CN103606657A - Lithium ion battery zinc oxide/porous carbon composite negative electrode material with high capacity and preparation method thereof - Google Patents

Lithium ion battery zinc oxide/porous carbon composite negative electrode material with high capacity and preparation method thereof Download PDF

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Publication number
CN103606657A
CN103606657A CN201310665385.9A CN201310665385A CN103606657A CN 103606657 A CN103606657 A CN 103606657A CN 201310665385 A CN201310665385 A CN 201310665385A CN 103606657 A CN103606657 A CN 103606657A
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porous carbon
zinc oxide
lithium ion
ion battery
carbon composite
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穆道斌
沈雪阳
陈实
吴锋
吴伯荣
黄荣
赵章宏
陶丹
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GAOPING TANGYIXIN NEW ENERGY TECHNOLOGY Co Ltd
Beijing Institute of Technology BIT
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GAOPING TANGYIXIN NEW ENERGY TECHNOLOGY Co Ltd
Beijing Institute of Technology BIT
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Priority to CN201310665385.9A priority Critical patent/CN103606657A/en
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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
    • 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
    • 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 relates to a zinc oxide/porous carbon negative electrode material for a lithium ion battery with high capacity and a preparation method thereof, and belongs to the technical field of chemical industry electrode materials. A solvothermal method is adopted, porous carbon is dispersed in a mixed alcohol solution with zinc acetate, then sodium hydroxide is added to react for 24 hours at the temperature of 140DEG C, a product is washed by deionized water and filtered until the pH of the filter solution is neutral, a filter cake is dried to obtain the zinc oxide/porous carbon composite negative electrode material with a nanometer porous structure. The method is simple and easy, the preparation parameters are strong in controllability, the product has the nanometer porous structure, a buffering space is provided for the volume expansion of the zinc oxide, the conductivity of the material is enhanced by introducing the carbon, when the material is used as a negative electrode material of the lithium ion battery, the charging-discharging capacity is high, and the cycling performance is good (when the current density is 100mAg<-1>, the reversible capacity of the lithium ion battery is 653.7mAhg<-1> after the lithium ion battery is circularly charged and discharged for 100 circles).

Description

Lithium ion battery zinc oxide/porous carbon composite negative pole material of a kind of high power capacity and preparation method thereof
Technical field
The present invention relates to lithium ion battery zinc oxide/porous carbon composite negative pole material of a kind of high power capacity and preparation method thereof, belong to chemical industry electrode material technical field.
Background technology
Zinc oxide (ZnO), as a kind of functional material, has been widely used in solar cell, photoelectric device and zinc-nickel cell, also has very high theoretical capacity 978mAhg during as lithium ion battery negative material -1, the graphite negative electrodes material (372mAhg that this numerical value is used higher than nowadays commercialization far away -1), discharge voltage plateau is higher, and preparation method is simply various, and cost of material is cheap, has good prospect and potentiality.But up to now,, zinc oxide does not obtain practical on lithium ion battery, even paid close attention on a large scale as laboratory research yet.This is because ZnO exists very serious bulk effect when as lithium ion battery negative material, causes rapid attenuation and the battery failure of capacity.At present the improvement of ZnO negative material chemical property is mainly comprised the preparation of the coated and zno-based composite material of carbon, but result of study shows certain progress reversible capacity still reaches far away its theoretical level, so zno-based negative material also has very large room for promotion.
Porous carbon is that a class has the material with carbon element that enriches flourishing pore structure, has larger specific area, good conductivity and structural stability.Adopt inorganic substances CaCO 3as template, gelatin is that carbon source can make porous carbon, and its aperture can reach 30-50nm, very suitable to carrier material.Therefore can be using porous carbon as a kind of buffer medium, can be to a certain extent for the volumetric expansion of ZnO provides a space, avoid caving in and fragmentation of material structure, improve the stable circulation performance of zno-based negative material.
Summary of the invention
To the object of the invention is that existing lithium ion battery zinc oxide negative material cyclical stability is poor, capacity attenuation is fast and the dissatisfactory problem of conductivity in order solving, lithium ion battery zinc oxide/porous carbon composite negative pole material of a kind of high power capacity and preparation method thereof to be provided.
The object of the invention is to be achieved through the following technical solutions.
Lithium ion battery zinc oxide/porous carbon composite negative pole material of a kind of high power capacity of the present invention, is comprised of zinc oxide and porous carbon, with the gross mass of this composite material, calculates, and the quality percentage composition of each several part is:
Zinc oxide 5%-95%;
Porous carbon 95%-5%.
The preparation method of lithium ion battery zinc oxide/porous carbon composite negative pole material of a kind of high power capacity of the present invention, concrete preparation process is as follows:
Step 1, by zinc acetate (Zn (CH 3cOO) 22H 2o) join in alcoholic solution, stir it is dissolved completely, obtain solution;
In step 2, the solution that obtains to step 1, add successively porous carbon and NaOH; In temperature, be to react under the condition of 50～250 ℃, until react completely;
Step 3, after step 2 has been reacted, washing suction filtration is neutral to filtrate pH, by suction filtration product vacuum drying, obtains having zinc oxide/porous carbon composite material of nano-porous structure.
Described in step 1, alcohols comprises polyethylene glycol, ethanol and ethylene glycol, and the mixed liquor that in them, both mix with arbitrary proportion arbitrarily;
In step 1, the concentration of acetic acid zinc solution is 0.001～1gmL -1.
In step 2, the aperture of porous carbon is 1nm-5um.
In step 2, the mass ratio of porous carbon and zinc acetate is 1:0.05-10.
In step 2, the mass ratio of NaOH and zinc acetate is 1:0.01-10;
Beneficial effect
1, the lithium ion battery of a kind of high power capacity of the present invention zinc oxide/porous carbon composite negative pole material, there is nano-porous structure, alleviated to a certain extent the volumetric expansion of zinc oxide, the simultaneously introducing of carbon has strengthened the conductivity of material and electrically contacting of electrode, shows high charging and discharging capacity and good cycle performance (is 100mAg in current density during as lithium ion battery negative material -1discharge and recharge under system, the reversible capacity after 100 weeks that circulates is 653.7mAhg -1), to compare with pure ZnO negative material, capacity attenuation phenomenon has obtained obvious improvement, and cyclical stability is greatly improved, and has certain promotional value and application prospect.
2, the preparation method of the lithium ion battery of a kind of high power capacity of the present invention zinc oxide/porous carbon composite negative pole material, preparation is simple, and preparation parameter controllability is strong, and raw material is cheap pollution-free.
Accompanying drawing explanation
Fig. 1 is the XRD figure of zinc oxide/porous carbon composite negative pole material;
Fig. 2 is the SEM figure of zinc oxide-65/ porous carbon composite negative pole material;
Fig. 3 is the SEM figure of zinc oxide-54/ porous carbon composite negative pole material;
Fig. 4 is the SEM figure of zinc oxide-33/ porous carbon composite negative pole material;
Fig. 5 is that zinc oxide/porous carbon composite negative pole material is at 100mAg -1the charge and discharge cycles discharge curve of 100 weeks.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is elaborated
Embodiment 1
Lithium ion battery zinc oxide/porous carbon composite negative pole material of a kind of high power capacity of the present invention, is comprised of zinc oxide and porous carbon, with the gross mass of this composite material, calculates, and the quality percentage composition of each several part is:
Zinc oxide 54%;
Porous carbon 46%.
Lithium ion battery zinc oxide/porous carbon composite negative pole material of a kind of high power capacity and preparation method thereof, concrete preparation process is as follows:
1) take 2gZn (CH 3cOO) 22H 2o adds in the mixed solution of 14mL polyethylene glycol and 76mL absolute ethyl alcohol, and magnetic agitation is fully dissolved it;
2) in above-mentioned solution, add the porous carbon of 0.5g, stir 15 minutes;
3) above-mentioned reactant is moved in the polytetrafluoroethylene cup that 0.7gNaOH is housed, at 140 ℃, react 24h;
4) reaction finishes rear cool to room temperature, takes out product and is washed till neutrality with distilled water, dries, and obtains having zinc oxide/porous carbon composite material of nano-porous structure.
Zinc oxide/porous carbon composite material prepared by said method is applied to carry out charging and discharging capacity and cycle performance test after lithium ion battery negative material: zinc oxide/porous carbon materials and conductive agent Super.P, binding agent Kynoar (PVDF) the by mass percentage ratio of 60%:20%:20% are mixed and made into electrode slice as work electrode, lithium metal is to electrode, the LiF of 1mol/L 6/ EC-DMC (volume ratio 1: 1) is electrolyte, in argon gas atmosphere glove box, is assembled into simulated battery.Simulated battery is carried out to charge-discharge test, and voltage range is 0.01～3V (vs.Li +/ Li), current density is 100mAg -1.
Test result: in zinc oxide/porous carbon composite negative pole material, the mass fraction of zinc oxide is 54%, the mass fraction of porous carbon is 46%, pattern is as shown in Figure 3.In zinc oxide/porous carbon composite negative pole material, the mass fraction of zinc oxide is 33%, and the mass fraction of porous carbon is 67%.Zinc oxide/porous carbon composite negative pole material is at 100mAg -1the charge and discharge cycles discharge curve of 100 weeks as shown in Figure 5, is 100mAg in current density -1time, after circulating 100 weeks, reversible capacity is 653.7mAhg -1, compare pure zinc oxide electrode capacity characteristic and stable circulation performance is greatly improved.
Embodiment 2
Lithium ion battery zinc oxide/porous carbon composite negative pole material of a kind of high power capacity of the present invention, is comprised of zinc oxide and porous carbon, with the gross mass of this composite material, calculates, and the quality percentage composition of each several part is:
Zinc oxide: 65%;
Porous carbon: 35%.
Lithium ion battery zinc oxide/porous carbon composite negative pole material of a kind of high power capacity and preparation method thereof, concrete preparation process is as follows:
1) take 2gZn (CH 3cOO) 22H 2o adds in 90mL polyglycol solution, and magnetic agitation is fully dissolved it;
2) in above-mentioned solution, add the porous carbon of 0.25g, stir 15 minutes;
3) above-mentioned reactant is moved in the polytetrafluoroethylene cup that 0.7gNaOH is housed, at 140 ℃, react 24h;
4) reaction finishes rear cool to room temperature, takes out product and is washed till neutrality with distilled water, dries, and obtains having zinc oxide/porous carbon composite material of nano-porous structure.
Zinc oxide/porous carbon composite material prepared by said method is applied to carry out charging and discharging capacity and cycle performance test after lithium ion battery negative material: zinc oxide/porous carbon materials and conductive agent Super.P, binding agent Kynoar (PVDF) the by mass percentage ratio of 60%:20%:20% are mixed and made into electrode slice as work electrode, lithium metal is to electrode, the LiF of 1mol/L 6/ EC-DMC (volume ratio 1: 1) is electrolyte, in argon gas atmosphere glove box, is assembled into simulated battery.Simulated battery is carried out to charge-discharge test, and voltage range is 0.01～3V (vs.Li +/ Li), current density is 100mAg -1.
Test result: in zinc oxide/porous carbon composite negative pole material, the mass fraction of zinc oxide is 65%, the mass fraction of porous carbon is 35%, shape appearance figure is as shown in Figure 2.Zinc oxide/porous carbon composite negative pole material is at 100mAg -1the charge and discharge cycles discharge curve of 100 weeks as shown in Figure 5, is 100mAg in current density -1time, after circulating 100 weeks, reversible capacity is 375.7mAhg -1, compare pure zinc oxide electrode capacity characteristic and stable circulation performance has obtained certain lifting.
Embodiment 3
Lithium ion battery zinc oxide/porous carbon composite negative pole material of a kind of high power capacity of the present invention, is comprised of zinc oxide and porous carbon, with the gross mass of this composite material, calculates, and the quality percentage composition of each several part is:
Zinc oxide 33%;
Porous carbon 67%.
Lithium ion battery zinc oxide/porous carbon composite negative pole material of a kind of high power capacity and preparation method thereof, concrete preparation process is as follows:
1) take 2gZn (CH 3cOO) 22H 2o adds in 90mL polyglycol solution, and magnetic agitation is fully dissolved it;
2) in above-mentioned solution, add the porous carbon of 1g, stir 15 minutes;
3) above-mentioned reactant is moved in the polytetrafluoroethylene cup that 0.7gNaOH is housed, at 140 ℃, react 24h;
4) reaction finishes rear cool to room temperature, takes out product and is washed till neutrality with distilled water, dries, and obtains having zinc oxide/porous carbon composite material of nano-porous structure.
Zinc oxide/porous carbon composite material prepared by said method is applied to carry out charging and discharging capacity and cycle performance test after lithium ion battery negative material: zinc oxide/porous carbon materials and conductive agent Super.P, binding agent Kynoar (PVDF) the by mass percentage ratio of 60%:20%:20% are mixed and made into electrode slice as work electrode, lithium metal is to electrode, the LiF of 1mol/L 6/ EC-DMC (volume ratio 1: 1) is electrolyte, in argon gas atmosphere glove box, is assembled into simulated battery.Simulated battery is carried out to charge-discharge test, and voltage range is 0.01～3V (vs.Li +/ Li), current density is 100mAg -1.
Test result: in zinc oxide/porous carbon composite negative pole material, the mass fraction of zinc oxide is 33%, the mass fraction of porous carbon is 67%, shape appearance figure is as shown in Figure 4.Zinc oxide/porous carbon composite negative pole material is at 100mAg -1the charge and discharge cycles discharge curve of 100 weeks as shown in Figure 5, is 100mAg in current density -1time, after circulating 100 weeks, reversible capacity is 450.2mAhg -1, compare pure zinc oxide electrode capacity characteristic and stable circulation performance is greatly improved.

Claims (7)

1. the lithium ion battery of high power capacity zinc oxide/porous carbon composite negative pole material, is characterized in that: zinc oxide and porous carbon, consist of; Gross mass with this composite material is calculated, and the shared quality percentage composition of zinc oxide is 5%-95%; All the other are porous carbon.
2. a preparation method for the lithium ion battery of high power capacity zinc oxide/porous carbon composite negative pole material, is characterized in that: concrete preparation process is as follows:
Step 1, by zinc acetate (Zn (CH 3cOO) 22H 2o) join in alcoholic solution, stir it is dissolved completely, obtain solution;
In step 2, the solution that obtains to step 1, add successively porous carbon and NaOH; In temperature, be to react under the condition of 50～250 ℃, until react completely;
Step 3, after step 2 has been reacted, washing suction filtration is neutral to filtrate pH, by suction filtration product vacuum drying, obtains having zinc oxide/porous carbon composite material of nano-porous structure.
3. the preparation method of the lithium ion battery of a kind of high power capacity as claimed in claim 2 zinc oxide/porous carbon composite negative pole material, it is characterized in that: described in step 1, alcohols comprises polyethylene glycol, ethanol and ethylene glycol, and the mixed liquor that in them, both mix with arbitrary proportion arbitrarily.
4. the preparation method of the lithium ion battery of a kind of high power capacity as claimed in claim 2 zinc oxide/porous carbon composite negative pole material, is characterized in that: in step 1, the concentration of acetic acid zinc solution is 0.001～1gmL -1.
5. the preparation method of the lithium ion battery of a kind of high power capacity as claimed in claim 2 zinc oxide/porous carbon composite negative pole material, is characterized in that: in step 2, the aperture of porous carbon is 1nm-5um.
6. the preparation method of the lithium ion battery of a kind of high power capacity as claimed in claim 2 zinc oxide/porous carbon composite negative pole material, is characterized in that: in step 2, the mass ratio of porous carbon and zinc acetate is 1:0.05-10.
7. the preparation method of the lithium ion battery of a kind of high power capacity as claimed in claim 2 zinc oxide/porous carbon composite negative pole material, is characterized in that: in step 2, the mass ratio of NaOH and zinc acetate is 1:0.01-10.
CN201310665385.9A 2013-12-10 2013-12-10 Lithium ion battery zinc oxide/porous carbon composite negative electrode material with high capacity and preparation method thereof Pending CN103606657A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104183837A (en) * 2014-07-09 2014-12-03 浙江大学 Carbon network supported zinc oxide nanocrystalline composite material and preparation method and application thereof
CN104201361A (en) * 2014-08-29 2014-12-10 合肥国轩高科动力能源股份公司 Preparation method of zinc oxide quantum dot negative electrode material coated with multilevel structure carbon
CN107394151A (en) * 2017-07-18 2017-11-24 大连理工大学 A kind of preparation method of the nickel zinc battery cathode material based on porous carbon nanocapsule in-stiu coating zinc oxide
CN107464923A (en) * 2017-07-19 2017-12-12 成都理工大学 A kind of compound high-capacity lithium ion cell material of nano zine oxide/porous carbon in situ and preparation method thereof
CN109273669A (en) * 2018-10-10 2019-01-25 南京邮电大学 A kind of super integrated flexible cathode of lithium ion battery and preparation method thereof
CN110289401A (en) * 2019-05-28 2019-09-27 超威电源有限公司 A kind of lead storage battery cathode carbon composite and cathode lead plaster, lead storage battery
CN112864365A (en) * 2021-04-20 2021-05-28 杭州芳闻新型材料有限公司 Nitrogen-sulfur co-doped porous carbon loaded zinc oxide negative electrode material and preparation method thereof

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CN102867943A (en) * 2011-07-04 2013-01-09 东台天祥新能源有限公司 Preparation method and application method for zinc cathode active material of zinc-nickel secondary battery

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CN1724138A (en) * 2005-06-22 2006-01-25 中山大学 Porous carbon adsorbing agent containing nano zinc oxide micropartical and its preparation process and application
CN102867943A (en) * 2011-07-04 2013-01-09 东台天祥新能源有限公司 Preparation method and application method for zinc cathode active material of zinc-nickel secondary battery

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104183837A (en) * 2014-07-09 2014-12-03 浙江大学 Carbon network supported zinc oxide nanocrystalline composite material and preparation method and application thereof
CN104201361A (en) * 2014-08-29 2014-12-10 合肥国轩高科动力能源股份公司 Preparation method of zinc oxide quantum dot negative electrode material coated with multilevel structure carbon
CN107394151A (en) * 2017-07-18 2017-11-24 大连理工大学 A kind of preparation method of the nickel zinc battery cathode material based on porous carbon nanocapsule in-stiu coating zinc oxide
CN107394151B (en) * 2017-07-18 2019-10-11 大连理工大学 A kind of preparation method of the nickel zinc battery cathode material based on porous carbon nanocapsule in-stiu coating zinc oxide
CN107464923A (en) * 2017-07-19 2017-12-12 成都理工大学 A kind of compound high-capacity lithium ion cell material of nano zine oxide/porous carbon in situ and preparation method thereof
CN109273669A (en) * 2018-10-10 2019-01-25 南京邮电大学 A kind of super integrated flexible cathode of lithium ion battery and preparation method thereof
CN110289401A (en) * 2019-05-28 2019-09-27 超威电源有限公司 A kind of lead storage battery cathode carbon composite and cathode lead plaster, lead storage battery
CN112864365A (en) * 2021-04-20 2021-05-28 杭州芳闻新型材料有限公司 Nitrogen-sulfur co-doped porous carbon loaded zinc oxide negative electrode material and preparation method thereof

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Application publication date: 20140226