CN103606673A - Preparation method of laminar-spinel compound sosoloid anode material - Google Patents

Preparation method of laminar-spinel compound sosoloid anode material Download PDF

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CN103606673A
CN103606673A CN201310564159.1A CN201310564159A CN103606673A CN 103606673 A CN103606673 A CN 103606673A CN 201310564159 A CN201310564159 A CN 201310564159A CN 103606673 A CN103606673 A CN 103606673A
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positive electrode
lithium
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CN103606673B (en
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刘云建
高彦涌
窦爱春
潘凌理
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Jiangsu 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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • 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 Kinetics & Catalysis (AREA)
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Abstract

The invention relates to a lithium-rich sosoloid anode material and particularly relates to a preparation method of a laminar-spinel compound sosoloid anode material. The preparation method comprises the following steps: preparing Li0.5+xNi0.25Mn0.75O2+x/2 by adopting an ultrasonic outer field-assisted coprecipitation method, wherein x is greater than 0 and less than 1; weighing lithium salt and titanium salt according to a chemical metering ratio of Li4Ti5O12, weighing excessive 20% of organic chelating agent according to the chemical metering ratio, dissolving the lithium salt, the titanium salt and the organic chelating agent into aqueous liquor, and stirring at 50 DEG C-90 DEG C to form gel; dispersing a proper proportion of Li0.5+xNi0.25Mn0.75O2+x/2 powder into the gel until a solvent is evaporated into gel; and finally, drying the gel and roasting for 1 hour -12 hours in an air atmosphere of 500 DEG C-800 DEG C, and cooling to obtain the anode material. Li4Ti5O12-coated Li0.5+xNi0.25Mn0.75O2+x/2 anode material prepared by the preparation method disclosed by the invention effectively improves surface transmission of the lithium ion anode material by utilizing the Li4Ti5O12 with quick ion conductivity as a coating, so that rate capability of the material is improved.

Description

A kind of preparation method of stratiform-spinelle composite solid solution positive electrode
Technical field
The present invention relates to a kind of rich lithium solid solution cathode material, refer in particular to a kind of preparation method of stratiform-spinelle composite solid solution positive electrode, belong to new energy materials field.
Background technology
In recent years, rich lithium solid solution cathode material Li 1.5ni 0.25mn 0.75o 2.5because it has higher specific discharge capacity, cycle performance is better, and energy density is high, forms the study hotspot into people, is considered to the first-selected positive electrode of lithium-ion-power cell for New Generation of Electric Vehicle.
Along with going deep into of research, it is found that Li 1.5ni 0.25mn 0.75o 2.5although positive electrode has higher specific discharge capacity and energy density, also exist the shortcomings such as coulombic efficiency is lower first, and high rate performance is poor, these shortcomings have had a strong impact on Li 1.5ni 0.25mn 0.75o 2.5positive electrode is in the application in electric automobile field.
At Li 1.5ni 0.25mn 0.75o 2.5in the study on the modification of positive electrode, find spinel-type LiNi 0.5mn 1.5o 4positive electrode belongs to cubic system, has special three-dimensional lithium ion diffusion admittance, has ensured that it has good high rate performance, due to LiNi 0.5mn 1.5o 4and Li 1.5ni 0.25mn 0.75o 2.5there is identical oxygen accumulation mode, and can utilize identical presoma (nickel manganese mol ratio is 1:3) and synthetic method to be prepared, the M. M. Thackeray spinel-type LiNi that takes the lead in having proposed to utilize 0.5mn 1.5o 4to layed solid-solution Li 1.5ni 0.25mn 0.75o 2.5carry out the method for modification, and prepared novel lamellar-spinelle composite solid solution positive electrode Li 0.5+xni 0.25mn 0.75o 2+x/2(0<x<1), this material has stratiform and spinel structure simultaneously, combines LiNi 0.5mn 1.5o 4and Li 1.5ni 0.25mn 0.75o 2.5charge-discharge characteristic, and there is higher discharge capacity, coulombic efficiency and good cycle performance first, be therefore expected to become lithium ion power battery cathode material of new generation.
But research finds that novel stratiform-spinelle composite solid solution positive electrode also exists following shortcoming: material operating voltage is higher, SEI is thicker on surface, affect lithium ion in surperficial transmission, and then affect the high rate performance of positive electrode, be therefore necessary this material to carry out further modification.
Summary of the invention
The invention provides a kind of stratiform-spinelle composite solid solution positive electrode Li of finishing type 0.5+xni 0.25mn 0.75o 2+x/2(0<x<1) and preparation method thereof, concrete summary of the invention is as follows:
1. first adopt the auxiliary coprecipitation of ultrasonic external field to prepare stratiform-spinelle composite solid solution positive electrode Li 0.5+xni 0.25mn 0.75o 2+x/2(0<x<1): the precipitation reagent that takes nickel salt, manganese salt and excessive 20% according to stoichiometric proportion, be mixed with certain density solution, by ultrasonic external field, assist coprecipitation, control suitable temperature and pH value, prepare presoma, then and the lithium salts taking by stoichiometric proportion mix, through mechanical activation 1-12h, roasting 1-12h at 400-600 ℃, roasting 8-24h at 750-900 ℃ again, last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains 0.5+xni 0.25mn 0.75o 2+x/2(0<x<1).
2. Li 4ti 5o 12the preparation of coated composite solid solution positive electrode: according to Li 4ti 5o 12stoichiometric proportion take lithium salts and titanium salt, weigh the organic sequestering agent by stoichiometric proportion excessive 20%, by the water-soluble solution of lithium salts, titanium salt and organic sequestering agent, and stir into gel at 50-90 ℃; Stratiform-spinelle composite solid solution positive electrode Li of proper proportion 0.5+xni 0.25mn 0.75o 2+x/2(0<x<1) powder is scattered in colloidal sol, until solvent flashes to gel; Finally will after gel drying, in the air atmosphere of 500-800 ℃, calcine 1-12h again, obtain Li after cooling 4ti 5o 12coated stratiform-spinelle composite solid solution positive electrode Li 0.5+xni 0.25mn 0.75o 2+x/2(0<x<1).
3. in above-mentioned steps 1, nickel salt is nickelous sulfate, nickel chloride, nickel nitrate or nickel acetate; Manganese salt is manganese sulfate, manganese chloride, manganese nitrate or manganese acetate; Precipitation reagent is NaOH, potassium hydroxide, sodium carbonate or potash; Lithium salts is lithium hydroxide, lithium carbonate, lithium nitrate or lithium acetate; The concentration of nickel salt, the concentration of cobalt salt, the concentration of manganese salt and the concentration of precipitation reagent are 0.1-1mol/L; The temperature of co-precipitation is 50-90 ℃, and pH value is 7.0-13.0.
4. in above-mentioned steps 2, lithium salts is lithium hydroxide, lithium carbonate, lithium nitrate or lithium acetate, and titanium salt is Ti (C 4h 9o) 4, organic sequestering agent is oxalic acid, citric acid or ethylene glycol.
5. at Li 4ti 5o 12coated Li 0.5+xni 0.25mn 0.75o 2+x/2in positive electrode, Li 4ti 5o 12mass fraction be Li 4ti 5o 12coated Li 0.5+xni 0.25mn 0.75o 2+x/2the 0.1-5% of positive electrode gross mass.
By said method, the Li of preparation 4ti 5o 12coated Li 0.5+xni 0.25mn 0.75o 2+x/2positive electrode, this material is because utilization has the Li of fast ion conduction 4ti 5o 12as coating, effectively improved lithium ion at Li 0.5+xni 0.25mn 0.75o 2+x/2the transmission on positive electrode surface, and then improved its high rate performance.
Accompanying drawing explanation
Accompanying drawing 1 is Li 4ti 5o 12coated Li 0.5+xni 0.25mn 0.75o 2+x/2positive electrode SEM figure;
Accompanying drawing 2 is Li 0.5+xni 0.25mn 0.75o 2+x/2the figure of electric discharge first before and after positive electrode is coated;
Accompanying drawing 3 is Li 0.5+xni 0.25mn 0.75o 2+x/2high rate performance figure before and after positive electrode is coated;
As can be seen from Figure 1, there is the nano level particle of one deck in the positive electrode surface after being coated, as can be seen from Figure 2, positive electrode after coated, discharge capacity has obtained obvious increase first, and as can be seen from Figure 3, the high rate performance of coated rear positive electrode has obtained obvious improvement.
Embodiment
Specific embodiment is as follows:
Embodiment 1: by stoichiometric proportion, take the NaOH of nickelous sulfate and manganese sulfate and excessive 20%, be mixed with the solution of 0.1mol/L, by ultrasonic external field, assist coprecipitation, aqueous temperature is controlled to 50 ℃, pH value is controlled at 7.0, prepares presoma; Then mix with lithium carbonate, through mechanical activation 1h, roasting 1h at 400 ℃, then at 750 ℃ roasting 8h, last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains 1.1ni 0.25mn 0.75o 2.3; Then according to Li 4ti 5o 12stoichiometric proportion take lithium acetate and Ti (C 4h 9o) 4, selecting is organic sequestering agent by the oxalic acid of stoichiometric proportion excessive 20%, by lithium acetate, Ti (C 4h 9o) 4in the water-soluble solution of oxalic acid, and stir into gel at 50 ℃, stratiform-spinelle composite solid solution positive electrode Li of proper proportion 1.1ni 0.25mn 0.75o 2.3powder is scattered in colloidal sol, until solvent flashes to gel; Finally will after gel drying, in the air atmosphere of 500 ℃, calcine 1h again, obtain Li after cooling 4ti 5o 12coated stratiform-spinelle composite solid solution positive electrode Li 1.1ni 0.25mn 0.75o 2.3, control Li 4ti 5o 12covering amount be 0.1%.
Embodiment 2: by stoichiometric proportion, take the KOH of nickel chloride and manganese chloride and excessive 20%, be mixed with the solution of 1mol/L, by ultrasonic external field, assist coprecipitation, aqueous temperature is controlled to 90 ℃, pH value is controlled at 13.0, prepares presoma; Then mix with lithium acetate, through mechanical activation 12h, roasting 12h at 600 ℃, then at 900 ℃ roasting 24h, last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains 1.3ni 0.25mn 0.75o 2.4; Then according to Li 4ti 5o 12stoichiometric proportion take lithium acetate and Ti (C 4h 9o) 4, selecting is organic sequestering agent by the citric acid of stoichiometric proportion excessive 20%, by their water-soluble solution, and stirs into gel at 90 ℃, stratiform-spinelle composite solid solution positive electrode Li of proper proportion 1.3ni 0.25mn 0.75o 2.4powder is scattered in colloidal sol, until solvent flashes to gel, finally will after gel drying, calcine 12h again in the air atmosphere of 800 ℃, obtains Li after cooling 4ti 5o 12coated stratiform-spinelle composite solid solution positive electrode Li 1.3ni 0.25mn 0.75o 2.4.Control Li 4ti 5o 12covering amount be 5%.
Embodiment 3: the Na that takes nickel nitrate and manganese nitrate and excessive 20% by stoichiometric proportion 2cO 3be mixed with the solution of 0.5mol/L, by ultrasonic external field, assist coprecipitation, aqueous temperature is controlled to 70 ℃, pH value is controlled at 10.0, prepare presoma, then mix with lithium hydroxide, through mechanical activation 6h, roasting 6h at 500 ℃, roasting 24h at 900 ℃ again, last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains 1.2ni 0.25mn 0.75o 2.35, then according to Li 4ti 5o 12stoichiometric proportion take lithium carbonate and Ti (C 4h 9o) 4, selecting is organic sequestering agent by the ethylene glycol of stoichiometric proportion excessive 20%, by their water-soluble solution, and stirs into gel at 75 ℃.Stratiform-spinelle composite solid solution positive electrode Li of proper proportion 1.2ni 0.25mn 0.75o 2.35powder is scattered in colloidal sol, until solvent flashes to gel, finally will after gel drying, calcine 6h again in the air atmosphere of 600 ℃, obtains Li after cooling 4ti 5o 12coated stratiform-spinelle composite solid solution positive electrode Li 1.2ni 0.25mn 0.75o 2.35, control Li 4ti 5o 12covering amount be 2.5%.
Embodiment 4: the NaOH that takes nickelous sulfate and manganese sulfate and excessive 20% by stoichiometric proportion, be mixed with the solution of 0.2mol/L, by ultrasonic external field, assist coprecipitation, aqueous temperature is controlled to 60 ℃, pH value is controlled at 9.0, prepare presoma, then mix with lithium carbonate, through mechanical activation 4h, roasting 1h at 500 ℃, roasting 12h at 850 ℃ again, last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains 1.42ni 0.25mn 0.75o 2.46; Then according to Li 4ti 5o 12stoichiometric proportion take lithium acetate and Ti (C 4h 9o) 4, selecting is organic sequestering agent by the citric acid of stoichiometric proportion excessive 20%, by their water-soluble solution, and stirs into gel at 60 ℃, stratiform-spinelle composite solid solution positive electrode Li of proper proportion 1.42ni 0.25mn 0.75o 2.45powder is scattered in colloidal sol, until solvent flashes to gel, finally will after gel drying, calcine 8h again in the air atmosphere of 600 ℃, obtains Li after cooling 4ti 5o 12coated stratiform-spinelle composite solid solution positive electrode Li 1.42ni 0.25mn 0.75o 2.46.Control Li 4ti 5o 12covering amount be 3%.

Claims (3)

1. a preparation method for stratiform-spinelle composite solid solution positive electrode, described positive electrode is Li 4ti 5o 12coated Li 0.5+xni 0.25mn 0.75o 2+x/2positive electrode, 0<x<1; Li 4ti 5o 12mass fraction be the 0.1-5% of positive electrode quality,
It is characterized in that preparation method is as follows:
(1) first adopt the auxiliary coprecipitation of ultrasonic external field to prepare stratiform-spinelle composite solid solution positive electrode Li 0.5+xni 0.25mn 0.75o 2+x/20<x<1: the precipitation reagent that takes nickel salt, manganese salt and excessive 20% according to stoichiometric proportion, be mixed with certain density solution, by ultrasonic external field, assist coprecipitation, control suitable temperature and pH value, prepare presoma, then and the lithium salts taking by stoichiometric proportion mix, through mechanical activation 1-12h, roasting 1-12h at 400-600 ℃, roasting 8-24h at 750-900 ℃ again, last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains 0.5+xni 0.25mn 0.75o 2+x/2;
(2) Li 4ti 5o 12the preparation of coated composite solid solution positive electrode: according to Li 4ti 5o 12stoichiometric proportion take lithium salts and titanium salt, weigh the organic sequestering agent by stoichiometric proportion excessive 20%, by the water-soluble solution of lithium salts, titanium salt and organic sequestering agent, and stir into gel at 50-90 ℃; Stratiform-spinelle composite solid solution positive electrode Li of proper proportion 0.5+xni 0.25mn 0.75o 2+x/2powder is scattered in colloidal sol, until solvent flashes to gel; Finally will after gel drying, in the air atmosphere of 500-800 ℃, calcine 1-12h again, obtain Li after cooling 4ti 5o 12coated stratiform-spinelle composite solid solution positive electrode Li 0.5+xni 0.25mn 0.75o 2+x/2.
2. the preparation method of a kind of stratiform-spinelle composite solid solution positive electrode as claimed in claim 1, is characterized in that: in step 1, nickel salt is nickelous sulfate, nickel chloride, nickel nitrate or nickel acetate; Manganese salt is manganese sulfate, manganese chloride, manganese nitrate or manganese acetate; Precipitation reagent is NaOH, potassium hydroxide, sodium carbonate or potash; Lithium salts is lithium hydroxide, lithium carbonate, lithium nitrate or lithium acetate; The concentration of nickel salt, the concentration of cobalt salt, the concentration of manganese salt and the concentration of precipitation reagent are 0.1-1mol/L; The temperature of co-precipitation is 50-90 ℃, and pH value is 7.0-13.0.
3. the preparation method of a kind of stratiform-spinelle composite solid solution positive electrode as claimed in claim 1, is characterized in that: in step 2, lithium salts is lithium hydroxide, lithium carbonate, lithium nitrate or lithium acetate, and titanium salt is Ti (C 4h 9o) 4, organic sequestering agent is oxalic acid, citric acid or ethylene glycol.
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Cited By (10)

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CN103872328A (en) * 2014-03-12 2014-06-18 南通瑞翔新材料有限公司 Positive electrode active material for lithium ion secondary battery and preparation method for positive electrode active material
CN103943846A (en) * 2014-04-18 2014-07-23 江苏大学 Preparation method of lithium ion battery positive-electrode material precursor
CN103943845A (en) * 2014-04-18 2014-07-23 江苏大学 Preparation method of layered-spinel composite solid solution positive-electrode material
CN104218241A (en) * 2014-09-30 2014-12-17 奇瑞汽车股份有限公司 Lithium ion battery anode lithium-rich material modification method
CN105428637A (en) * 2014-09-18 2016-03-23 宁德时代新能源科技有限公司 Lithium ion battery, positive electrode material of lithium ion battery and preparation method for positive electrode material
CN105932250A (en) * 2016-06-03 2016-09-07 中南大学 Preparation method and application of metal doped spinel structured and fast ionic conductor coated nickel-containing cathode material
CN109904402A (en) * 2017-12-11 2019-06-18 中国科学院大连化学物理研究所 A kind of lithium-rich manganese base material and its preparation and application
CN113871589A (en) * 2021-09-16 2021-12-31 南开大学 Lithium-rich manganese-based positive electrode material coated with lithium titanate assisted by molten salt and preparation method thereof
CN114094060A (en) * 2021-10-08 2022-02-25 中南大学 Preparation method of high-voltage positive electrode material with core-shell structure
CN116177624A (en) * 2023-03-20 2023-05-30 合肥工业大学 Simple preparation method of high-nickel ternary positive electrode material with spinel structure coating layer

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Publication number Priority date Publication date Assignee Title
CN103872328A (en) * 2014-03-12 2014-06-18 南通瑞翔新材料有限公司 Positive electrode active material for lithium ion secondary battery and preparation method for positive electrode active material
CN103943846B (en) * 2014-04-18 2016-11-23 江苏大学 A kind of preparation method of precursor of lithium ionic cell positive material
CN103943846A (en) * 2014-04-18 2014-07-23 江苏大学 Preparation method of lithium ion battery positive-electrode material precursor
CN103943845A (en) * 2014-04-18 2014-07-23 江苏大学 Preparation method of layered-spinel composite solid solution positive-electrode material
CN105428637A (en) * 2014-09-18 2016-03-23 宁德时代新能源科技有限公司 Lithium ion battery, positive electrode material of lithium ion battery and preparation method for positive electrode material
CN105428637B (en) * 2014-09-18 2019-03-29 宁德时代新能源科技股份有限公司 Lithium ion battery and preparation method of anode material thereof
CN104218241A (en) * 2014-09-30 2014-12-17 奇瑞汽车股份有限公司 Lithium ion battery anode lithium-rich material modification method
CN105932250A (en) * 2016-06-03 2016-09-07 中南大学 Preparation method and application of metal doped spinel structured and fast ionic conductor coated nickel-containing cathode material
CN109904402A (en) * 2017-12-11 2019-06-18 中国科学院大连化学物理研究所 A kind of lithium-rich manganese base material and its preparation and application
CN113871589A (en) * 2021-09-16 2021-12-31 南开大学 Lithium-rich manganese-based positive electrode material coated with lithium titanate assisted by molten salt and preparation method thereof
CN113871589B (en) * 2021-09-16 2023-10-24 南开大学 Lithium-rich manganese-based positive electrode material coated by molten salt-assisted lithium titanate and preparation method thereof
CN114094060A (en) * 2021-10-08 2022-02-25 中南大学 Preparation method of high-voltage positive electrode material with core-shell structure
CN116177624A (en) * 2023-03-20 2023-05-30 合肥工业大学 Simple preparation method of high-nickel ternary positive electrode material with spinel structure coating layer

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