CN103943845A - Preparation method of layered-spinel composite solid solution positive-electrode material - Google Patents

Preparation method of layered-spinel composite solid solution positive-electrode material Download PDF

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CN103943845A
CN103943845A CN201410156400.1A CN201410156400A CN103943845A CN 103943845 A CN103943845 A CN 103943845A CN 201410156400 A CN201410156400 A CN 201410156400A CN 103943845 A CN103943845 A CN 103943845A
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solid solution
positive electrode
composite solid
preparation
stratiform
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刘云建
王启亮
高彦涌
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
    • H01M4/626—Metals
    • 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
    • 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)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to a sodium-ion-doped layered-spinel composite solid solution positive-electrode material which belongs to the field of new energy materials. A preparation method of the positive-electrode material comprises the following steps: firstly, dissolving nickel salt and manganese salt weighed in a stoichiometric ratio into deionized water to prepare a multi-element metal salt solution; secondly, preparing an alkaline solution; then in the presence of an ultrasonic out-field, adding the multi-element metal salt solution and the excess alkaline solution in a stoichiometric ratio during stirring and reacting, wherein the reaction temperature and the adding speed of the salt solution and the alkaline solution are well controlled; after reaction, continuously stirring, then standing and filtering to obtain a solid substance; washing the solid substance with the deionized water until the pH value reaches below 7.8, and drying the washed substance to obtain a nickel and manganese multi-element lithium ion battery positive-electrode material precursor; mixing the precursor with lithium salt and a sodium source weighed in a stoichiometric ratio, performing mechanical activation and calcination, and finally cooling to obtain the layered-spinel composite solid solution positive-electrode material. By virtue of the method, the rate capability of the positive-electrode material can be effectively enhanced.

Description

A kind of preparation method of stratiform-spinelle composite solid solution positive electrode
Technical field
Stratiform-spinelle composite solid solution the positive electrode that the present invention relates to a kind of sodium ion doping, belongs 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 New Generation of Electric Vehicle lithium-ion-power cell.
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, first coulombic efficiency and good cycle performance, be therefore expected to become lithium ion power battery cathode material of new generation.
But research finds that the high rate performance of novel stratiform-spinelle composite solid solution positive electrode is not also fine, is therefore necessary further its high rate performance to be improved.
Summary of the invention
The invention provides one and improve stratiform-spinelle composite solid solution positive electrode Li 0.5+xni 0.25mn 0.75o 2+x/2(0<x<1) new method of high rate performance, concrete summary of the invention is as follows:
1. first, by the nickel salt weighing by stoichiometric proportion, the dissolving of manganese salt, be configured to the multi-element metal salting liquid that total metal ion molar concentration is 0.3-3mol/L with deionized water, secondly, preparation aqueous slkali; Then, react while stirring under the effect of ultrasonic external field by salting liquid and according to the aqueous slkali of stoichiometric proportion excessive 20%, control temperature at 40 DEG C-80 DEG C, control the speed that adds of salt, aqueous slkali well, make pH value of reaction system be controlled at 9-12; Continue after completion of the reaction to stir, after continuing to stir, leave standstill, filter, obtain solid content, wash to pH value below 7.8 with deionized water, be dried, obtain the polynary precursor of lithium ionic cell positive material of nickel manganese, molecular formula is: Ni 0.25mn 0.75(OH) 2.
Described aqueous slkali is the aqueous solution of NaOH, potassium hydroxide or lithium hydroxide, and concentration is 1-4mol/L.
The mixing speed that stir on described limit is turn/min of 100-600.
The time that described continuation is stirred is 0.5-12 h.
Described time of repose is 1-5 h.
Then and the lithium salts taking by stoichiometric proportion and sodium source mix, through mechanical activation 1-12h, roasting 1-12h at 400-600 DEG C, then at 750-900 DEG C roasting 8-24h, last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains 0.5+xna yni 0.25mn 0.75o 2+ (x+y)/2(0<x+y<1; 0<y<0.3).
In described 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.
In described step 2, lithium salts is lithium hydroxide, lithium carbonate, lithium nitrate or lithium acetate, and sodium source is sodium carbonate, NaOH, sodium sulphate, sodium nitrate.
By said method, the Li of the sodium ion doping of preparation 0.5+xna yni 0.25mn 0.75o 2+ (x+y)/2(0<x+y<1; 0<y<0.3) positive electrode, has improved the high rate performance of positive electrode effectively.
Brief description of the drawings
The Li of the sodium ion doping in Fig. 1 embodiment 1 1.1na 0.1ni 0.25mn 0.75o 2.35positive electrode SEM figure, as can be seen from the figure, the Li of sodium ion doping 1.1na 0.1ni 0.25mn 0.75o 2.35positive electrode has good spherical morphology, is conducive to the positive electrode energy density improving.
The Li of sodium ion doping in Fig. 2 embodiment 1 1.1na 0.1ni 0.25mn 0.75o 2.35positive electrode and micro-Li doped 1.2ni 0.25mn 0.75o 2.35positive electrode high rate performance comparison diagram, as can be seen from the figure, through the positive electrode of Na ion doping, its high rate performance has obtained obvious lifting.
Embodiment
Embodiment 1: first, nickelous sulfate, manganese sulfate are dissolved with deionized water, the multi-element metal salting liquid that the total metal ion molar concentration that is configured to 1L is 0.3mol/L, secondly, the sodium hydroxide solution of compound concentration 1mol/L; Then, react under the effect of ultrasonic external field by salting liquid and according to the sodium hydroxide solution of stoichiometric proportion excessive 20%, control temperature at 40 DEG C, mixing speed is 100 turn/min, control the speed that adds of salt, aqueous slkali well, make pH value of reaction system be controlled at 9; Continue after completion of the reaction to stir 0.5 h, leave standstill 1 h, filter, obtain solids, wash to pH value below 7.8 with deionized water, be dried, obtain nickel cobalt manganese hydroxide presoma, molecular formula is: Ni 0.25mn 0.75(OH) 2; Then add lithium carbonate and sodium carbonate to mix according to stoichiometric proportion, through mechanical activation 1h, roasting 1h at 600 DEG C, then at 900 DEG C roasting 8h, the last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains sodium doping 1.1na 0.1ni 0.25mn 0.75o 2.35.
Embodiment 2: first, nickelous sulfate, manganese sulfate are dissolved with deionized water, the multi-element metal salting liquid that the total metal ion molar concentration that is configured to 1L is 1mol/L, secondly, the potassium hydroxide solution of compound concentration 3mol/L; Then, react under the effect of ultrasonic external field by salting liquid and according to the potassium hydroxide solution of stoichiometric proportion excessive 20%, control temperature at 50 DEG C, mixing speed is 600 turn/min, control the speed that adds of salt, aqueous slkali well, make pH value of reaction system be controlled at 12; Continue after completion of the reaction to stir 12 h, leave standstill 5 h, filter, obtain solids, wash to pH value below 7.8 with deionized water, be dried, obtain nickel cobalt manganese hydroxide presoma, molecular formula is: Ni 0.25mn 0.75(OH) 2; Then add lithium carbonate and sodium carbonate to mix according to stoichiometric proportion, through mechanical activation 12h, roasting 12h at 400 DEG C, then at 750 DEG C roasting 24h, the last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains sodium doping 1.1na 0.2ni 0.25mn 0.75o 2.4.
Embodiment 3: first, nickelous sulfate, manganese sulfate are dissolved with deionized water, the multi-element metal salting liquid that the total metal ion molar concentration that is configured to 1L is 0.5mol/L, secondly, the sodium hydroxide solution of compound concentration 1.5mol/L; Then, react under the effect of ultrasonic external field by salting liquid and according to the NaOH aqueous slkali of stoichiometric proportion excessive 20%, control temperature at 60 DEG C, mixing speed is 300 turn/min, control the speed that adds of salt, aqueous slkali well, make pH value of reaction system be controlled at 11; Continue after completion of the reaction to stir 4 h, leave standstill 2 h, filter, obtain solids, wash to pH value below 7.8 with deionized water, be dried, obtain nickel cobalt manganese hydroxide presoma, molecular formula is: Ni 0.25mn 0.75(OH) 2; Then add lithium carbonate and sodium carbonate to mix according to stoichiometric proportion, through mechanical activation 5h, roasting 5h at 400 DEG C, then at 880 DEG C roasting 12h, the last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains sodium doping 1.2na 0.1ni 0.25mn 0.75o 2.4.
Embodiment 4: first, nickelous sulfate, manganese sulfate are dissolved with deionized water, the multi-element metal salting liquid that the total metal ion molar concentration that is configured to 1L is 0.5mol/L, secondly, the lithium hydroxide solution of compound concentration 2mol/L; Then, react under the effect of ultrasonic external field by salting liquid and according to the lithium hydroxide aqueous slkali of stoichiometric proportion excessive 20%, control temperature at 70 DEG C, mixing speed is 300 turn/min, control the speed that adds of salt, aqueous slkali well, make pH value of reaction system be controlled at 11; Continue after completion of the reaction to stir 3 h, leave standstill 2 h, filter, obtain solids, wash to pH value below 7.8 with deionized water, be dried, obtain nickel cobalt manganese hydroxide presoma, molecular formula is: Ni 0.25mn 0.75(OH) 2; Then add lithium carbonate and sodium carbonate to mix according to stoichiometric proportion, through mechanical activation 4h, roasting 6h at 500 DEG C, then at 850 DEG C roasting 16h, the last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains sodium doping 1.2na 0.2ni 0.25mn 0.75o 2.45.
Embodiment 5: first, nickelous sulfate, manganese sulfate are dissolved with deionized water, the multi-element metal salting liquid that the total metal ion molar concentration that is configured to 1L is 1mol/L, secondly, the sodium hydroxide solution of compound concentration 2mol/L; Then, react under the effect of ultrasonic external field by salting liquid and according to the NaOH aqueous slkali of stoichiometric proportion excessive 20%, control temperature at 80 DEG C, mixing speed is 400 turn/min, control the speed that adds of salt, aqueous slkali well, make pH value of reaction system be controlled at 10; Continue after completion of the reaction to stir 3 h, leave standstill 3 h, filter, obtain solids, wash to pH value below 7.8 with deionized water, be dried, obtain nickel cobalt manganese hydroxide presoma, molecular formula is: Ni 0.25mn 0.75(OH) 2; Then add lithium carbonate and sodium carbonate to mix according to stoichiometric proportion, through mechanical activation 2h, roasting 4h at 500 DEG C, then at 850 DEG C roasting 15h, the last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains sodium doping 0.9na 0.2ni 0.25mn 0.75o 2.3.

Claims (8)

1. a preparation method for stratiform-spinelle composite solid solution positive electrode, is characterized in that comprising the steps:
(1) first, the nickel salt weighing, manganese salt are dissolved and be configured to multi-element metal salting liquid with deionized water by stoichiometric proportion, secondly, preparation aqueous slkali; Then, multi-element metal salting liquid and the excessive aqueous slkali of stoichiometric proportion are stirred and add limit to react below in the effect of ultrasonic external field, control temperature at 40 DEG C-80 DEG C, control the speed that adds of salt, aqueous slkali well, make pH value of reaction system be controlled at 9-12; Continue after completion of the reaction to stir, after continuing to stir, leave standstill, filter, obtain solid content, wash to pH value below 7.8 with deionized water, be dried, obtain the polynary precursor of lithium ionic cell positive material of nickel manganese, molecular formula is: Ni 0.25mn 0.75(OH) 2;
(2) then and the lithium salts taking by stoichiometric proportion and sodium source mix, through mechanical activation 1-12h, roasting 1-12h at 400-600 DEG C, then at 750-900 DEG C roasting 8-24h, last cooling stratiform-spinelle composite solid solution positive electrode Li that obtains 0.5+xna yni 0.25mn 0.75o 2+ (x+y)/2, 0<x+y<1; 0<y<0.3.
2. the preparation method of a kind of stratiform-spinelle composite solid solution positive electrode as claimed in claim 1, is characterized in that: total metal ion molar concentration of described multi-element metal salting liquid is 0.3-3mol/L.
3. the preparation method of a kind of stratiform-spinelle composite solid solution positive electrode as claimed in claim 1, is characterized in that: the excessive finger stoichiometric proportion excessive 20% of described stoichiometric proportion.
4. the preparation method of a kind of stratiform-spinelle composite solid solution positive electrode as claimed in claim 1, is characterized in that: described aqueous slkali is the aqueous solution of NaOH, potassium hydroxide or lithium hydroxide, and concentration is 1-4mol/L.
5. the preparation method of a kind of stratiform-spinelle composite solid solution positive electrode as claimed in claim 1, is characterized in that: the mixing speed that stir on described limit is turn/min of 100-600.
6. the preparation method of a kind of stratiform-spinelle composite solid solution positive electrode as claimed in claim 1, is characterized in that: the time that described continuation is stirred is 0.5-12 h; Described time of repose is 1-5 h.
7. the preparation method of a kind of stratiform-spinelle composite solid solution positive electrode as claimed in claim 1, is characterized in that: in described 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.
8. the preparation method of a kind of stratiform-spinelle composite solid solution positive electrode as claimed in claim 1, is characterized in that: in described step 2, lithium salts is lithium hydroxide, lithium carbonate, lithium nitrate or lithium acetate, sodium source is sodium carbonate, NaOH, sodium sulphate, sodium nitrate.
CN201410156400.1A 2014-04-18 2014-04-18 Preparation method of layered-spinel composite solid solution positive-electrode material Pending CN103943845A (en)

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Cited By (3)

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CN110112410A (en) * 2019-05-29 2019-08-09 新乡学院 A kind of modification lithium-ion battery anode material and preparation method thereof
CN114094080A (en) * 2021-11-18 2022-02-25 天津巴莫科技有限责任公司 Single crystal type lithium-rich layered-spinel composite cathode material and preparation method thereof
CN114975977A (en) * 2022-08-03 2022-08-30 四川新能源汽车创新中心有限公司 Lithium nickel manganese oxide-sodium nickel manganese oxide composite cathode material and preparation method and application thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110112410A (en) * 2019-05-29 2019-08-09 新乡学院 A kind of modification lithium-ion battery anode material and preparation method thereof
CN114094080A (en) * 2021-11-18 2022-02-25 天津巴莫科技有限责任公司 Single crystal type lithium-rich layered-spinel composite cathode material and preparation method thereof
CN114094080B (en) * 2021-11-18 2024-06-11 天津巴莫科技有限责任公司 Single crystal type lithium-rich layered-spinel composite positive electrode material and preparation method thereof
CN114975977A (en) * 2022-08-03 2022-08-30 四川新能源汽车创新中心有限公司 Lithium nickel manganese oxide-sodium nickel manganese oxide composite cathode material and preparation method and application thereof
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Application publication date: 20140723