CN1300870C - Electrolytic manganese dioxide for doped modified lithium manganese dioxide buttery - Google Patents

Electrolytic manganese dioxide for doped modified lithium manganese dioxide buttery Download PDF

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CN1300870C
CN1300870C CNB2004100610583A CN200410061058A CN1300870C CN 1300870 C CN1300870 C CN 1300870C CN B2004100610583 A CNB2004100610583 A CN B2004100610583A CN 200410061058 A CN200410061058 A CN 200410061058A CN 1300870 C CN1300870 C CN 1300870C
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manganese dioxide
mno
sio
property
lithium manganese
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CN1619865A (en
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王圣平
代江华
杨问华
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China University of Geosciences
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China University of Geosciences
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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
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Primary Cells (AREA)

Abstract

The present invention relates to industrial material of batteries, particularly to doping modified electrolytic manganese dioxide for lithium manganese dioxide batteries, which comprises gamma-MnO 2. The present invention is characterized in that the present invention is mixed with one kind or more than two kinds of mixtures in V2O5, SiO2 and Bi2O3. When one kind or more than two kinds of the mixtures in the V2O5, the SiO2 and the Bi2O3 are mixed, the ingredients have the weight percentages that the weight percentage of the V2O5 is 0.3 to 12.5 percent, the weight percentage of the SiO2 is 0.12 to 10.0 percent, and the weight percentage of the Bi2O3 is 0.01 to 6.0 percent. The content sum of the weight percentages of the ingredients is 100 percent, and the ingredients are formed by mixing and calcination. Because the gamma-MnO2 adopted by the present invention is in a layer-shaped structure which is regulated and analysed by adding the V2O5, the SiO2 and the Bi2O3 which are non-metallic oxide so as to be convenient for lithium ions to be inserted into the layer-shaped structure, and thereby, the electrochemical activity of the manganese dioxide is increased, the electrochemical polarization of battery reaction is reduced, and the discharge capacity of batteries is obviously increased.

Description

A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property
Technical field
The present invention relates to a kind of battery industry material, particularly a kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property.
Background technology
The electrical property of lithium-manganese dioxide electrochemical system battery depends primarily on cathode material manganese dioxide, especially the heavy load discharge performance and the discharge capacity of battery.Existing technology is to put into production after the high-temperature calcination modification with the manganese dioxide after the direct electrolysis.
The main performance of current battery has certain difference with external like product, and other technological level difference is little, and the lithium-manganese dioxide electrochemical system battery of prior art polarizes easily, and its electro-chemical activity of single manganese dioxide is not high.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of raising manganese bioxide electrochemical activity at the deficiency of prior art existence, the lithium manganese dioxide cell electrochemical polarization is reduced, the lithium manganese dioxide cell electrolytic manganese dioxide of the doping vario-property of the discharge capacity of raising battery.
The present invention is that the technical scheme that the problem of the above-mentioned proposition of solution adopts is: a kind of lithium manganese dioxide cell of doping vario-property electrolytic manganese dioxide comprises γ-MnO 2, it is characterized in that: also be mixed with V 2O 5, SiO 2, Bi 2O 3In the above mixture of any one or any two, V 2O 5, SiO 2, Bi 2O 3In any one or any two during above the mixing the shared percentage by weight of each component be:
V 2O 50.3～12.5%, SiO 20.12～10.0%, Bi 2O 30.01～6.0%, γ-MnO 2With V 2O 5, SiO 2, Bi 2O 3In the percentage by weight sum of any one or any two above mixture be 100%, form through mixed calcining.
Described γ-MnO 2In be mixed with V 2O 5, SiO 2And Bi 2O 3, each component and weight percentage thereof are:
V 2O 50.3～12.5%, SiO 20.12～10.0%, Bi 2O 30.01～6.0%, γ-MnO 271.5～99.57%, described component weight percent content sum is 100%, forms through mixed calcining.
Described γ-MnO 2In be mixed with V 2O 5, SiO 2And Bi 2O 3, each component and weight percentage thereof are:
V 2O 52.0～10.0%, SiO 22.0～8.0%, Bi 2O 32.0～5.0% γ-MnO 280.0～94.0%, described component weight percent content sum is 100%, forms through mixed calcining.
Described γ-MnO 2In be mixed with V 2O 5, SiO 2And Bi 2O 3, each component and weight percentage thereof are:
V 2O 55.0%, SiO 25.0%, Bi 2O 32.0%, γ-MnO 288.0%, form through mixed calcining.
Beneficial effect of the present invention is: because γ-MnO that lithium manganese dioxide cell adopts 2Be layer structure, by adding nonmetal oxide V 2O 5, SiO 2, Bi 2O 3Regulate γ-MnO 2, β-MnO 2The crystal layer structure, being convenient to lithium ion inserts in the layer structure better, thereby can improve the electro-chemical activity of manganese dioxide in lithium manganese dioxide cell, reduce the activation polarization of cell reaction, improve significantly discharge capacity and the heavy load ability of battery.
The present invention is at γ-MnO 2In mix V 2O 5, SiO 2And Bi 2O 3, having significantly improved the manganese bioxide electrochemical activity, the average discharge capacity of battery is brought up to 51.6h, 1548mAh by existing 44.9h, 1347mAh.
Description of drawings
Fig. 1 is the part of production flow chart of existing C R123A battery
Embodiment
The invention will be further described below by embodiment and comparative example, but the present invention is not limited only to these examples.The present invention is on the existing technical foundation of processing electrolytic manganese dioxide technology, before high-temperature calcination with V 2O 5, SiO 2, Bi 2O 3In the above metal oxide of any one or any two be mixed in the manganese dioxide powder.
The electrochemical system of lithium manganese dioxide cell is:
Li|LiClO 4+PC+DME+DIOX|MnO 2
Cell electrochemical reaction is:
Embodiment 1:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property, it is by γ-MnO 2, V 2O 5, SiO 2And Bi 2O 3Form, at γ-MnO 2Mix nonmetal oxide V in the powder 2O 5, SiO 2And Bi 2O 3, the each component percentage by weight is V 2O 51.25%, SiO 25%, Bi 2O 33%, γ-MnO 290.75%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product in 24 hours.
The lithium manganese dioxide cell of doping vario-property is assembled the CR123A Experimental cell with electrolytic manganese dioxide according to the manufacturing technique requirent of prior art CR123A battery, do blank contrast to producing normal Modified Electrolytic Manganese Dioxide simultaneously, see Table 1.
The part of production of existing C R123A battery is as follows:
1. technological process, as shown in Figure 1.
2. manganese dioxide heat treatment temperature and time
Under 375 ℃ of conditions, handled electrolytic manganese dioxide 24 hours with 500 ℃ of air dry ovens;
3. positive pole and powder
Prescription, manganese dioxide: aquadag: acetylene carbon black: tetrafluoro: alcohol=46.5kg: 1.8kg: 1.7kg: 3.5L: 2L requires to mix.
4. electrolyte
Prescription: 1mol/l LiClO 4PC (propene carbonate), DME (glycol dimethyl ether) and the mixed solution (wherein volume ratio PC50%, DME20%, DIOX30%) of DIOX (dioxolanes), electric liquid water content:＜0.2mg/ml, every battery electrolyte amount 3.0g.
5. manganese dioxide positive pole pole piece technology
Length (210 ± 0.5mm), and width (24 ± 0.2mm), weight (6.7-7.8g).
6. lithium band cathode pole piece technology
Length (230.5 ± 0.5mm), width (22 ± 0.1mm).
7. battery capacity is according to IEC standard (IEC60086-2) discharge, promptly under 23 ± 2 ℃ of conditions 100 Ω constant-resistance discharges to 2.0V.
Table 1
The lithium manganese dioxide cell of the doping vario-property Experimental cell of electrolytic manganese dioxide Produce the Experimental cell of normal modification electrolytic manganese dioxide
Sequence number Discharge capacity Average discharge capacity Sequence number Discharge capacity Average discharge capacity
1 58.3h 51.6h 1548mAh 1 49.3h 44.9h 1347mAh
2 53.1h 2 41.3h
3 49.7h 3 39.8h
4 46.5h 4 46.5h
5 51.0h 5 47.2h
6 57.6h 6 47.3h
7 48.3h 7 43.9h
8 48.4h 8 44.1h
9 52.2h 9 44.7h
IEC standard 40h (1200mAh)
Embodiment 2:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property, it is by γ-MnO 2, V 2O 5, SiO 2And Bi 2O 3Form, at γ-MnO 2Mix nonmetal oxide V in the powder 2O 5, SiO 2And Bi 2O 3, the each component percentage by weight is V 2O 52.5%, SiO 20.12%, Bi 2O 35.7%, γ-MnO 291.68%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
With the manufacturing technique requirent assembling CR123A Experimental cell of product according to prior art CR123A battery, battery detecting situation such as table 2.
Table 2
The lithium manganese dioxide cell of the doping vario-property Experimental cell of electrolytic manganese dioxide
Sequence number Discharge capacity Average discharge capacity
1 51.7h
2 44.4h 50.1h 1503mAh
3 51.3h
4 48.9h
5 52.3h
6 52.4h
7 55.7h
8 45.5h
9 48.7h
IEC standard 40h (1200mAh)
Embodiment 3:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property, it is by γ-MnO 2, V 2O 5, SiO 2And Bi 2O 3Form, at γ-MnO 2Mix nonmetal oxide V in the powder 2O 5, SiO 2And Bi 2O 3, the each component percentage by weight is V 2O 512.5%, SiO 20.3%, Bi 2O 30.03%, γ-MnO 297.17%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
With the manufacturing technique requirent assembling CR123A Experimental cell of product according to prior art CR123A battery, battery detecting situation such as table 3.
Table 3
The lithium manganese dioxide cell of the doping vario-property Experimental cell of electrolytic manganese dioxide
Sequence number Discharge capacity Average discharge capacity
1 59.1h 51.2h 1536mAh
2 47.7h
3 46.3h
4 53.8h
5 52.4h
6 47.6h
7 49.9h
8 48.7h
9 55.3h
IEC standard 40h (1200mAh)
Embodiment 4:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide V in the powder 2O 5, SiO 2And Bi 2O 3, the each component percentage by weight is V 2O 50.3%, SiO 20.12%, Bi 2O 30.01%, γ-MnO 299.57%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 5:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide V in the powder 2O 5, SiO 2And Bi 2O 3, the each component percentage by weight is V 2O 512.5%, SiO 210.0%, Bi 2O 36.0%, γ-MnO 271.5%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 6:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide V in the powder 2O 5, SiO 2And Bi 2O 3, the each component percentage by weight is V 2O 52.0%, SiO 22.0%, Bi 2O 32.0%, γ-MnO 294.0%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 7:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide V in the powder 2O 5, SiO 2And Bi 2O 3, the each component percentage by weight is V 2O 510.0%, SiO 28.0%, Bi 2O 35.0%, γ-MnO 277%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 8:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide V in the powder 2O 5, the each component percentage by weight is V 2O 50.3%, γ-MnO 299.7%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 9:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide V in the powder 2O 5, the each component percentage by weight is V 2O 512.5%, γ-MnO 287.5%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 10:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide SiO in the powder 2, the each component percentage by weight is SiO 20.12%, γ-MnO 299.88%; The mixing back is handled under 375 ℃ of conditions with 500 ℃ of air dry ovens and was got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 11:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide SiO in the powder 2, the each component percentage by weight is SiO 210.0%, γ-MnO 290.0%; The mixing back is handled under 375 ℃ of conditions with 500 ℃ of air dry ovens and was got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 12:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide Bi in the powder 2O 3, the each component percentage by weight is Bi 2O 30.01%, γ-MnO 299.99%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 13:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide Bi in the powder 2O 3, the each component percentage by weight is Bi 2O 36.0%, γ-MnO 294.0%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 14:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide V in the powder 2O 5, and SiO 2, the each component percentage by weight is V 2O 50.3%, SiO 20.12%, γ-MnO 299.58%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 15:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide V in the powder 2O 5, and SiO 2, the each component percentage by weight is V 2O 512.5%, SiO 210.0%, γ-MnO 277.5%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 16:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide SiO in the powder 2And Bi 2O 3, the each component percentage by weight is SiO 20.12%, Bi 2O 30.01%, γ-MnO 299.87%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.
Embodiment 17:
A kind of lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property is at γ-MnO 2Mix nonmetal oxide SiO in the powder 2And Bi 2O 3, the each component percentage by weight is SiO 210.0%, Bi 2O 36.0%, γ-MnO 284.0%; Mix rear under 375 ℃ of conditions, the processing with 500 ℃ of air dry ovens and got product---the lithium manganese dioxide cell electrolytic manganese dioxide of doping vario-property in 24 hours.

Claims (4)

1. the lithium manganese dioxide cell electrolytic manganese dioxide of a doping vario-property comprises γ-MnO 2, it is characterized in that: also be mixed with V 2O 5, SiO 2, Bi 2O 3In the above mixture of any one or any two, V 2O 5, SiO 2, Bi 2O 3In any one or any two during above the mixing the shared percentage by weight of each component be:
V 2O 50.3～12.5%, SiO 20.12～10.0%, Bi 2O 30.01～6.0%, γ-MnO 2With V 2O 5, SiO 2, Bi 2O 3In the percentage by weight sum of any one or any two above mixture be 100%, form through mixed calcining.
2. the lithium manganese dioxide cell electrolytic manganese dioxide of a kind of doping vario-property according to claim 1 is characterized in that: described γ-MnO 2In be mixed with V 2O 5, SiO 2And Bi 2O 3, each component and weight percentage thereof are:
V 2O 50.3～12.5%, SiO 20.12～10.0%, Bi 2O 30.01～6.0%, γ-MnO 271.5～99.57%, described component weight percent content sum is 100%, forms through mixed calcining.
3. the lithium manganese dioxide cell electrolytic manganese dioxide of a kind of doping vario-property according to claim 1 and 2 is characterized in that: described γ-MnO 2In be mixed with V 2O 5, SiO 2And Bi 2O 3, each component and weight percentage thereof are:
V 2O 52.0～10.0%, SiO 22.0～8.0%, Bi 2O 32.0～5.0% γ-MnO 280.0～94.0%, described component weight percent content sum is 100%, forms through mixed calcining.
4. the lithium manganese dioxide cell electrolytic manganese dioxide of a kind of doping vario-property according to claim 3 is characterized in that: described γ-MnO 2In be mixed with V 2O 5, SiO 2And Bi 2O 3, each component and weight percentage thereof are:
V 2O 55.0%, SiO 25.0%, Bi 2O 32.0%, γ-MnO 288.0%, form through mixed calcining.
CNB2004100610583A 2004-11-08 2004-11-08 Electrolytic manganese dioxide for doped modified lithium manganese dioxide buttery Expired - Fee Related CN1300870C (en)

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CN102013527B (en) * 2009-09-08 2012-08-29 清华大学深圳研究生院 Rechargeable zinc ion battery
CN103579604A (en) * 2013-11-07 2014-02-12 广西桂柳化工有限责任公司 Modification treatment method of electrolytic manganese dioxide used for lithium battery
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
CN109201044B (en) * 2018-11-14 2020-11-10 中国科学院过程工程研究所 Potassium-doped gamma manganese dioxide catalyst and preparation method and application thereof
CN113772736B (en) * 2021-09-16 2023-04-07 清华大学 Composite metal oxide, preparation method and application thereof, and iodine removal method
CN114497504B (en) * 2022-01-28 2023-11-03 惠州亿纬锂能股份有限公司 Lithium primary battery positive electrode active material, and preparation method and application thereof

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