CN106252633A - A kind of preparation method of lithium ion battery negative material - Google Patents

A kind of preparation method of lithium ion battery negative material Download PDF

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Publication number
CN106252633A
CN106252633A CN201610828515.XA CN201610828515A CN106252633A CN 106252633 A CN106252633 A CN 106252633A CN 201610828515 A CN201610828515 A CN 201610828515A CN 106252633 A CN106252633 A CN 106252633A
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lithium ion
ion battery
negative material
battery negative
preparation
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曹丽云
王瑞谊
李瑞梓
许占位
黄剑锋
李嘉胤
李康
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Shaanxi University of Science and Technology
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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
    • 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
    • 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 present invention relates to the preparation method of a kind of lithium ion battery negative material, described negative material is Mn3O4The complex of/CNTs, with potassium permanganate, manganese sulfate and carboxylated CNT as raw material, prepares the complex of manganese dioxide and CNT initially with low-temperature co-precipitation method, after by its heat treatment, obtain Mn3O4/ CNTs complex, can be as the negative material of lithium ion battery；Compared with prior art, the preparation technology of the present invention is simple, and raw material is simple and easy to get, and the addition of CNTs greatly improves Mn3O4Electric conductivity so that the transmission speed of electronics and lithium ion is accelerated, and battery impedance reduces, and capacity increases.

Description

A kind of preparation method of lithium ion battery negative material
Technical field
The invention belongs to field of lithium ion battery, be specifically related to the preparation method of a kind of lithium ion battery negative material.
Background technology
Lithium ion battery is high with its specific energy, power density high, have extended cycle life, self discharge is little, the ratio of performance to price is high Advantage has become as the main selection object of the rechargeable formula power supply of current portable type electronic product.It is widely used in pen Remember in the portable electric appts such as this computer, hand-held terminal machine, wireless phone, wireless device, video camera, digital camera, certainly As the electrokinetic cell of following electric automobile, it also it is one of the application prospect of great potential.Positive and negative pole material and electrolyte are lithiums The key component of ion battery, determines the overall performance of battery.Positive electrode current material and electrolyte have obtained very fast development.From Within 1980, J.B.Gooodenough finds the LiCoO of layer structure2Since material, people find multiple positive electrode the most successively, Such as: LiV3O8、LiMn2O4And LiFePO4Deng.In the middle of these materials, LiCoO2、LiV3O8There is of a relatively high specific capacity, LiMn2O4And LiFePO4Material safety is good and can meet fast charging and discharging, and therefore negative material becomes development lithium-ion electric The key point in pond.
Transition metal oxide is recognized due to its high theoretical capacity (2～3 times of Graphene) and abundant natural resources For being the candidate of the most electrode material of prospect.Wherein, Mn3O4The theoretical specific capacity high due to it and hypotoxicity, raw material are rich The advantages such as rich, operation voltage is low are widely used.But, Li+At Mn3O4In storage have following obstacle in actual applications: (1)Li+Embedding and deintercalation during big bulk effect, easily cause electrode material efflorescence, therefore result in low capacity； (2) low conductivity result in low battery performance.For solving problem above, the present invention selects and the CNT of high conductivity Compound, on the one hand make Mn with CNT for template3O4Direction along tube wall grows and is uniformly distributed on the carbon nanotubes, Two is to drastically increase Mn3O4As the electric conductivity of electrode material, and then improve the circulation of lithium ion battery and the most forthright Energy.
At present it has been reported that preparation Mn3O4/ CNTs has as the preparation method of lithium ion battery electrode material: solvent thermal Method, thermal decomposition method etc..Zhaohui Wang et al. passes through solvent with sodium acetate, manganese nitrate, ethylene glycol and CNT for raw material The heat treatment route in heat and later stage is prepared for, Mn3O4/ CNTs complex, as lithium ion battery negative material, in electric current density For 100mAg-1Time, after circulation 50 circle, reversible specific capacity is 592mA h g-1。[Wang Z H,Yuan L X,Shao Q G,et al.Mn3O4nanocrystals anchored on multi-walled carbon nanotubes as high- performance anode materials for lithium-ion batteries[J].Materials Letters, 2012,80:110-113.].Although the method has successfully prepared Mn3O4/ CNTs complex, but preparation process is complicated, required Energy higher, be unsuitable for industrialization large-scale production, and its performance of lithium ion battery negative material the most be not for he The most preferable.Shu Luo et al. by by thin film dipped for SACNT in manganese nitrate solution then in Muffle furnace heat treatment prepare Mn3O4/ SACNT, as the cell negative electrode material of lithium ion, after circulation 100 circle, reversible specific capacity is 390mA h g-1。[Luo S,Wu H,Wu Y,et al.Mn3O4nanoparticles anchored on continuous carbon nanotube network as superior anodes for lithium ion batteries[J].Journal of Power Sources,2014,249:463-469.].Although the method preparation process is simple, better performances, but the preparation of raw material is more multiple Miscellaneous, it is not suitable for large-scale industrial production yet.
Summary of the invention
It is an object of the invention to provide the preparation of the lithium ion battery negative material that a kind of technique is simple, raw material is simple and easy to get Method.
For achieving the above object, its concrete technical scheme is as follows:
1) take the CNT of 0.05-0.2g, use deionized water, ultrasonic disperse；
2) potassium permanganate and manganese sulfate are configured to respectively potassium permanganate solution that mass fraction is 2%-5% and quality is divided Number is the manganese sulfate solution of 3-10%；
3) scattered CNT is added stirring in potassium permanganate solution, uniform to system；
4) manganese sulfate solution prepared is slowly added into step 3) obtained by homogeneous system in, be stirred continuously, Separate out to black precipitate；
5) by step 4) black precipitate of gained washing, filter, dry, heat treatment in tube-type atmosphere furnace, the most available Mn3O4/ CNTs lithium ion battery negative material.
Described step 1) CNT be carboxylated a diameter of 20-30nm CNT.
Described step 3) stirring be magnetic agitation.
Described step 4) the rotating speed of stirring be 500-1200r min-1。
Described step 4) time of stirring be 3-12h.
Described step 5) in washing liquid be deionized water and dehydrated alcohol.
Described step 5) in tube-type atmosphere furnace be argon gas atmosphere.
Described step 5) in heat treatment temperature be 300-600 DEG C, the time is 1-5h.
The present invention is with potassium permanganate, manganese sulfate and carboxylated CNT as raw material, initially with low-temperature co-precipitation method Prepare the complex of manganese dioxide and CNT, after by its heat treatment, obtain Mn3O4/ CNTs complex, can as lithium from The negative material of sub-battery.Compared with prior art, the preparation technology of the present invention is simple, and raw material is simple and easy to get, and the adding of CNTs Enter and greatly improve Mn3O4Electric conductivity so that the transmission speed of electronics and lithium ion is accelerated, and battery impedance reduces, and capacity increases Greatly.
Accompanying drawing explanation
Fig. 1 is lithium ion battery negative material Mn prepared by the present invention3O4SEM (scanning electron microscope) figure (times magnification of/CNTs Several 100,000 times).
Fig. 2 is lithium ion battery negative material Mn prepared by the present invention3O4SEM (scanning electron microscope) figure (times magnification of/CNTs Several 200,000 times).
Fig. 3 is lithium ion battery negative material Mn prepared by the present invention3O4XRD (X-ray diffraction) figure of/CNTs.
Fig. 4 is lithium ion battery negative material Mn prepared by the present invention3O4/ CNTs cyclical stability figure.
Detailed description of the invention
Embodiment 1:
1) take carboxylated a diameter of 20-30nm CNT of 0.05g, use deionized water, ultrasonic disperse；
2) potassium permanganate and manganese sulfate are configured to respectively potassium permanganate solution that mass fraction is 2% and mass fraction is The manganese sulfate solution of 3%；
3) scattered CNT is added magnetic agitation in potassium permanganate solution, uniform to system；
4) manganese sulfate solution prepared is slowly added into step 3) obtained by homogeneous system in, with 500r min-1Stirring 12h, separates out to black precipitate；
5) by step 4) the black precipitate deionized water of gained and absolute ethanol washing, filter, dry, in argon gas atmosphere With 300 DEG C in tube-type atmosphere furnace, heat treatment 5h, i.e. can get Mn3O4/ CNTs lithium ion battery negative material.
Embodiment 2:
1) take carboxylated a diameter of 20-30nm CNT of 0.1g, use deionized water, ultrasonic disperse；
2) potassium permanganate and manganese sulfate are configured to respectively potassium permanganate solution that mass fraction is 3% and mass fraction is The manganese sulfate solution of 6%；
3) scattered CNT is added magnetic agitation in potassium permanganate solution, uniform to system；
4) manganese sulfate solution prepared is slowly added into step 3) obtained by homogeneous system in, with 800r min-1Stirring 8h, separates out to black precipitate；
5) by step 4) the black precipitate deionized water of gained and absolute ethanol washing, filter, dry, in argon gas atmosphere With 400 DEG C in tube-type atmosphere furnace, heat treatment 3h, i.e. can get Mn3O4/ CNTs lithium ion battery negative material.
Embodiment 3:
1) take carboxylated a diameter of 20-30nm CNT of 0.15g, use deionized water, ultrasonic disperse；
2) potassium permanganate and manganese sulfate are configured to respectively potassium permanganate solution that mass fraction is 4% and mass fraction is The manganese sulfate solution of 8%；
3) scattered CNT is added magnetic agitation in potassium permanganate solution, uniform to system；
4) manganese sulfate solution prepared is slowly added into step 3) obtained by homogeneous system in, with 700r min-1Stirring 6h, separates out to black precipitate；
5) by step 4) the black precipitate deionized water of gained and absolute ethanol washing, filter, dry, in argon gas atmosphere With 500 DEG C in tube-type atmosphere furnace, heat treatment 2h, i.e. can get Mn3O4/ CNTs lithium ion battery negative material.
Embodiment 4:
1) take carboxylated a diameter of 20-30nm CNT of 0.2g, use deionized water, ultrasonic disperse；
2) potassium permanganate and manganese sulfate are configured to respectively potassium permanganate solution that mass fraction is 5% and mass fraction is The manganese sulfate solution of 10%；
3) scattered CNT is added magnetic agitation in potassium permanganate solution, uniform to system；
4) manganese sulfate solution prepared is slowly added into step 3) obtained by homogeneous system in, with 900r min-1Stirring 10h, separates out to black precipitate；
5) by step 4) the black precipitate deionized water of gained and absolute ethanol washing, filter, dry, in argon gas atmosphere With 600 DEG C in tube-type atmosphere furnace, heat treatment 1h, i.e. can get Mn3O4/ CNTs lithium ion battery negative material.
Embodiment 5:
1) take carboxylated a diameter of 20-30nm CNT of 0.15g, use deionized water, ultrasonic disperse；
2) potassium permanganate and manganese sulfate are configured to respectively potassium permanganate solution that mass fraction is 3% and mass fraction is The manganese sulfate solution of 9%；
3) scattered CNT is added magnetic agitation in potassium permanganate solution, uniform to system；
4) manganese sulfate solution prepared is slowly added into step 3) obtained by homogeneous system in, with 1000r min-1Stirring 5h, separates out to black precipitate；
5) by step 4) the black precipitate deionized water of gained and absolute ethanol washing, filter, dry, in argon gas atmosphere With 500 DEG C in tube-type atmosphere furnace, heat treatment 3h, i.e. can get Mn3O4/ CNTs lithium ion battery negative material.
Embodiment 6:
1) take carboxylated a diameter of 20-30nm CNT of 0.1g, use deionized water, ultrasonic disperse；
2) potassium permanganate and manganese sulfate are configured to respectively potassium permanganate solution that mass fraction is 2% and mass fraction is The manganese sulfate solution of 5%；
3) scattered CNT is added magnetic agitation in potassium permanganate solution, uniform to system；
4) manganese sulfate solution prepared is slowly added into step 3) obtained by homogeneous system in, with 1200r min-1Stirring 3h, separates out to black precipitate；
5) by step 4) the black precipitate deionized water of gained and absolute ethanol washing, filter, dry, in argon gas atmosphere With 400 DEG C in tube-type atmosphere furnace, heat treatment 2h, i.e. can get Mn3O4/ CNTs lithium ion battery negative material.
From Fig. 1 to find out, the Mn prepared3O4/ CNTs lithium ion battery negative material presents tubulose and Mn3O4Granule is equal The pattern of even distribution.
From Fig. 2 to find out, granular Mn3O4There is the least size, about about 20nm, be evenly distributed in very much Around CNTs.
From figure 3, it can be seen that successfully prepared the Mn of Tetragonal by the preparation method of the present invention3O4And CNT Complex.
It can be seen from figure 4 that the lithium ion battery negative material Mn prepared by the preparation method of the present invention3O4/ CNTs has good chemical property, and first discharge specific capacity is 859mA h g-1, after 50 circles, reversible specific capacity is 650mAh g-1。

Claims (8)

1. the preparation method of a lithium ion battery negative material, it is characterised in that: comprise the following steps:
1) take the CNT of 0.05-0.2g, use deionized water, ultrasonic disperse；
2) potassium permanganate and manganese sulfate are configured to respectively potassium permanganate solution that mass fraction is 2%-5% and mass fraction is The manganese sulfate solution of 3-10%；
3) scattered CNT is added stirring in potassium permanganate solution, uniform to system；
4) manganese sulfate solution prepared is slowly added into step 3) obtained by homogeneous system in, be stirred continuously, to the most black Color Precipitation；
5) by step 4) black precipitate of gained washing, filter, dry, heat treatment in tube-type atmosphere furnace, i.e. can get Mn3O4/ CNTs lithium ion battery negative material.
The preparation method of a kind of lithium ion battery negative material the most according to claim 1, it is characterised in that: described step 1) CNT is carboxylated a diameter of 20-30nm CNT.
The preparation method of a kind of lithium ion battery negative material the most according to claim 1, it is characterised in that: described step 3) stirring is magnetic agitation.
The preparation method of a kind of lithium ion battery negative material the most according to claim 1, it is characterised in that: described step 4) rotating speed of stirring is 500-1200r min-1。
The preparation method of a kind of lithium ion battery negative material the most according to claim 1, it is characterised in that: described step 4) time of stirring is 3-12h.
The preparation method of a kind of lithium ion battery negative material the most according to claim 1, it is characterised in that: described step 5) washing liquid in is deionized water and dehydrated alcohol.
The preparation method of a kind of lithium ion battery negative material the most according to claim 1, it is characterised in that: described step 5) tube-type atmosphere furnace in is argon gas atmosphere.
The preparation method of a kind of lithium ion battery negative material the most according to claim 1, it is characterised in that: described step 5) heat treatment temperature in is 300-600 DEG C, and the time is 1-5h.
CN201610828515.XA 2016-09-18 2016-09-18 A kind of preparation method of lithium ion battery negative material Pending CN106252633A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107104229A (en) * 2017-06-15 2017-08-29 中南大学 Lithium ion battery negative material silica-doping manganese oxide/carbon pipe and preparation method
CN108461726A (en) * 2018-03-12 2018-08-28 陕西科技大学 A kind of polycrystalline manganese dioxide/carbon nanotube composite material and its preparation method and application
CN108511731A (en) * 2018-05-09 2018-09-07 南京卡耐新能源技术发展有限公司 A kind of carbon composite CNTs@Mn3O4Fast preparation method
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
CN111640926A (en) * 2020-06-17 2020-09-08 郑州轻工业大学 Carbon nano tube/Mn of core-sheath nano cable structure3O4Composite material and preparation method thereof
CN111653740A (en) * 2020-05-07 2020-09-11 广东格林赛福能源科技有限公司 Flexible manganous-manganic oxide cathode and preparation method thereof

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CN105609752A (en) * 2016-02-02 2016-05-25 陕西科技大学 Preparation method for nano-granular Mn3O4/Super P lithium ion battery negative electrode material

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CN105609752A (en) * 2016-02-02 2016-05-25 陕西科技大学 Preparation method for nano-granular Mn3O4/Super P lithium ion battery negative electrode material

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107104229A (en) * 2017-06-15 2017-08-29 中南大学 Lithium ion battery negative material silica-doping manganese oxide/carbon pipe and preparation method
CN107104229B (en) * 2017-06-15 2020-04-14 中南大学 Lithium ion battery cathode material silicon oxide doped manganese oxide/carbon tube and preparation method thereof
CN108461726A (en) * 2018-03-12 2018-08-28 陕西科技大学 A kind of polycrystalline manganese dioxide/carbon nanotube composite material and its preparation method and application
CN108461726B (en) * 2018-03-12 2020-09-29 陕西科技大学 Polycrystalline manganese dioxide/carbon nanotube composite material and preparation method and application thereof
CN108511731A (en) * 2018-05-09 2018-09-07 南京卡耐新能源技术发展有限公司 A kind of carbon composite CNTs@Mn3O4Fast preparation method
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
CN111653740A (en) * 2020-05-07 2020-09-11 广东格林赛福能源科技有限公司 Flexible manganous-manganic oxide cathode and preparation method thereof
CN111640926A (en) * 2020-06-17 2020-09-08 郑州轻工业大学 Carbon nano tube/Mn of core-sheath nano cable structure3O4Composite material and preparation method thereof

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