CN106252641B - Ternary cathode material of lithium ion battery and preparation method are covered in carbon and ceria double-contracting - Google Patents

Ternary cathode material of lithium ion battery and preparation method are covered in carbon and ceria double-contracting Download PDF

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CN106252641B
CN106252641B CN201610941053.2A CN201610941053A CN106252641B CN 106252641 B CN106252641 B CN 106252641B CN 201610941053 A CN201610941053 A CN 201610941053A CN 106252641 B CN106252641 B CN 106252641B
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cathode material
ceria
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carbon
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CN106252641A (en
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刘慧勇
管浩
吴宏
任璐
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Fuzhou University
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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • 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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides 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
    • H01M4/36—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
    • 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
    • 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
    • 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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Abstract

The invention discloses a kind of carbon and ceria double-contracting to cover ternary cathode material of lithium ion battery and preparation method.The chemical formula of the tertiary cathode material is LiaNixCoyMnzO2, wherein 0.9<a<1.5,4<x<7,1<y<4,2<z<5, x+y+z=10；The present invention is to carry out coating modification to positive electrode using carbon and ceria, the performance of comprehensive carbon and metal oxide, material electronics electrical conductivity and its stability with electrolyte under high voltages are improved, best cladding ratio is sought, the material prepared has better high rate performance and cycle performance.

Description

Ternary cathode material of lithium ion battery and preparation method are covered in carbon and ceria double-contracting
Technical field
The invention belongs to energy storage material preparation fields, and in particular to a kind of carbon and the double coated lithium ion batteries three of ceria First positive electrode and preparation method.
Background technique
Mainstream power battery of the lithium battery as future development, many advantages not having with conventional batteries and has larger Skill upgrading and cost decline space.Therefore 2013 ~ 2015 years countries issue subsidy policy to new-energy automobile, illustrate country The attention that it is developed.
And research hotspot one of of the ternary material as anode material of lithium battery, with capacity is high, thermal stability is good, price The advantages that relative moderate, lower toxicity, but there is also first charge-discharge efficiencies not high, positive electrode and electrolyte solution occur it is anti- It answers, poor circulation, electronic conductivity are low etc. insufficient restricts its development.Surface cladding be exactly improve above-mentioned insufficient method it One, the contact area and the generation of side reaction of active material and electrolyte can be effectively reduced by coating, and prevent metal ion Dissolution in the electrolytic solution prevents the variation of particle volume in circulation, effectively improves the chemical property of material.
CeO2Cladding can effectively inhibit the side reaction between positive electrode and electrolyte, improve its cyclical stability；Carbon packet The electronic conductivity that can improve material is covered, and low in raw material price is easy to get.
Summary of the invention
It is an object of that present invention to provide a kind of carbon and ceria double-contracting to cover ternary cathode material of lithium ion battery and preparation Method；Best covering amount is found out by the double dominant for combining carbon coating and ceria to coat, improving electronic conductivity improves The deficiency of its poor circulation improves capacity and high rate performance.
The present invention solves technical solution used by above-mentioned technical problem：
A kind of carbon and ceria double-contracting are covering ternary described in ternary cathode material of lithium ion battery and preparation method just The chemical formula of pole material is LiaNixCoyMnzO2, wherein 0.9<a<1.5,0.4<x<0.7,0.1<y<0.4,0.2<z<0.5, x+y+ z=1；The double-contracting cover in ternary cathode material of lithium ion battery the mass ratio of ceria and tertiary cathode material be 0.001 ~ 0.05:1, the mass ratio of carbon and tertiary cathode material is 0.001 ~ 0.05:1.
Cladding process is：Positive electrode → ceria cladding → carbon coating → double-contracting coated positive pole material.Specifically include with Lower step：
（1）The cladding of ceria
A, with deionized water dissolving cerium salt；
B, tertiary cathode material is added, is mixed at 20 ~ 100 DEG C until solution evaporates, then dry 5 at 80 ~ 150 DEG C ~ 15 hours；
C, the obtained powder of step B is placed in tube furnace, 1 ~ 6h is calcined at 400 ~ 800 DEG C, obtains ceria packet The tertiary cathode material covered.
（2）Carbon coated
A, carbon source is dissolved in 50 ~ 100 DEG C of hot deionized waters, the tertiary cathode material of ceria cladding is added, no Disconnected stirring until at dark thick substance, calcine under 300 ~ 600 DEG C of air atmospheres be made within 30 ~ 90 minutes pair coating modification lithiums from Sub- positive electrode.
Cerium salt is cerous nitrate or cerium chloride in step (1), and dioxy in ternary cathode material of lithium ion battery is covered in gained double-contracting The mass ratio for changing cerium and positive electrode is 0.001 ~ 0.05:1.
Carbon source in step (2) is one or more of PVA, sucrose, glucose, the double coated lithium ion batteries three of gained The mass ratio of carbon and positive electrode is 0.001 ~ 0.05 in first positive electrode:1.
Compared to the prior art, the present invention has the following advantages：
1. the present invention, which sufficiently combines carbon coating, which can improve material electronics electrical conductivity and ceria, can improve electrode material With the respective advantage of the stability of electrolyte under high voltages, covered effect is better than single layer cladding.
2. the sample after present invention cladding does not change its prototype structure and generates without miscellaneous phase, the material after coating Show lesser cationic mixing degree.
3. double coated lithium ion batteries prepared by the present invention have higher capacity, high rate performance and cycle performance.
Detailed description of the invention
Fig. 1 is that XRD analysis figure before and after tertiary cathode material is covered in double-contracting in the embodiment of the present invention 1.
Fig. 2 is that tertiary cathode material SEM photograph is covered in double-contracting in the embodiment of the present invention 1.
Fig. 3 is that discharge curve for the first time is covered under tertiary cathode material different multiplying in double-contracting in the embodiment of the present invention 1.
Fig. 4 is that discharge cycles song of the tertiary cathode material front and back under 0.2C multiplying power is covered in double-contracting in the embodiment of the present invention 1 Line.
Specific embodiment
Combined with specific embodiments below, it further illustrates, but these case study on implementation are merely to illustrate the present invention and do not have to In limiting the scope of the invention, after reading this disclosure, the modification of various equivalent forms belongs to the claim of this application institute The range of restriction.
Embodiment 1
The preparation method of ternary cathode material of lithium ion battery is covered in a kind of carbon and ceria double-contracting comprising following step Suddenly：
(1) 1 g cerous nitrate is added in the beaker of 1000ml, 300ml deionized water stirring and dissolving is added, be added 20gLiNi0.5Co0.2Mn0.3O2Positive electrode, the magnetic agitation at 80 DEG C is until solution evaporates, at 120 DEG C of obtained powder very It is 10 hours dry in empty drying box, the powder after drying is placed in tube furnace at 700 DEG C under air atmosphere and is calcined five hours, is obtained The lithium ion anode material coated to ceria.
(2) 2gPVA is dissolved in 90 DEG C of the deionized water of heat, is then added（1）Resulting materials obtain suspension, with Ceaselessly stir, solution is evaporated up to black gelatinous mass and obtains, by air in obtained 400 DEG C of pipe type furnaces of gelatinous mass It is calcined 30 minutes under atmosphere, obtains the lithium ion anode material that double-contracting is covered.
(3) the positive electrode LiNi for covering double-contracting obtained0.5Co0.2Mn0.3O2With uncoated LiNi0.5Co0.2Mn0.3O2 Respectively with conductive agent SP, KS-6, binder PVDF in mass ratio 85:5:5:5 ratios are uniformly mixed, and appropriate -2 pyrrole of 1- methyl is added It is made into slurry within pyrrolidone ball milling 2 hours to be evenly coated on aluminium flake collector, drying, tabletting.Then button is assembled into glove box Formula battery, discharge capacity is 171mAh/g to the material after coating for the first time under 0.2C multiplying power, decays to 162 after 50 circulations MAh/g capacity retention rate is 94%.
(4) lithium ion anode material LiNi is covered to double-contracting obtained with X-ray diffractometer (XRD)0.5Co0.2Mn0.3O2With The LiNi not coated0.5Co0.2Mn0.3O2Bulk material carries out X-ray diffraction, and diffracting spectrum is not as shown in Figure 1, the two has Additional symbols cladding process does not influence material structure, and Fig. 2 is material SEM figure, can be clearly seen from figure LiNi0.5Co0.2Mn0.3O2Ontology is smooth, but the material surface after coating uniformly is scattered the little particle of covering material.Fig. 3 Be charge-discharge magnification from 0.2C to 1C when cladding after material discharging specific capacity.
Fig. 4 is the cyclic curve under 0.2C multiplying power, it can be seen that material after the coating capacity after 50 circulations declines Lapse rate is about 6%, and the material capacity attenuation rate of pure phase reaches 13%.
Embodiment 2
The preparation method of ternary cathode material of lithium ion battery is covered in a kind of carbon and ceria double-contracting comprising following step Suddenly：
(1) 1.2 g cerous nitrates are added in the beaker of 1000ml, 300ml deionized water stirring and dissolving is added, be added 20gLiNi0.5Co0.2Mn0.3O2Positive electrode, the magnetic agitation at 80 DEG C is until solution evaporates, at 120 DEG C of obtained powder very It is 10 hours dry in empty drying box, the powder after drying is placed in tube furnace at 700 DEG C under air atmosphere and is calcined five hours, is obtained The lithium ion anode material coated to ceria.
(2) 1.5gPVA is dissolved in 90 DEG C of the deionized water of heat, is then added（1）Resulting materials obtain suspension, With ceaselessly stirring, solution is evaporated up to black gelatinous mass and obtains, and obtained 400 DEG C of pipe type furnaces of gelatinous mass are hollow Atmosphere encloses lower calcining 30 minutes, obtains the lithium ion anode material of double coating modifications.
(3) the positive electrode LiNi for covering double-contracting obtained0.5Co0.2Mn0.3O2With uncoated LiNi0.5Co0.2Mn0.3O2 Respectively with conductive agent SP, KS-6, binder PVDF in mass ratio 85:5:5:5 ratios are uniformly mixed, and appropriate -2 pyrrole of 1- methyl is added It is made into slurry within pyrrolidone ball milling 2 hours to be evenly coated on aluminium flake collector, drying, tabletting.Then button is assembled into glove box Formula battery, discharge capacity is 165.5mAh/g to the material after coating for the first time under 0.2C multiplying power, is decayed to after 50 circulations 153.0 mAh/g capacity retention rates are 92.4%.
Embodiment 3
The preparation method of ternary cathode material of lithium ion battery is covered in a kind of carbon and ceria double-contracting comprising following step Suddenly：
(1) 0.8 g cerous nitrate is added in the beaker of 1000ml, 300ml deionized water stirring and dissolving is added, be added 20gLiNi0.5Co0.2Mn0.3O2Positive electrode, the magnetic agitation at 80 DEG C is until solution evaporates, at 120 DEG C of obtained powder very It is 10 hours dry in empty drying box, the powder after drying is placed in tube furnace at 700 DEG C under air atmosphere and is calcined five hours, is obtained The lithium ion anode material coated to ceria.
(2) 2.1gPVA is dissolved in 90 DEG C of the deionized water of heat, is then added（1）Resulting materials obtain suspension, With ceaselessly stirring, solution is evaporated up to black gelatinous mass and obtains, and obtained 400 DEG C of pipe type furnaces of gelatinous mass are hollow Atmosphere encloses lower calcining 30 minutes, obtains the lithium ion anode material of double coating modifications.
(3) the positive electrode LiNi for covering double-contracting obtained0.5Co0.2Mn0.3O2With uncoated modification LiNi0.5Co0.2Mn0.3O2Respectively with conductive agent SP, KS-6, binder PVDF in mass ratio 85:5:5:5 ratios are uniformly mixed, and are added Enter appropriate -2 pyrrolidones ball milling of 1- methyl and be made within 2 hours slurry to be evenly coated on aluminium flake collector, drying, tabletting.Then exist Button cell is assembled into glove box, the material after coating under 0.2C multiplying power for the first time discharge capacity be 162.0mAh/g, 50 It is 91.2% that 147.8 mAh/g capacity retention rates are decayed to after secondary circulation.
Embodiment 4
The preparation method of ternary cathode material of lithium ion battery is covered in a kind of carbon and ceria double-contracting comprising following step Suddenly：
(1) 1 g cerous nitrate is added in the beaker of 1000ml, 300ml deionized water stirring and dissolving is added, be added 20gLiNi0.5Co0.2Mn0.3O2Positive electrode, the magnetic agitation at 80 DEG C is until solution evaporates, at 120 DEG C of obtained powder very It is 10 hours dry in empty drying box, the powder after drying is placed in tube furnace at 700 DEG C under air atmosphere and is calcined five hours, is obtained The lithium ion anode material coated to ceria.
(2) 1.5gPVA is dissolved in 90 DEG C of the deionized water of heat, is then added（1）Resulting materials obtain suspension, With ceaselessly stirring, solution is evaporated up to black gelatinous mass and obtains, and obtained 400 DEG C of pipe type furnaces of gelatinous mass are hollow Atmosphere encloses lower calcining 30 minutes, obtains the lithium ion anode material of double coating modifications.
(3) the positive electrode LiNi for covering double-contracting obtained0.5Co0.2Mn0.3O2With uncoated modification LiNi0.5Co0.2Mn0.3O2Respectively with conductive agent SP, KS-6, binder PVDF in mass ratio 85:5:5:5 ratios are uniformly mixed, and are added Enter appropriate -2 pyrrolidones ball milling of 1- methyl and be made within 2 hours slurry to be evenly coated on aluminium flake collector, drying, tabletting.Then exist Button cell is assembled into glove box, the material after coating under 0.2C multiplying power for the first time discharge capacity be 160.0mAh/g, 50 It is 90.8% that 145.3 mAh/g capacity retention rates are decayed to after secondary circulation.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, is all covered by the present invention.

Claims (3)

1. the preparation method that ternary cathode material of lithium ion battery is covered in a kind of carbon and ceria double-contracting, which is characterized in that described Tertiary cathode material chemical formula be LiaNixCoyMnzO2, wherein 0.9<a<1.5,0.4<x<0.7,0.1<y<0.4,0.2<z< 0.5, x+y+z=1；The mass ratio of ceria and tertiary cathode material in ternary cathode material of lithium ion battery is covered in the double-contracting It is 0.001 ~ 0.05:1, the mass ratio of carbon and tertiary cathode material is 0.001 ~ 0.05:1；
The carbon and ceria double-contracting covers the preparation method of ternary cathode material of lithium ion battery, includes the following steps：
(1) ceria coats
A, with deionized water dissolving cerium salt；
B, tertiary cathode material is added, is mixed at 20 ~ 100 DEG C until solution evaporates, then dry 5 ~ 15 at 80 ~ 150 DEG C Hour；
C, the obtained powder of step B is placed in tube furnace, 1 ~ 6h is calcined at 400 ~ 800 DEG C, obtain ceria cladding Tertiary cathode material；
(2) carbon coating
A, carbon source is dissolved in 50 ~ 100 DEG C of hot deionized waters, the tertiary cathode material of ceria cladding is added, constantly stirs It mixes until calcining obtained double-contracting in 30 ~ 90 minutes at dark thick substance under 300 ~ 600 DEG C of air atmospheres and covering lithium ion anode material Material.
2. the preparation side that ternary cathode material of lithium ion battery is covered in a kind of carbon according to claim 1 and ceria double-contracting Method, which is characterized in that cerium salt is cerous nitrate or cerium chloride in step (1), and ternary cathode material of lithium ion battery is covered in gained double-contracting The mass ratio of middle ceria and tertiary cathode material is 0.001 ~ 0.05:1.
3. the preparation side that ternary cathode material of lithium ion battery is covered in a kind of carbon according to claim 1 and ceria double-contracting Method, which is characterized in that carbon source is one or more of PVA, sucrose, glucose in step (2), and lithium-ion electric is covered in gained double-contracting The mass ratio of carbon and tertiary cathode material is 0.001 ~ 0.05 in the tertiary cathode material of pond:1.
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