CN107425181A - A kind of preparation method of manganese oxide/starch base hard carbon composite negative pole material - Google Patents

A kind of preparation method of manganese oxide/starch base hard carbon composite negative pole material Download PDF

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CN107425181A
CN107425181A CN201610349491.XA CN201610349491A CN107425181A CN 107425181 A CN107425181 A CN 107425181A CN 201610349491 A CN201610349491 A CN 201610349491A CN 107425181 A CN107425181 A CN 107425181A
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hard carbon
starch base
base hard
preparation
manganese oxide
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CN107425181B (en
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王磊
苏蒙
谢秋生
乔永民
刘萍
王建明
吴志红
丁晓阳
杜辉玉
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NINGBO SHANSHAN NEW MATERILA TECHNOLOGY Co Ltd
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NINGBO SHANSHAN NEW MATERILA TECHNOLOGY 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
    • H01M4/366—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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • 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

The present invention relates to lithium ion battery material technical field, the preparation method of specifically a kind of manganese oxide/starch base hard carbon composite negative pole material, it is characterised in that use following preparation process：(1), pre- carbonization obtains the pre- carbonized powder product of black；(2) starch base hard carbon material (3), mixing, are prepared；(4), hydro-thermal reaction；(5) finished product, is obtained.The present invention forms the manganese oxide protective layer of impalpable structure on starch base hard carbon surface compared with prior art, by hydro-thermal method, the lithium ion that electrode surface is consumed with electrolyte formation SEI films is reduced, so as to improve the coulombic efficiency first of negative material；The manganese oxide for the lithium ion battery negative material/starch base hard carbon prepared has the characteristics of chemical property is good, good cycling stability and batch products uniformity are outstanding；And preparation method is simple, environmentally friendly, the easy large-scale production of production and product quality are easily controlled.

Description

A kind of preparation method of manganese oxide/starch base hard carbon composite negative pole material
Technical field
The present invention relates to lithium ion battery material technical field, specifically a kind of manganese oxide/starch base hard carbon The preparation method of composite negative pole material.
Background technology
Lithium ion battery is to start practical novel high-energy secondary cell the last century 90's, has work Voltage is high, in light weight, bigger than energy, self discharge is small, have extended cycle life, memory-less effect and environmental pollution The advantages that small.Lithium ion battery negative material mainly has Delanium, native graphite and without fixed based on carbon Shape carbon.But there is problems with current graphite cathode：1st, the current potential of potential plateau and lithium metal approaches, Yi Xi Go out dendrite Li and cause short circuit；2nd, SEI films are unstable, and Li easily occurs+Graphite is embedded in jointly with organic solvent Layer, cause graphite stripping and efflorescence；3rd, graphite C interlamellar spacing (d002≤ 0.34nm) ＜ LixC6(~0.37nm), Volume Changes 8%, it is easily caused graphite linings stripping and efflorescence；4th, exothermic reaction occurs for graphite and organic solvent, It is also easy to produce fuel gas, battery easy firing；5、Li+Diffusion coefficient is small, difficult quick charge.
Amorphous carbon can be divided into hard carbon and soft carbon by graphited complexity.With graphite Comparatively speaking, without fixed Hard carbon in shape carbon has that electrode expansion is small, and warpage, high cycle life-span and good rate capability etc. do not occur for battery Advantage.Hard carbon can by sources be divided into biomass and the class of fossil resource two, and hard carbon forerunner is used as by the use of biomass starch Body has environmental protection and low cost and other advantages.Starch base hard carbon material refers to using starch as raw material, by certain bar Amorphous carbon material prepared by the heat treatment of part, belong to biomass class hard carbon material.Compared to fossil resource Class hard carbon, it has advantages below：1st, wide material sources, raw material have recyclability；2nd, preparation technology letter Just, it is environment-friendly；3rd, cost is cheap, is adapted to industrialization.
At present, mainly efficiency is low first and voltage delay phenomenon be present the shortcomings that hard carbon cathode material.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, and hard carbon cathode material passes through compound other negative pole materials Material, to improve the order on hard carbon material surface, reduce electrode surface and form firm SEI films with electrolyte The lithium ion consumed, be advantageous to improve lithium ion coulombic efficiency, while first excellent by other electrodes itself Different electrical property, improve the overall chemical property of combination electrode.
To achieve the above object, a kind of preparation method of manganese oxide/starch base hard carbon composite negative pole material is designed, It is characterized in that using following preparation process：
(1), pre- carbonization：By starch, constant temperature keeps 24-48h in 200-250 DEG C of vacuum drying chamber, obtains The pre- carbonized powder product of black；
(2) starch base hard carbon material, is prepared：By the pre- carbonized powder product obtained by above-mentioned preparation, in inertia In atmosphere, temperature rises to 900-1100 DEG C with 1-10 DEG C/min, keeps being down to room temperature with stove after 1-4h, obtains To starch base hard carbon material；
(3), mix：By weight by manganese salt：Starch base hard carbon material：Distilled water=5-15:100：800 Mixed, stirring is completely dissolved up to manganese salt, obtains mixture；
(4), hydro-thermal reaction：By mixture in hydrothermal reaction kettle, 5-15h is heat-treated with 150-200 DEG C, Obtain black product；
(5) finished product, is obtained：Black product is through washing, being dried to obtain manganese oxide/starch base hard carbon composite negative pole material Material；
Described manganese salt is one kind in potassium permanganate, manganese nitrate, manganous hydroxide.
Described inert atmosphere is one or both of nitrogen, argon gas, helium.
In described preparation starch base hard carbon material step, described temperature is 1000 DEG C.
In described hydro-thermal reaction step, mixture is in hydrothermal reaction kettle, with 160 DEG C of heat treatment 10h.
The present invention forms impalpable structure on starch base hard carbon surface compared with prior art, by hydro-thermal method Manganese oxide protective layer, imperfect crystal formation degree is relatively low, is advantageous to the movement of ion, and it is hard to eliminate starch base The anisotropy of carbon material surface, the lithium ion that electrode surface is consumed with electrolyte formation SEI films is reduced, So as to improve the coulombic efficiency first of negative material；The oxidation for lithium ion battery negative material prepared Manganese/starch base hard carbon has the spy that chemical property is good, good cycling stability and batch products uniformity are outstanding Point；And preparation method is simple, environmentally friendly, the easy large-scale production of production and product quality are easily controlled.
Brief description of the drawings
Fig. 1 is the SEM figures of manganese oxide/starch base hard carbon composite negative pole material prepared by the present invention.
Fig. 2 is manganese oxide/starch base hard carbon composite negative pole material and identical preparation prepared by the embodiment of the present invention 2 The 0.1C head Zhou Xunhuan discharge curve comparison diagrams for the starch base hard carbon cathode material that condition obtains.
Embodiment
The present invention is further described in conjunction with embodiment.
Embodiment 1
A, pre- carbonization：By starch, constant temperature keeps 24h in 200 DEG C of vacuum drying chambers, obtains the pre- carbon of black Change powdered product；
B, starch base hard carbon material is prepared：By pre- carbonized powder product, the temperature in inert atmosphere is nitrogen 900 DEG C are risen to 10 DEG C/min, are kept being down to room temperature with stove after 1h, are obtained starch base hard carbon material.
C, mix：By potassium permanganate and starch base hard carbon material and distilled water by weight 5:100：800 is mixed Close, by stirring until potassium permanganate is completely dissolved to obtain mixture.
D, hydro-thermal reaction：Mixture is heat-treated 5h with 150 DEG C in hydrothermal reaction kettle, obtains black product.
E, finished product is obtained：By black product through washing, being dried to obtain manganese oxide/starch base hard carbon composite negative pole material.
Embodiment 2
A, pre- carbonization：By starch, constant temperature keeps 48h in 250 DEG C of vacuum drying chambers, obtains the pre- carbon of black Change powdered product；
B, starch base hard carbon material is prepared：It is temperature of argon gas with 1 DEG C in inert atmosphere by pre- carbonized powder product / min rises to 1100 DEG C, keeps being down to room temperature with stove after 4h, obtains starch base hard carbon material.
C, mix：By manganese nitrate and starch base hard carbon material and distilled water by weight 15:100：800 is mixed Close, by stirring until manganese nitrate is completely dissolved, obtain mixture.
D, hydro-thermal reaction：Mixture is heat-treated 15h with 200 DEG C in hydrothermal reaction kettle, obtains black product.
E, finished product is obtained：By black product through washing, being dried to obtain manganese oxide/starch base hard carbon composite negative pole material.
Embodiment 3
A, pre- carbonization：By starch, constant temperature keeps 36h in 220 DEG C of vacuum drying chambers, obtains the pre- carbon of black Change powdered product；
B, starch base hard carbon material is prepared：By pre- carbonized powder product, in inert atmosphere is helium, temperature 1000 DEG C are risen to 5 DEG C/min, are kept being down to room temperature with stove after 2h, are obtained starch base hard carbon material.
C, mix：By manganous hydroxide and starch base hard carbon material and distilled water by weight 10:100：800 Mixing, by stirring until manganous hydroxide is completely dissolved, obtain mixture.
D, hydro-thermal reaction：Mixture is heat-treated 10h with 160 DEG C in hydrothermal reaction kettle, obtains black product.
E, finished product is obtained：By black product through washing, being dried to obtain manganese oxide/starch base hard carbon composite negative pole material.
Embodiment 4
A, pre- carbonization：By starch, constant temperature keeps 48h in 200 DEG C of vacuum drying chambers, obtains the pre- carbon of black Change powdered product；
B, starch base hard carbon material is prepared：It is that nitrogen, argon gas mix in inert atmosphere by pre- carbonized powder product Close in gas, temperature rises to 1050 DEG C with 7 DEG C/min, keeps being down to room temperature with stove after 3h, it is hard to obtain starch base Carbon material.
C, mix：By potassium permanganate and starch base hard carbon material and distilled water by weight 6:100：800 is mixed Close, by stirring until potassium permanganate is completely dissolved, mixture.
D, hydro-thermal reaction：Mixture is heat-treated 9h with 170 DEG C in hydrothermal reaction kettle, obtains black product.
E, finished product is obtained：Black product is washed, is dried to obtain manganese oxide/starch base hard carbon composite negative pole material.
Embodiment 5
A, pre- carbonization：By starch, constant temperature keeps 40h in 230 DEG C of vacuum drying chambers, obtains the pre- carbon of black Change powdered product；
B, starch base hard carbon material is prepared：It is that nitrogen, helium mix in inert atmosphere by pre- carbonized powder product Close in gas, temperature rises to 950 DEG C with 7 DEG C/min, is down to room temperature after keeping 4h, obtains starch base hard carbon material Material.
C, mix：By manganese nitrate and starch base hard carbon material and distilled water by weight 12:100：800 is mixed Close, by stirring until manganese nitrate is completely dissolved, mixture.
D, hydro-thermal reaction：Mixture is heat-treated 12h with 180 DEG C in hydrothermal reaction kettle, obtains black product.
E, finished product is obtained：By black product through washing, being dried to obtain manganese oxide/starch base hard carbon composite negative pole material.
Now by taking the manganese oxide prepared by example 2/starch base hard carbon composite negative pole material as an example, its electrochemistry is tested Performance, it is specific as follows：
Manganese oxide prepared by embodiment 2/starch base hard carbon composite negative pole material and identical preparation condition are obtained Starch base hard carbon cathode material, respectively with conductive agent acetylene black, polyfluortetraethylene of binding element emulsion by weight Than 80:15:5 are well mixed in aqueous, and on copper foil negative plate is made, with metal lithium sheet in then tabletting For negative pole, the ethylene carbonate of 1mol/L lithium hexafluoro phosphates and the solution of dimethyl carbonate as electrolyte, Celgard2400 microporous polypropylene membranes are barrier film, are assembled into CR2025 type buttons lithium ion battery and carry out charge and discharge Electricity, system are that constant current 0.1C is discharged to 2mV, are discharged to 1mV again with 0.01C after shelving 10 minutes, most 2V is charged to 0.1C afterwards, its test curve is obtained, referring to Fig. 2.Wherein starch base hard carbon cathode material First discharge specific capacity and first coulombic efficiency are 568.7/375.7mAh g respectively-1With 66.5%.Manganese oxide/ Starch base hard carbon composite negative pole material first charge-discharge specific capacity and first coulombic efficiency are 746.7/508.1 respectively mAh g-1With 68.0%.Manganese oxide/starch base hard carbon composite negative pole material is shown than starch base hard carbon cathode The more excellent chemical property of material.

Claims (4)

1. the preparation method of a kind of manganese oxide/starch base hard carbon composite negative pole material, it is characterised in that using as follows Preparation process：
(1), pre- carbonization：By starch, constant temperature keeps 24-48h in 200-250 DEG C of vacuum drying chamber, Obtain the pre- carbonized powder product of black；
(2) starch base hard carbon material, is prepared：By the pre- carbonized powder product obtained by above-mentioned preparation, In inert atmosphere, temperature rises to 900-1100 DEG C with 1-10 DEG C/min, is down to after keeping 1-4h with stove Room temperature, obtain starch base hard carbon material；
(3), mix：By weight by manganese salt：Starch base hard carbon material：Distilled water=5-15:100： 800 are mixed, and stirring is completely dissolved up to manganese salt, obtains mixture；
(4), hydro-thermal reaction：By mixture in hydrothermal reaction kettle, with 150-200 DEG C of heat treatment 5-15h, obtain black product；
(5) finished product, is obtained：Black product is compound through washing, being dried to obtain manganese oxide/starch base hard carbon Negative material；
Described manganese salt is one kind in potassium permanganate, manganese nitrate, manganous hydroxide.
2. preparation method as claimed in claim 1, it is characterised in that：Described inert atmosphere is nitrogen, argon One or both of gas, helium.
3. preparation method as claimed in claim 1, it is characterised in that：In described preparation starch base hard carbon material Expect in step, described temperature is 1000 DEG C.
4. preparation method as claimed in claim 1, it is characterised in that：In described hydro-thermal reaction step, Mixture is in hydrothermal reaction kettle, with 160 DEG C of heat treatment 10h.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108155023A (en) * 2017-12-25 2018-06-12 温州大学新材料与产业技术研究院 A kind of preparation method of nitrogen-phosphor codoping biological carbon/manganese compound composite material
CN112547052A (en) * 2020-12-25 2021-03-26 陕西科技大学 Manganese oxide formaldehyde degradation material, preparation method thereof and catalyst
WO2023173772A1 (en) * 2022-03-15 2023-09-21 广东邦普循环科技有限公司 Preparation method for and use of hard carbon negative electrode material

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CN104600258A (en) * 2014-12-26 2015-05-06 宁夏共享新能源材料有限公司 Composite negative pole material for lithium ion batteries and preparation method thereof
CN104992852A (en) * 2015-07-21 2015-10-21 湖北吉隆危废处理技术有限公司 A method for preparing an electrode material with graphene coated with manganese dioxide

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Publication number Priority date Publication date Assignee Title
CN101417820A (en) * 2008-09-24 2009-04-29 上海大学 Method for preparing multi-morphology nano manganese dioxide
KR20110100497A (en) * 2010-03-04 2011-09-14 (주)포스코켐텍 Carbon anode material for lithium secondary battery, method for preparing the same, and lithium secondary battery using the same
CN102059082A (en) * 2010-11-30 2011-05-18 重庆大学 Method for preparing nano manganese dioxide/carbon composite microsphere
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CN104183823A (en) * 2014-08-29 2014-12-03 华中师范大学 SnO2, MnO or Mn3O4-based composite material based on three-dimensional carbon sphere framework structure and preparation method of material
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108155023A (en) * 2017-12-25 2018-06-12 温州大学新材料与产业技术研究院 A kind of preparation method of nitrogen-phosphor codoping biological carbon/manganese compound composite material
CN112547052A (en) * 2020-12-25 2021-03-26 陕西科技大学 Manganese oxide formaldehyde degradation material, preparation method thereof and catalyst
WO2023173772A1 (en) * 2022-03-15 2023-09-21 广东邦普循环科技有限公司 Preparation method for and use of hard carbon negative electrode material

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