CN104485453A - Preparation method of neodymium-doped lithium cobalt oxide composite positive electrode material clad with hydroxyl graphene - Google Patents

Preparation method of neodymium-doped lithium cobalt oxide composite positive electrode material clad with hydroxyl graphene Download PDF

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CN104485453A
CN104485453A CN201510010939.0A CN201510010939A CN104485453A CN 104485453 A CN104485453 A CN 104485453A CN 201510010939 A CN201510010939 A CN 201510010939A CN 104485453 A CN104485453 A CN 104485453A
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neodymium
solution
lithium
doped
graphene
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宫香娥
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Ding Huangxiang
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宫香娥
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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
    • H01M4/52—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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M4/625—Carbon or graphite
    • 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

Abstract

The invention relates to a preparation method of a neodymium-doped lithium cobalt oxide composite positive electrode material clad with hydroxyl graphene. The chemical formula of neodymium-doped composite lithium cobalt oxide is LiCo1-xNixNdyO2, wherein x=0.35-0.45, and y=0.01-0.025. The method comprises the steps of (1) preparing the neodymium-doped composite lithium cobalt oxide, (2) preparing hydroxyl graphene oxide, and (3) carrying out cladding. According to the composite positive electrode material prepared through the method, firstly, high-nickel-doped lithium cobalt oxide is further doped with the rare earth element Nd to be modified to improve material activity, and then the surface of the product is clad with a layer of hydroxyl graphene in an embedment mode to further improve the electrical conductivity and cyclic stability of the composite positive electrode material. Thus, when applied to lithium ion batteries, the composite material has high first discharge reversible capacity and long service life.

Description

A kind of preparation method of cobalt acid lithium composite positive pole of hydroxyl graphene coated neodymium doping
Technical field
The present invention relates to the preparation method of the cobalt acid lithium composite positive pole of a kind of hydroxyl graphene coated neodymium doping.
Background technology
Along with the development of various new forms of energy, the miniaturization of portable electric appts and electric automobile are to the widespread demand of large-capacity high-power chemical power source, the capacity problem of lithium ion battery electrode material more and more becomes the emphasis of research and development.Traditional commercial lithium ion battery adopts inorganic positive pole/graphite system mostly, the system of the active material of these positive poles mainly LiFePO4, LiMn2O4, cobalt acid lithium, lithium nickelate and mixing.Although the electrochemical performance of this kind of system, because itself specific capacity is lower, the theoretical specific capacity as LiFePO4 only has 170mAh/g, so the positive electrode of other kind of development of new receives the attention widely of people.
Under the prerequisite playing identical capacity, the volume energy density of battery be improved, just need improve the loading of cell active materials unit volume.For conventional cobalt acid lithium material, its particle is larger, and the compacted density of material is larger, and volume loading is also larger, and its volume energy density is higher.But find in the evaluation procedure to bulky grain cobalt acid lithium material: after particle increases, the electro-chemical activity of positive electrode can reduce, and shows as the obvious variation of cycle performance and multiplying power discharging property.
Summary of the invention
The invention provides the preparation method of the cobalt acid lithium composite positive pole of a kind of hydroxyl graphene coated neodymium doping, use positive electrode prepared by the method, while there is high-energy-density, the cycle performance that also tool is good.
To achieve these goals, the preparation method of the cobalt acid lithium composite positive pole of a kind of hydroxyl graphene coated neodymium doping provided by the invention, the chemical formula of this neodymium doped and compounded cobalt acid lithium is LiCo 1-xni xnd yo 2, wherein: x=0.35-0.45, y=0.01-0.025, the method comprises the steps:
(1) neodymium doped and compounded cobalt acid lithium is prepared
Lithium acetate, nickel chloride, cobalt hydroxide, neodymium nitrate is taken according to the mole of Li, Ni, Co, Nd in above-mentioned chemical formula, for subsequent use; By water-soluble for the above-mentioned nickel chloride nickel chloride solution being configured to 1-2mol/L, above-mentioned neodymium nitrate is configured to the neodymium nitrate solution of 0.05-0.1mol/L, this two all solution is mixed and obtains mixing salt solution; Configuration concentration is the sodium hydroxide solution of 3-4mol/L, and configuration concentration is the ammonia spirit of 1-2mol/L;
Slowly joined by ammonia spirit in above-mentioned mixing salt solution, wherein ammonia spirit and mixed liquor volume are than being 1:4-6, stir 1-2h, add the cobalt hydroxide taken, fully stir 15-20min after stirring, and treat cobalt hydroxide surface complete wetting;
Above-mentioned sodium hydroxide solution is joined above-mentioned infiltration by the mixed solution of cobaltosic oxide by peristaltic pump, control the pH value of reaction within the scope of 10-11, the temperature of reaction is within the scope of 60-75 DEG C, and mixing speed is within the scope of 400-500/min, and solution adds and terminates rear continuation stirring, after ageing, Separation of Solid and Liquid, spends deionized water and is less than 8 to pH, dries, sintering oxidation, obtains neodymium doped and compounded cobalt acid lithium presoma; Neodymium doped and compounded cobalt acid lithium presoma mix with above-mentioned load weighted lithium oxalate, by compound in planetary ball mill with rotating speed 300-400r/min ball milling 10-15h, dry, sinter and obtain the sour lithium of neodymium doped and compounded cobalt;
(2) hydroxyl oxidize grapheme material is prepared
Graphite oxide has been joined N, in dinethylformamide, ultrasonic agitation preparation quality concentration is the graphene oxide suspension of 1-1.5g/L, the propanol solution of hydroxyanilines is added subsequently in graphene oxide suspension, and the 15-20min that refluxes at 90-95 DEG C, obtain hydroxyl oxidize grapheme material, wherein, the mass concentration of the alcoholic solution of described hydroxyanilines is 1-1.5g/L, and the mass ratio of graphene oxide and hydroxyanilines is 1:1-2;
(3) coated
Reflux the described acid of neodymium doped and compounded cobalt lithium, hydroxyl oxidize Graphene and hydrazine hydrate at 80 DEG C 6-8h, wherein the mass ratio of neodymium doped and compounded cobalt acid lithium, hydroxyl oxidize Graphene and hydrazine hydrate is 100:5-10:20-30, filter, dry, obtain the composite positive pole of hydroxyl graphene coated.
Composite positive pole prepared by the present invention, first by the cobalt of nickelic doping acid lithium, further doped with rare-earth elements Nd carrys out modification to improve species activity, then embeds coated one deck hydroxyl grapheme material on its surface, improves its electric conductivity and cyclical stability further.Therefore this composite material is when for lithium ion battery, has higher discharging reversible capacity and longer useful life first.
Embodiment
embodiment one
The active material chemical formula of neodymium doped and compounded cobalt acid lithium prepared by the present embodiment is LiCo 0.74ni 0.35nd 0.01o 2.
Lithium acetate, nickel chloride, cobalt hydroxide, neodymium nitrate is taken according to the mole of Li, Ni, Co, Nd in above-mentioned chemical formula, for subsequent use; By water-soluble for the above-mentioned nickel chloride nickel chloride solution being configured to 1mol/L, above-mentioned neodymium nitrate is configured to the neodymium nitrate solution of 0.05mol/L, this two all solution is mixed and obtains mixing salt solution; Configuration concentration is the sodium hydroxide solution of 3mol/L, and configuration concentration is the ammonia spirit of 1mol/L; Slowly joined by ammonia spirit in above-mentioned mixing salt solution, wherein ammonia spirit and mixed liquor volume are than being 1:4, stir 1h, add the cobalt hydroxide taken, fully stir 15min after stirring, and treat cobalt hydroxide surface complete wetting.
Above-mentioned sodium hydroxide solution is joined above-mentioned infiltration by the mixed solution of cobaltosic oxide by peristaltic pump, control the pH value of reaction within the scope of 10-11, the temperature of reaction is within the scope of 60 DEG C, and mixing speed is at 400/min, and solution adds and terminates rear continuation stirring, after ageing, Separation of Solid and Liquid, spends deionized water and is less than 8 to pH, dries, sintering oxidation, obtains neodymium doped and compounded cobalt acid lithium presoma; Neodymium doped and compounded cobalt acid lithium presoma mix with above-mentioned load weighted lithium oxalate, by compound in planetary ball mill with rotating speed 300r/min ball milling 15h, dry, sinter and obtain the sour lithium of neodymium doped and compounded cobalt.
Graphite oxide has been joined N, in dinethylformamide, ultrasonic agitation preparation quality concentration is the graphene oxide suspension of 1g/L, the propanol solution of hydroxyanilines is added subsequently in graphene oxide suspension, and the 20min that refluxes at 90 DEG C, obtain hydroxyl oxidize grapheme material, wherein, the mass concentration of the alcoholic solution of described hydroxyanilines is 1g/L, and the mass ratio of graphene oxide and hydroxyanilines is 1:1.
Reflux the described acid of neodymium doped and compounded cobalt lithium, hydroxyl oxidize Graphene and hydrazine hydrate at 80 DEG C 6h, wherein the mass ratio of neodymium doped and compounded cobalt acid lithium, hydroxyl oxidize Graphene and hydrazine hydrate is 100:5:20, filter, dry, obtain the composite positive pole of hydroxyl graphene coated.
embodiment two
The active material chemical formula of neodymium doped and compounded cobalt acid lithium prepared by the present embodiment is LiCo 0.525ni 0.45nd 0.025o 2.
Lithium acetate, nickel chloride, cobalt hydroxide, neodymium nitrate is taken according to the mole of Li, Ni, Co, Nd in above-mentioned chemical formula, for subsequent use; By water-soluble for the above-mentioned nickel chloride nickel chloride solution being configured to 2mol/L, above-mentioned neodymium nitrate is configured to the neodymium nitrate solution of 0.1mol/L, this two all solution is mixed and obtains mixing salt solution; Configuration concentration is the sodium hydroxide solution of 4mol/L, and configuration concentration is the ammonia spirit of 2mol/L; Slowly joined by ammonia spirit in above-mentioned mixing salt solution, wherein ammonia spirit and mixed liquor volume are than being 1:6, stir 2h, add the cobalt hydroxide taken, fully stir 20min after stirring, and treat cobalt hydroxide surface complete wetting.
Above-mentioned sodium hydroxide solution is joined above-mentioned infiltration by the mixed solution of cobaltosic oxide by peristaltic pump, control the pH value of reaction within the scope of 10-11, the temperature of reaction is within the scope of 75 DEG C, and mixing speed is at 500/min, and solution adds and terminates rear continuation stirring, after ageing, Separation of Solid and Liquid, spends deionized water and is less than 8 to pH, dries, sintering oxidation, obtains neodymium doped and compounded cobalt acid lithium presoma; Neodymium doped and compounded cobalt acid lithium presoma mix with above-mentioned load weighted lithium oxalate, by compound in planetary ball mill with rotating speed 400r/min ball milling 10h, dry, sinter and obtain the sour lithium of neodymium doped and compounded cobalt.
Graphite oxide has been joined N, in dinethylformamide, ultrasonic agitation preparation quality concentration is the graphene oxide suspension of 1.5g/L, the propanol solution of hydroxyanilines is added subsequently in graphene oxide suspension, and the 15min that refluxes at 95 DEG C, obtain hydroxyl oxidize grapheme material, wherein, the mass concentration of the alcoholic solution of described hydroxyanilines is 1.5g/L, and the mass ratio of graphene oxide and hydroxyanilines is 1:2.
Reflux the described acid of neodymium doped and compounded cobalt lithium, hydroxyl oxidize Graphene and hydrazine hydrate at 80 DEG C 8h, wherein the mass ratio of neodymium doped and compounded cobalt acid lithium, hydroxyl oxidize Graphene and hydrazine hydrate is 100:10:30, filter, dry, obtain the composite positive pole of hydroxyl graphene coated.
comparative example
Select battery-level lithium carbonate and cobaltosic oxide to be raw material, and carry out proportioning according to the ratio of lithium cobalt mol ratio 1.035:1.Add TiO 2, ZrO 2and Nb 2o 5as additive T1, wherein TiO 2interpolation weight be cobaltosic oxide weight 0.12%, ZrO 2interpolation weight be cobaltosic oxide weight 0.1%, Nb 2o 5interpolation weight be 0.15% of cobaltosic oxide weight.By battery-level lithium carbonate, cobaltosic oxide, TiO 2, ZrO 2and Nb 2o 5carry out doping mixture, and mix.The material obtaining mixing is loaded in fire resistant sagger, pushes in high temperature pusher kiln, be incubated 12 hours at 600 ~ 1100 DEG C of temperature after, slowly release kiln.In cobalt acid lithium one defective material obtained, add the Al of cobalt acid lithium one defective material weight 0.2% 2o 3, and mix.The material mixed is loaded in fire resistant sagger, pushes in high temperature pusher kiln, be incubated 12 hours at 600 ~ 1100 DEG C of temperature after, slowly release kiln.The material of coming out of the stove is carried out pulverize, sieve, can lithium cobaltate cathode material be obtained.
Adopt NMP as solvent above-described embodiment one, two and comparative example products therefrom, by active material: SP: PVDF=90: 5: 5 be mixed with solid content be 70% slurry be evenly coated on Al paper tinsel, make positive pole.Negative pole adopts deionized water as solvent, by graphite: SP: SBR: CMC=90: 4: 3: 3 to be mixed with solid content be that the slurry of 45% is evenly on Cu paper tinsel.Electrolyte is the LiPF of 1mol/L 6solution, solvent is the mixed solvent of EC, DEC and EMC, and volume ratio is 1: 1: 1.The negative pole of button cell uses Li sheet.In the glove box of argon shield, positive pole, negative pole, electrolyte, barrier film and battery case are assembled into button cell.At probe temperature is 25 DEG C, carry out electric performance test, after tested this embodiment one with two material compared with the product of comparative example, first charge-discharge reversible capacity improves 22-25%, and useful life improves more than 50%.

Claims (1)

1. a preparation method for the cobalt acid lithium composite positive pole of hydroxyl graphene coated neodymium doping, the chemical formula of this neodymium doped and compounded cobalt acid lithium is LiCo 1-xni xnd yo2, wherein: x=0.35-0.45, y=0.01-0.025, the method comprises the steps:
(1) neodymium doped and compounded cobalt acid lithium is prepared
Lithium acetate, nickel chloride, cobalt hydroxide, neodymium nitrate is taken according to the mole of Li, Ni, Co, Nd in above-mentioned chemical formula, for subsequent use; By water-soluble for the above-mentioned nickel chloride nickel chloride solution being configured to 1-2mol/L, above-mentioned neodymium nitrate is configured to the neodymium nitrate solution of 0.05-0.1mol/L, this two all solution is mixed and obtains mixing salt solution; Configuration concentration is the sodium hydroxide solution of 3-4mol/L, and configuration concentration is the ammonia spirit of 1-2mol/L;
Slowly joined by ammonia spirit in above-mentioned mixing salt solution, wherein ammonia spirit and mixed liquor volume are than being 1:4-6, stir 1-2h, add the cobalt hydroxide taken, fully stir 15-20min after stirring, and treat cobalt hydroxide surface complete wetting;
Above-mentioned sodium hydroxide solution is joined above-mentioned infiltration by the mixed solution of cobaltosic oxide by peristaltic pump, control the pH value of reaction within the scope of 10-11, the temperature of reaction is within the scope of 60-75 DEG C, and mixing speed is within the scope of 400-500/min, and solution adds and terminates rear continuation stirring, after ageing, Separation of Solid and Liquid, spends deionized water and is less than 8 to pH, dries, sintering oxidation, obtains neodymium doped and compounded cobalt acid lithium presoma; Neodymium doped and compounded cobalt acid lithium presoma mix with above-mentioned load weighted lithium oxalate, by compound in planetary ball mill with rotating speed 300-400r/min ball milling 10-15h, dry, sinter and obtain the sour lithium of neodymium doped and compounded cobalt;
(2) hydroxyl oxidize grapheme material is prepared
Graphite oxide has been joined N, in dinethylformamide, ultrasonic agitation preparation quality concentration is the graphene oxide suspension of 1-1.5g/L, the propanol solution of hydroxyanilines is added subsequently in graphene oxide suspension, and the 15-20min that refluxes at 90-95 DEG C, obtain hydroxyl oxidize grapheme material, wherein, the mass concentration of the alcoholic solution of described hydroxyanilines is 1-1.5g/L, and the mass ratio of graphene oxide and hydroxyanilines is 1:1-2;
(3) coated
Reflux the described acid of neodymium doped and compounded cobalt lithium, hydroxyl oxidize Graphene and hydrazine hydrate at 80 DEG C 6-8h, wherein the mass ratio of neodymium doped and compounded cobalt acid lithium, hydroxyl oxidize Graphene and hydrazine hydrate is 100:5-10:20-30, filter, dry, obtain the composite positive pole of hydroxyl graphene coated.
CN201510010939.0A 2015-01-09 2015-01-09 Preparation method of neodymium-doped lithium cobalt oxide composite positive electrode material clad with hydroxyl graphene Pending CN104485453A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107369826A (en) * 2017-08-04 2017-11-21 长沙理工大学 Doping and the lithium/sodium layered metal oxide positive electrode and its one-step method for synthesizing for coating dual modification
CN107742705A (en) * 2017-10-03 2018-02-27 长沙仲善新能源科技有限公司 Compound lithium cobaltate cathode material of a kind of graphene and preparation method thereof
CN109728269A (en) * 2018-12-18 2019-05-07 南京理工大学 The preparation method of graphene coated cobalt lithium aluminate electrode material

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107369826A (en) * 2017-08-04 2017-11-21 长沙理工大学 Doping and the lithium/sodium layered metal oxide positive electrode and its one-step method for synthesizing for coating dual modification
CN107369826B (en) * 2017-08-04 2019-08-02 长沙理工大学 Doping and the lithium/sodium layered metal oxide positive electrode and its one-step method for synthesizing for coating dual modification
CN107742705A (en) * 2017-10-03 2018-02-27 长沙仲善新能源科技有限公司 Compound lithium cobaltate cathode material of a kind of graphene and preparation method thereof
CN109728269A (en) * 2018-12-18 2019-05-07 南京理工大学 The preparation method of graphene coated cobalt lithium aluminate electrode material
CN109728269B (en) * 2018-12-18 2022-02-15 南京理工大学 Preparation method of graphene-coated cobalt lithium aluminate electrode material

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