixed solvent of 20ml absolute ethyl alcohol and the formation of 80ml deionized water, subsequently 1.5g Delanium (FSNC-4, FSNC-4 are also often called for short FSN-4, Shanghai Shanshan Science and Technology Co., Ltd) added in above-mentioned solution, stir 0.1h, leave standstill 0.5h.By above-mentioned standing liquid suction filtration, cyclic washing is placed on dry 24h in 80 DEG C of air dry ovens.Get the above-mentioned dried powder of 1g, at N 2be warming up to 500 DEG C with the speed of 5 DEG C/min under protective atmosphere, insulation 6h, obtains product after cooling, i.e. graphite/Mn 3o 4composite material.Fig. 1 is this graphite/Mn 3o 4the XRD diffraction pattern of composite material, reference standard card is known, and products therefrom is mangano-manganic oxide.Fig. 2 is this graphite/Mn 3o 4the SEM photo that composite material is corresponding.
Electrode is made as follows with the composite material obtained by embodiment 1.
Graphite/Mn is taken respectively with the mass ratio of 80:10:10 3o 4composite material, acetylene black, polytetrafluoroethylene, be coated on Copper Foil after grinding evenly and make negative electrode, electrolyte is 1mol/L LiPF 6/ EC – DMC (volume ratio is 1:1:1), polypropylene microporous film (Celgard 2300) is barrier film, is assembled into simulation lithium ion battery.Fig. 3 is that battery is at 100mAg -1charging and discharging curve, can see that first charge-discharge specific capacity is very high, reach 1450mAhg -1and have stable charge and discharge platform at about 0.3 ~ 0.5V.Fig. 4 is 100mAg -1the cyclic curve that discharge and recharge is 80 times, can see that capacity still remains on 600mAhg after 80 times -1.Fig. 5 is curve of double curvature figure, and as can be seen from the figure this material still also has certain capacity under high current density, when current density gets back to 50mAg -1, its capacity stablizes is at 600mAhg -1left and right.Fig. 6 is the cyclic voltammogram of this material.
Embodiment 2
By 4gKMnO 4and 3.6gNa 2sO 4be dissolved in the mixed solvent of 20ml absolute ethyl alcohol and the formation of 80ml deionized water, subsequently 1.5g Delanium (FSNC-4, Shanghai Shanshan Science and Technology Co., Ltd) added in above-mentioned solution, stir 0.1h, leave standstill 0.5h.By above-mentioned standing liquid suction filtration, cyclic washing is placed on dry 24h in 80 DEG C of air dry ovens.Get the above-mentioned dried powder of 1g, at N 2be warming up to 500 DEG C with the speed of 15 DEG C/min under protective atmosphere, insulation 6h, obtains product after cooling, i.e. graphite/Mn 3o 4composite material.
100mAg -1the cyclic curve that discharge and recharge is 80 times, can see that capacity still remains on 500mAhg after 80 times -1.
Differently from embodiment 1 be that heating rate is different, as seen under 5 DEG C/min Elevated Temperature Conditions, better electric property can be had.
Embodiment 3
By 4gKMnO 4and 3.6gNa 2sO 4be dissolved in the mixed solvent of 20ml absolute ethyl alcohol and the formation of 80ml deionized water, subsequently 1.5g Delanium (FSNC-4, Shanghai Shanshan Science and Technology Co., Ltd) added in above-mentioned solution, stir 0.1h, leave standstill 0.5h.By above-mentioned standing liquid suction filtration, cyclic washing is placed on dry 24h in 80 DEG C of air dry ovens.Get the above-mentioned dried powder of 1g, at N 2be warming up to 600 DEG C with the speed of 5 DEG C/min under protective atmosphere, insulation 6h, obtains product after cooling, i.e. graphite/Mn 3o 4composite material.Fig. 1 is this graphite/Mn 3o 4the XRD diffraction pattern of composite material, reference standard card is known, and products therefrom is mangano-manganic oxide.Fig. 2 is this graphite/Mn 3o 4the SEM photo that composite material is corresponding.
100mAg -1the cyclic curve that discharge and recharge is 80 times, can see that capacity still remains on 500mAhg after 80 times -1.
Differently from embodiment 1 be that the final temperature be warmed up to is different, as seen at 500 DEG C, better electric property can be had.
Embodiment 4
By 2gKMnO 4and 1.8Na 2sO 4be dissolved in the mixed solvent of 30ml absolute ethyl alcohol and the formation of 70ml deionized water, subsequently 2g Delanium (FSNC-4, Shanghai Shanshan Science and Technology Co., Ltd) added in above-mentioned solution, stir 0.2h, leave standstill 1h.By above-mentioned standing liquid suction filtration, cyclic washing is placed on dry 24h in 80 DEG C of air dry ovens.Get the above-mentioned dried powder of 1g, at N 2be warming up to 550 DEG C with the speed of 15 DEG C/min under protective atmosphere, insulation 5h, obtains product after cooling, i.e. graphite/Mn 3o 4composite material.
With obtained graphite/Mn 3o 4composite material makes electrode by the method for embodiment 1, is assembled into simulation lithium ion battery, and first charge-discharge capacity is about 1000mAhg -1, 100mAg -1discharge capacity close to 400mAhg -1.
Embodiment 5
By 3gKMnO 4and 2.7Na 2sO 4be dissolved in the mixed solvent of 40ml absolute ethyl alcohol and the formation of 60ml deionized water, subsequently 1g Delanium (FSNC-4, Shanghai Shanshan Science and Technology Co., Ltd) added in above-mentioned solution, stir 0.5h, leave standstill 1h.By above-mentioned standing liquid suction filtration, cyclic washing is placed on dry 24h in 80 DEG C of air dry ovens.Get the above-mentioned dried powder of 2.5g, at N 2be warming up to 450 DEG C with the speed of 10 DEG C/min under protective atmosphere, insulation 5h, obtains product after cooling, i.e. graphite/Mn 3o 4composite material.
With obtained graphite/Mn 3o 4composite material makes electrode by the method for embodiment 1, is assembled into simulation lithium ion battery, and first charge-discharge capacity is about 1100mAhg -1, 100mAg -1discharge capacity close to 450mAhg -1.
Embodiment 6
By 6gKMnO 4and 5.4Na 2sO 4be dissolved in the mixed liquor of 10ml absolute ethyl alcohol and the formation of 90ml deionized water, subsequently 4g Delanium (FSNC-4, Shanghai Shanshan Science and Technology Co., Ltd) added in above-mentioned solution, stir 0.5h, leave standstill 2h.By above-mentioned standing liquid suction filtration, cyclic washing is placed on dry 24h in 80 DEG C of air dry ovens.Get the above-mentioned dried powder of 3g, at N 2be warming up to 600 DEG C with the speed of 20 DEG C/min under protective atmosphere, insulation 4h, obtains product after cooling, i.e. graphite/Mn 3o 4composite material.
With obtained graphite/Mn 3o 4composite material makes electrode by the method for embodiment 1, is assembled into simulation lithium ion battery, and first charge-discharge capacity is about 1200mAhg -1, 100mAg -1discharge capacity close to 480mAhg -1.

Claims (10)

1. graphite/Mn 3o 4the preparation method of composite material, is characterized in that, comprises the following steps:
(1) potassium permanganate and sodium sulphate are dissolved in the mixed solvent be made up of water and ethanol, form chemical plating fluid;
(2) Delanium is added in chemical plating fluid, stirs 0.1 ~ 1h, leave standstill immersion 0.1 ~ 2h, potassium permanganate is reduced become mangano-manganic oxide and uniform load on the Delanium surface of non-hydrophilic, after filtration, washing, obtain product after drying;
(3) product obtained is warming up to 400 DEG C ~ 800 DEG C under protective atmosphere, insulation 2 ~ 8h, cooling afterwards obtains graphite/Mn 3o 4composite material.
2. graphite/Mn according to claim 1 3o 4the preparation method of composite material, is characterized in that, in step (1), in the described mixed solvent be made up of water and ethanol, the volume ratio of water and ethanol is 1 ~ 10:1.
3. graphite/Mn according to claim 2 3o 4the preparation method of composite material, is characterized in that, in step (1), in the described mixed solvent be made up of water and ethanol, the volume ratio of water and ethanol is 3 ~ 6:1.
4. graphite/Mn according to claim 1 3o 4the preparation method of composite material, is characterized in that, in step (1), described potassium permanganate and the mol ratio of sodium sulphate are 2 ~ 0.2:1, and in described chemical plating fluid, the total concentration of potassium permanganate and sodium sulphate is 0.1 ~ 5mol/L.
5. graphite/Mn according to claim 1 3o 4the preparation method of composite material, is characterized in that, in step (2), the mass ratio that feeds intake of described Delanium and potassium permanganate is 0.1 ~ 3:1.
6. graphite/Mn according to claim 1 3o 4the preparation method of composite material, is characterized in that, in step (2), described protective atmosphere adopts nitrogen.
7. graphite/Mn according to claim 1 3o 4the preparation method of composite material, is characterized in that, in step (3), is warming up to 400 ~ 800 DEG C and is incubated 2 ~ 8h with the heating rate of 5 ~ 20 DEG C/min.
8. graphite/Mn according to claim 7 3o 4the preparation method of composite material, is characterized in that, in step (3), is warming up to 600 DEG C and is incubated 4 ~ 8h with the heating rate of 5 DEG C/min.
9. graphite/Mn prepared by the preparation method according to any one of claim 1 ~ 8 3o 4composite material.
10. graphite/Mn according to claim 9 3o 4composite material is in the application as lithium ion battery negative material.
CN201410853670.8A 2014-12-31 2014-12-31 Graphite/Mn3O4 composite material and preparation method and application thereof Active CN104600261B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109309217A (en) * 2018-08-20 2019-02-05 中国航发北京航空材料研究院 A kind of preparation method of lithium sulfur battery anode material
CN114634206A (en) * 2020-12-16 2022-06-17 中国计量大学 Preparation method of mangano-manganic oxide

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109309217A (en) * 2018-08-20 2019-02-05 中国航发北京航空材料研究院 A kind of preparation method of lithium sulfur battery anode material
CN109309217B (en) * 2018-08-20 2021-09-14 中国航发北京航空材料研究院 Preparation method of lithium-sulfur battery positive electrode material
CN114634206A (en) * 2020-12-16 2022-06-17 中国计量大学 Preparation method of mangano-manganic oxide
CN114634206B (en) * 2020-12-16 2023-11-17 中国计量大学 Preparation method of manganous-manganic oxide

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