CN1274041C - Positive pole material of nonaqueous secondary cell and producing method thereof - Google Patents

Positive pole material of nonaqueous secondary cell and producing method thereof Download PDF

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CN1274041C
CN1274041C CNB031265553A CN03126555A CN1274041C CN 1274041 C CN1274041 C CN 1274041C CN B031265553 A CNB031265553 A CN B031265553A CN 03126555 A CN03126555 A CN 03126555A CN 1274041 C CN1274041 C CN 1274041C
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lini
lithium
cobalt
licoo
mol ratio
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CN1549365A (en
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王传福
姜占峰
董俊卿
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BYD Co Ltd
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BYD Co Ltd
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Priority to US10/823,931 priority patent/US20040191161A1/en
Priority to US10/841,760 priority patent/US20040223906A1/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
    • H01M4/04—Processes of manufacture in general
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention provides a positive pole material of lithium nickel cobalt oxides LiNi (1-x) CoxO2 wrapped by lithium cobalt oxide LiCoO2 and a preparation method thereof, wherein x is equal to or larger than 0.15 and equal to or less than 0.30. The material has the advantage of favorable discharge magnification characteristics, cycle properties of charge and discharge, safe properties and storage properties.

Description

Non-aqueous secondary batteries positive electrode and preparation method thereof
[technical field]
The present invention relates to a kind of positive electrode of non-aqueous secondary batteries, particularly a kind of lithium-nickel-cobalt-oxygen thing positive electrode that coats with lithium and cobalt oxides and preparation method thereof.
[background technology]
Present most widely used positive electrode is LiCoO in lithium rechargeable battery 2, but because cobalt resource is limited and cost an arm and a leg, thereby make LiCoO 2The use of material and battery thereof is restricted.LiNiO 2Be considered to LiCoO 2One of the most competitive substitution material.Its theoretical capacity and LiCoO 2Approaching, and its self-discharge rate is low, and environmentally safe is with LiCoO 2Compare the advantage that has on price and the resource.But LiNiO 2The synthesis condition harshness, thermal stability is relatively poor, easily causes safety issue.Therefore people attempt at LiNiO 2The middle elements such as Co, Mn, Ga, Al, F that add improve its charge/discharge capacity and cycle life to increase the stability of material.
The lithium-nickel-cobalt-oxygen thing LiNi that mixes of cobalt wherein 1-xCo xO 2(0.15≤x≤0.30, down together) material list reveals more excellent comprehensive performance.Present LiNi 1-xCo xO 2The reversible specific capacity of material can reach more than the 180mAh/g, is higher than LiCoO far away 2Material (about 140mAh/g) and LiMn 2O 4Material (about 120mAh/g) can utilize LiNi simultaneously 1-xCo xO 2The higher irreversible capacity of material provides lithium ion for negative pole SEI film forms, thereby reduces anodal extra useful load.We can say LiNi 1-xCo xO 2Material has not only possessed LiCoO 2Characteristic (easily synthetic, stable performance), more have LiNiO concurrently 2Height ratio capacity, advantage cheaply.
Though LiNi 1-xCo xO 2Material has above-mentioned advantage, but also has the part shortcoming, becomes the obstacle of this material large-scale commercial.
Thermal stability under the positive electrode charged state is the key factor that influences battery safety.The electrolyte oxidation be can cause when overcharging state when positive electrode is in, produce gas, the inner pressure of battery and the internal resistance of cell increased.With LiCoO 2And LiMn 2O 4Material is compared, LiNiO 2The thermal stability of material after taking off lithium is the poorest: Li 0.3NiO 2About 200 ℃, will decompose precipitated oxygen, Li 0.4CoO 2240 ℃ of decomposition, and λ-MnO 2Decomposition temperature be about 385 ℃.
Although LiNi 1-xCo xO 2Material does not undergo phase transition process in the charge and discharge cycles process, but still has MO 6(M=Ni, Co) octahedra along with Li +The taking off embedding of ion and slight distortion takes place, the continuous convergent-divergent of structure cell can cause active material particle that the fracture efflorescence takes place equally; In addition, under charged state, Ni, Co ion are in+4 valencys, have high reaction activity and high, and easy and organic solvent reacts, and causes MO 2The dissolving of M ion in the layer.These all can influence LiNi 1-xCo xO 2The cycle performance of material.In addition, with than heavy-current discharge the time, the quick aggravation of structure cell distortion can hinder Li +Ion take off embedding, thereby the decline of guiding discharge capacity, so LiNi 1-xCo xO 2The multiplying power discharging property of material is worse than LiCoO slightly 2Material.
LiNi 1-xCo xO 2Existing another problem of material is a shelf characteric.Because itself alkalescence is higher, in depositing process easily with airborne moisture content and carbon dioxide reaction, thereby cause the deterioration of material property, its course of reaction is:
Even LiNi at room temperature, 1-xCo xO 2Material still has Li and takes off and be embedded in material matrix surface and form lithium carbonate.Find LiNi after deliberation 1-xCo xO 2When material was placed in 25 ℃, the air of 55%RH, the conversion ratio of lithium carbonate was directly proportional with its square root of standing time in air.After placing 500h, 8% Li will change lithium carbonate into.And in the time of 675 ℃, the Li more than 70% can deviate from from basal body structure and carbon dioxide reaction, forms lithium carbonate.
Find that after deliberation above-mentioned adverse reaction and lattice distort process at first occur in material surface, so industry begins LiNi 1-xCo xO 2Material carries out surface-treated research, to improve the thermal stability and the multiplying power property of material.Open use aluminium method for coating raising LiNi in the flat 2001-143708 patent as the spy 1-xCo xO 2The stability of material.Experiment is found, after the Al coating through 15～20% molar ratios, under 25 ℃, still can keep cell safety even overcharge to 10V.
To LiNi 1-xCo xO 2The coating of the metal ion that material carries out, though can improve thermal stability, multiplying power property and the overcharging resisting ability of material, this is that specific discharge capacity with expendable material is a cost.That is to say that the metal ion covering amount reaches is enough to improve LiNi 1-xCo xO 2When the thermal stability of material, multiplying power property and overcharging resisting ability, the specific discharge capacity of material descends a lot.
[summary of the invention]
The purpose of this invention is to provide a kind of use LiCoO 2Coat LiNi 1-xCo xO 2Material and preparation method thereof, thus LiNi improved 1-xCo xO 2The thermal stability of material, multiplying power property, charge-discharge performance and shelf characteric can keep higher specific discharge capacity again simultaneously.
The objective of the invention is to be achieved through the following technical solutions:
Non-aqueous secondary batteries positive electrode of the present invention is that coated with uniform has one deck LiCoO 2LiNi 1-xCo xO 2In order to guarantee LiCoO 2Can be at the LiNi that is coated 1-xCo xO 2Particle surface forms the layer of even shell, makes LiNi 1-xCo xO 2Material has better electrochemical performance, generally requires its particle between 6～10 μ m, requires to coat the LiCoO of usefulness 2Material granule is below 1 μ m.LiCoO 2Material and LiNi 1-xCo xO 2The mol ratio of material should remain between 1～15%.
Further improve LiCoO as the present invention 2Material and LiNi 1-xCo xO 2The mol ratio of material should remain between 5～10%.
A kind of a kind of preparation method of non-aqueous secondary batteries positive electrode, it comprises the steps:
＜1〉with particle diameter is the Ni of 7～8 μ m 1-xCo x(OH) 2, 0.15≤x≤0.30, and Li 2CO 3(Ni+Co): Li=1 in molar ratio: after 1.05 ratios are fully mixed, under oxygen atmosphere, 600-750 ℃ of roasting 4-8h, 750-900 ℃ roasting 10-20 hour, obtain even structure, particle diameter is the LiNi of 8～9 μ m 1-xCo xO 2Material, 0.15≤x≤0.30;
＜2〉with the soluble salt of lithium and cobalt Li: Co=1.01 in molar ratio: 1 mixed is dissolved in the deionized water, adds acrylic acid again as intercalating agent, wherein mol ratio acrylic acid: (Li+Co)=2: 1;
＜3〉under 60-100 ℃ of stirring, slowly add the above-mentioned LiNi for preparing 1-xCo xO 2Material, 0.15≤x≤0.30, its addition is finally to make mol ratio LiNi 1-xCo xO 2: LiCoO 2=1: 0.01-0.15 continues to stir, until obtaining black-and-blue gel;
＜4〉with the gel that obtains after 80-120 ℃ of following drying, in air atmosphere, 600-850 ℃ of following roasting 0.5-2h obtains LiCoO 2The LiNi that coats 1-xCo xO 2Material, 0.15≤x≤0.30, wherein LiCoO 2Consumption is LiNi 1-xCo xO 21%～15%.
The invention has the advantages that: the present invention LiCoO 2Coat LiNi 1-xCo xO 2Positive electrode, can improve LiNi 1-xCo xO 2The thermal stability of material, multiplying power property, charge-discharge performance and shelf characteric, the while can not reduced the specific discharge capacity of material.
Below main the present invention is described in detail by embodiment.
[embodiment]
Comparative Examples
With particle diameter is the Ni of 7～8 μ m 0.8Co 0.2(OH) 2And Li 2CO 3(Ni+Co): Li=1 in molar ratio: after 1.05 ratios are fully mixed, under oxygen atmosphere, 650 ℃ of roasting 6h, 800 ℃ of roastings 16 hours obtain even structure, particle diameter is the LiNi of 8～9 μ m 0.8Co 0.2O 2Material.
Embodiment 1
With lithium acetate and cobalt acetate Li: Co=1.01 in molar ratio: 1 mixed is dissolved in the deionized water, adds acrylic acid again as intercalating agent, wherein mol ratio acrylic acid: (Li+Co)=2: 1.At 80 ℃, stir the slow down LiNi for preparing in the Comparative Examples that adds 0.8Co 0.2O 2Material finally makes mol ratio LiNi 0.8Co 0.2O 2: LiCoO 2=1: 0.01, continue to stir, until obtaining black-and-blue gel.After 120 ℃ of following dryings, in air atmosphere, 750 ℃ of following roasting 1h obtain 1%LiCoO with the gel that obtains 2The LiNi that coats 0.8Co 0.2O 2Material.
Embodiment 2
Experimentation is with embodiment 1, and difference is mol ratio LiNi 0.8Co 0.2O 2: LiCoO 2=1: 0.05, finally obtain 5%LiCoO 2The LiNi that coats 0.8Co 0.2O 2Material.
Embodiment 3
Experimentation is with embodiment 1, and difference is mol ratio LiNi 0.8Co 0.2O 2: LiCoO 2=1: 0.10, finally obtain 10%LiCoO 2The LiNi that coats 0.8Co 0.2O 2Material.
Embodiment 4
Experimentation is with embodiment 1, and difference is mol ratio LiNi 0.8Co 0.2O 2: LiCoO 2=1: 0.15, finally obtain 15%LiCoO 2The LiNi that coats 0.8Co 0.2O 2Material.
Testing of materials
Be positive electrode with the material that obtains among Comparative Examples and each embodiment respectively, the preparation battery, carry out experiment of different multiplying current discharge and charge and discharge cycles experiment, wherein the 1C/0.5C in the multiplying power property, 2C/0.5C, 3C/0.5C are the ratio of discharge-rate, and be as shown in table 1:
The chemical property of each positive electrode in table 1 example
Experiment LiCoO 2Covering amount/% 0.5C specific discharge capacity/mAh/g Multiplying power property/% 100 circulation volume surplus ratio/%
1C/0.5C 2C/0.5C 3C/0.5C
Comparative Examples 0 181 95 86 65 84
Embodiment 1 1 181 95 87 68 88
Embodiment 2 5 180 98 94 80 95
Embodiment 3 10 179 98 95 82 96
Embodiment 4 15 168 99 96 83 96
Battery after the charging is disintegrated, scrape the positive electrode drying after, carry out the experiment of positive electrode charging back material breakdown temperature, this experiment is used difference formula to scan calorimetric (DSC) and is measured its decomposition temperature, heating rate is 5 ℃/min, experimental result is as shown in table 2:
Each positive electrode charging back material breakdown temperature in table 2 example
Experiment Comparative Examples Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
LiCoO 2Covering amount/% 0 1 5 10 15
Decomposition temperature/℃ 198.2 200.7 235.0 236.5 238.4
It is in the air ambient of 55%RH that prepared positive electrode is placed on 25 ℃, humidity, regularly uses atomic absorption spectrum (AAS) to measure its lithium content, and experimental result is as shown in table 3:
Each positive electrode contains the lithium amount after placing in table 3 example
Experiment LiCoO 2Covering amount/% Contain lithium amount/% 25 ℃, 55%RH air placement back residue/%
0h 50h 100h 250h 500h
Comparative Examples 0 7.11 100 97.5 96.5 94.4 91.8
Embodiment 1 1 7.11 100 97.8 96.9 95.2 93.2
Embodiment 2 5 7.10 100 99.8 99.7 99.4 99.2
Embodiment 3 10 7.11 100 99.8 99.8 99.6 99.5
Embodiment 4 15 7.10 100 99.9 99.8 99.7 99.6
Data from table 1,2,3 are worked as LiCoO as can be seen 2Covering amount is 5% when above, LiNi 0.8Co 0.2O 2Discharge-rate characteristic, cycle performance, security performance and the shelf characteric of material all improves greatly.When covering amount greater than 10% the time, LiNi 0.8Co 0.2O 2The performance boost of material is little, but its specific discharge capacity decline is more.

Claims (3)

1. non-aqueous secondary batteries positive electrode is characterized in that: this material is for chemical formula LiNi 1-xCo xO 2The lithium-nickel-cobalt-oxygen thing of expression is a kernel, 0.15≤x≤0.30 wherein, and the surface is coated with one deck lithium and cobalt oxides LiCoO 2, wherein lithium-nickel-cobalt-oxygen thing particle diameter is 6～10 μ m, and the lithium and cobalt oxides particle diameter is below 1 μ m, and the mol ratio consumption of lithium and cobalt oxides is 1～15% of a lithium-nickel-cobalt-oxygen thing.
2. as right 1 described non-aqueous secondary batteries positive electrode, wherein the mol ratio consumption of lithium and cobalt oxides is 5～10% of a lithium-nickel-cobalt-oxygen thing.
3. a kind of preparation method of non-aqueous secondary batteries positive electrode as claimed in claim 1 is characterized in that comprising:
＜1〉with particle diameter is the Ni of 7～8 μ m 1-xCo x(OH) 2, 0.15≤x≤0.30, and Li 2CO 3(Ni+Co): Li=1 in molar ratio: after 1.05 ratios are fully mixed, under oxygen atmosphere, 600-750 ℃ of roasting 4-8h, 750-900 ℃ roasting 10-20 hour, obtain even structure, particle diameter is the LiNi of 8～9 μ m 1-xCo xO 2Material, 0.15≤x≤0.30;
＜2〉with the soluble salt of lithium and cobalt Li: Co=1.01 in molar ratio: 1 mixed is dissolved in the deionized water, adds acrylic acid again as intercalating agent, wherein mol ratio acrylic acid: (Li+Co)=2: 1;
＜3〉under 60-100 ℃ of stirring, slowly add the above-mentioned LiNi for preparing 1-xCo xO 2Material, 0.15≤x≤0.30, its addition is finally to make mol ratio LiNi 1-xCo xO 2: LiCoO 2=1: 0.01-0.15 continues to stir, until obtaining black-and-blue gel;
＜4〉with the gel that obtains after 80-120 ℃ of following drying, in air atmosphere, 600-850 ℃ of following roasting 0.5-2h obtains LiCoO 2The LiNi that coats 1-xCo xO 2Material, 0.15≤x≤0.30, wherein LiCoO 2The mol ratio consumption be LiNi 1-xCo xO 21%～15%.
CNB031265553A 2002-11-19 2003-05-09 Positive pole material of nonaqueous secondary cell and producing method thereof Expired - Lifetime CN1274041C (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CNB031265553A CN1274041C (en) 2003-05-09 2003-05-09 Positive pole material of nonaqueous secondary cell and producing method thereof
US10/823,931 US20040191161A1 (en) 2002-11-19 2004-04-14 Compounds of lithium nickel cobalt metal oxide and the methods of their fabrication
US10/841,760 US20040223906A1 (en) 2003-05-09 2004-05-08 Lithium nickel cobalt oxides and their methods of fabrication

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB031265553A CN1274041C (en) 2003-05-09 2003-05-09 Positive pole material of nonaqueous secondary cell and producing method thereof

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CN1274041C true CN1274041C (en) 2006-09-06

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Publication number Priority date Publication date Assignee Title
CN1855587B (en) * 2005-04-28 2010-05-05 比亚迪股份有限公司 Battery anode preparation method and preparation method of lithium ion batteries using the battery anode
CN101916848A (en) * 2010-08-06 2010-12-15 山东久力电子科技有限公司 LiFePO4 coating LiMn2O4 composite electrode material and preparation method thereof
JP2016534521A (en) * 2013-09-09 2016-11-04 ユニヴェルシテ・カトリック・ドゥ・ルーヴァン Hybrid electrode for non-aqueous electrolyte secondary battery
CN104733723A (en) * 2015-02-11 2015-06-24 江苏科捷锂电池有限公司 Preparation method for LiCoO2-coated modified ternary cathode material

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