CN107093736A - A kind of preparation method of carbon composite silica ferrous silicate lithium composite - Google Patents

A kind of preparation method of carbon composite silica ferrous silicate lithium composite Download PDF

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CN107093736A
CN107093736A CN201710449433.9A CN201710449433A CN107093736A CN 107093736 A CN107093736 A CN 107093736A CN 201710449433 A CN201710449433 A CN 201710449433A CN 107093736 A CN107093736 A CN 107093736A
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lithium
ferrous
zinc oxide
solid product
reaction
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不公告发明人
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Suzhou Sichuang Yuanbo Electronic Technology Co Ltd
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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
    • H01M4/36—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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The present invention relates to a kind of preparation method of carbon composite silica ferrous silicate lithium composite, methods described is simple to operation, cost is low, it is time-consuming short, coated using the stratum level hole carbon material of three-dimensional structure, active component capacity is improved with meso-hole structure, and three-dimensional structure can effectively improve the scattering and permeating of electrolyte, electronic and ionic efficiency of transmission is improved, circulation and the high rate performance of positive electrode is effectively improved.

Description

A kind of preparation method of carbon composite silica ferrous silicate lithium composite
Technical field
The present invention relates to technical field of lithium batteries, and in particular to a kind of preparation of carbon composite silica ferrous silicate lithium composite Method.
Background technology
Lithium ion battery is new generation of green high-energy battery, with voltage is high, energy density is big, good cycle, is put certainly The many merits such as electric small, memory-less effect, operating temperature range be wide, are widely used in phone, notebook computer, electric tool Deng also being had a good application prospect in electric automobile, by it is believed that being 21 century significant high energy technology Product.
Current commercialized lithium ion anode material is mainly with ferrosilicon silicate of lithium (LiFePO4), ternary material (nickel cobalt manganese Ternary material NCM, nickel cobalt aluminium ternary material NCA) and LiMn2O4 (LiMn2O4) etc. based on, wherein lithium manganate battery cycle life Cycle life is worse under short and hot environment, and ternary material has safety issue as electrokinetic cell.Ferrosilicon silicate of lithium is former Expect that price is low, theoretical capacity is big, has extended cycle life, be the generally acknowledged most promising product of lithium battery.
Li2FeSiO4Have and low temperature li3PO4Similar structure, belongs to rhombic system, wherein oxygen atom is with positive tetrahedron Tightly packed mode is arranged, and Fe and Si is each in oxygen atom tetrahedron center.Ferrosilicon silicate of lithium is used as lithium ion battery The reversible charge-discharge performance of positive electrode, this positive electrode has caused extensive concern both domestic and external.But influence silicic acid The wide variety of principal element of ferrous lithium composite is that its electrical conductivity poor surface cladding is current improvement lithium ion battery One of not enough effective ways of positive electrode, clad can not only effectively suppress the side reaction between electrolyte and positive electrode, also Cycle performance under dissolving of transition metal etc. in material, the cyclical stability and high magnification of reinforcing material etc. can be suppressed, It is effectively improved the chemical property of material.
The content of the invention
The present invention provides a kind of preparation method of carbon composite silica ferrous silicate lithium composite, and methods described is simply easily grasped Make, cost is low, it is time-consuming short, coated using the stratum level hole carbon material of three-dimensional structure, activity is improved with meso-hole structure Composition capacity, and three-dimensional structure can effectively improve the scattering and permeating of electrolyte, improve electronic and ionic efficiency of transmission, be effectively improved The circulation of positive electrode and high rate performance.
To achieve these goals, the present invention provides a kind of preparation method of carbon composite silica ferrous silicate lithium composite, This method comprises the following steps：
（1）Prepare ferrosilicon silicate of lithium composite
Lithium oxalate, four water ferrous acetates, meta-aluminic acid ammonium mixing and ball milling are weighed into powder, obtain lithium in precursor, the front axle shell, Iron, silicon, the mol ratio of aluminium are 2: 1: (0.85-0.95)：(0.15-0.05)；
Plasma-arc is imposed under reducing atmosphere to precursor, melts reaction powder, plasma electric arc voltage 30- 50kV, plasma electric arc current 600-800A；
Frit reaction powder is spurted into cooling device with reducibility gas, particle crushed and screened after cooling, screening is obtained Granular size be 5-10 microns of ball-type ferrous metasilicate lithium material；The wherein described nozzle diameter 3-6mm for being used to spray；
（2）Prepare three-dimensional flower-shaped carbon material
Potassium hydroxide and zinc acetate progress hydro-thermal reaction soluble in water are obtained to the matter of flower shape zinc oxide, potassium hydroxide and zinc acetate Amount is than being 3:(2-4)；
Flower shape zinc oxide, mesoporous pore creating material are mixed in water into then addition trishydroxymethylaminomethane and dopamine hydrochloride to enter Row mixing coating reaction, product suction filtration is then dried, solid product is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction One, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine hydrochloride are 10:(3- 5):(2-3):(2-4)；
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, three hydroxyls are then sequentially added Aminomethane and dopamine hydrochloride carry out mixing coating reaction, on the basis of the meso-hole structure that solid product one is constructed One layer of microcellular structure is coated, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide template is removed with acid, is obtained Three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate potassium, three The mass ratio of hydroxymethyl aminomethane and dopamine hydrochloride is 10:(1-2):(4-5):(9-11)；
（3）Compound coating
The three-dimensional flower-shaped carbon material of gained and the ferrous metasilicate lithium material are combined, compound condition is：Under a nitrogen atmosphere, 150-200 DEG C is heated to, 20-24h is incubated, is then purged, the ferrous metasilicate lithium material being not filled by into duct is removed, carbon is multiple Mould assembly ferrosilicon silicate of lithium composite.
It is preferred that, the step（2）In, hydrothermal temperature is 80-90 DEG C, and the reaction time is 30-50min, described mixed The temperature for closing coating reaction is 25-40 DEG C, and the time is 6-8h.
The present invention possesses following advantage and remarkable result：
（1）The plasma high-temperature fusion technology that the present invention is used, is a kind of new technique developed in recent years, and principle is： After vacuum system preset vacuum, plasma working gas is introduced in melt chamber and cooling chamber, electricity is added between the two poles of the earth Inert gas plasma moment heating in pressure, melt chamber, temperature can reach thousands of degree, can make in addition feed appliance Powder is rapidly reached between molten condition, plasma high-speed motion, particle required for occurring sharp impacts, in-time generatin Material under molten condition, by be ejected come gas take melt chamber out of, enter in cooling chamber, obtained after cooling needed for Aluminium ferrous silicate lithium doped anode material.This method can be such that the ferrous silicate lithium doped material of aluminium is formed in moment, and can shape Into continuous production.
（2）The present invention is coated using the stratum level hole carbon material of three-dimensional structure, and activity is improved with meso-hole structure Composition capacity, and three-dimensional structure can effectively improve the scattering and permeating of electrolyte, improve electronic and ionic efficiency of transmission, be effectively improved The circulation of positive electrode and high rate performance.
Embodiment
Embodiment one
Lithium oxalate, four water ferrous acetates, meta-aluminic acid ammonium mixing and ball milling are weighed into powder, obtain lithium in precursor, the front axle shell, Iron, silicon, the mol ratio of aluminium are 2: 1: 0.85：0.15.
Plasma-arc is imposed under reducing atmosphere to precursor, melts reaction powder, plasma electric arc voltage 50kV, plasma electric arc current 600A；Frit reaction powder is spurted into cooling device with reducibility gas, after cooling to Grain is crushed and screened, and sieves the ball-type ferrous metasilicate lithium material that obtained granular size is 5 microns；The wherein described spray for being used to spray Outspoken footpath 3mm；The reducibility gas is the mixture of nitrogen and hydrogen, wherein percent by volume of the hydrogen in mixed gas 1%.
Potassium hydroxide and the zinc acetate hydro-thermal reaction soluble in water that carries out are obtained into flower shape zinc oxide, potassium hydroxide and zinc acetate Mass ratio be 3:2；Hydrothermal temperature is 80 DEG C, and the reaction time is 30min.
Flower shape zinc oxide, mesoporous pore creating material are mixed in water and then added trishydroxymethylaminomethane and dopamine hydrochloric acid Salt carries out mixing coating reaction, then dries product suction filtration, solid is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction Product one, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine hydrochloride are 10: 3:2:2；The temperature of the mixing coating reaction is 25 DEG C, and the time is 6h.
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, then sequentially added Trishydroxymethylaminomethane and dopamine hydrochloride carry out mixing coating reaction, the base for the meso-hole structure constructed in solid product one One layer of microcellular structure is coated on plinth, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide mould is removed with acid Plate, obtains the three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate The mass ratio of potassium, trishydroxymethylaminomethane and dopamine hydrochloride is 10:1:4:9.
The three-dimensional flower-shaped carbon material of gained and the ferrous metasilicate lithium material are combined, compound condition is：In nitrogen bar Under part, 150 DEG C are heated to, 20h is incubated, is then purged, the ferrous metasilicate lithium material being not filled by into duct is removed, carbon is combined Type ferrosilicon silicate of lithium composite.
Embodiment two
Lithium oxalate, four water ferrous acetates, meta-aluminic acid ammonium mixing and ball milling are weighed into powder, obtain lithium in precursor, the front axle shell, Iron, silicon, the mol ratio of aluminium are 2: 1: 0.95：0.05.
Plasma-arc is imposed under reducing atmosphere to precursor, melts reaction powder, plasma electric arc voltage 50kV, plasma electric arc current 600A；Frit reaction powder is spurted into cooling device with reducibility gas, after cooling to Grain is crushed and screened, and sieves the ball-type ferrous metasilicate lithium material that obtained granular size is 10 microns；It is wherein described to be used for what is sprayed Nozzle diameter 6mm；The reducibility gas is the mixture of nitrogen and hydrogen, wherein volume basis of the hydrogen in mixed gas Than 3%.
Potassium hydroxide and the zinc acetate hydro-thermal reaction soluble in water that carries out are obtained into flower shape zinc oxide, potassium hydroxide and zinc acetate Mass ratio be 3:4；Hydrothermal temperature is 90 DEG C, and the reaction time is 50min.
Flower shape zinc oxide, mesoporous pore creating material are mixed in water and then added trishydroxymethylaminomethane and dopamine hydrochloric acid Salt carries out mixing coating reaction, then dries product suction filtration, solid is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction Product one, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine hydrochloride are 10: 5:3:4；The temperature of the mixing coating reaction is 40 DEG C, and the time is 8h.
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, then sequentially added Trishydroxymethylaminomethane and dopamine hydrochloride carry out mixing coating reaction, the base for the meso-hole structure constructed in solid product one One layer of microcellular structure is coated on plinth, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide mould is removed with acid Plate, obtains the three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate The mass ratio of potassium, trishydroxymethylaminomethane and dopamine hydrochloride is 10:2:5:11.
The three-dimensional flower-shaped carbon material of gained and the ferrous metasilicate lithium material are combined, compound condition is：In nitrogen bar Under part, 200 DEG C are heated to, 24h is incubated, is then purged, the ferrous metasilicate lithium material being not filled by into duct is removed, carbon is combined Type ferrosilicon silicate of lithium composite.
Comparative example
Commercially available ferrosilicon silicate of lithium composite.
Above-described embodiment one, two and comparative example products therefrom are used into NMP as solvent, by active material: SP: PVDF Be configured to slurry that solid content be 70% at=90: 5: 5 is evenly applied on Al paper tinsels, and positive pole is made.Negative pole is from diameter 14mm's Metal lithium sheet, electrolyte selects 1mol LiFP6 (EC：DMC：EMC=1:1:1, v/v), with negative electrode casing-shell fragment-pad-lithium Battery is packaged by the order of piece-electrolyte-barrier film-positive plate-pad-anode cover, and whole process is all filled with argon Completed in the glove box of gas.Electric performance test is carried out in the case where test temperature is 25 DEG C, after tested the material of the embodiment one and two Compared with the product of comparative example, first charge-discharge reversible capacity improves 23-26%, and service life brings up to more than 20%.

Claims (2)

1. a kind of preparation method of carbon composite silica ferrous silicate lithium composite, this method comprises the following steps：
（1）Prepare ferrosilicon silicate of lithium composite
Lithium oxalate, four water ferrous acetates, meta-aluminic acid ammonium mixing and ball milling are weighed into powder, obtain lithium in precursor, the front axle shell, Iron, silicon, the mol ratio of aluminium are 2: 1: (0.85-0.95)：(0.15-0.05)；
Plasma-arc is imposed under reducing atmosphere to precursor, melts reaction powder, plasma electric arc voltage 30- 50kV, plasma electric arc current 600-800A；
Frit reaction powder is spurted into cooling device with reducibility gas, particle crushed and screened after cooling, screening is obtained Granular size be 5-10 microns of ball-type ferrous metasilicate lithium material；The wherein described nozzle diameter 3-6mm for being used to spray；
（2）Prepare three-dimensional flower-shaped carbon material
Potassium hydroxide and zinc acetate progress hydro-thermal reaction soluble in water are obtained to the matter of flower shape zinc oxide, potassium hydroxide and zinc acetate Amount is than being 3:(2-4)；
Flower shape zinc oxide, mesoporous pore creating material are mixed in water into then addition trishydroxymethylaminomethane and dopamine hydrochloride to enter Row mixing coating reaction, product suction filtration is then dried, solid product is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction One, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine hydrochloride are 10:(3- 5):(2-3):(2-4)；
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, three hydroxyls are then sequentially added Aminomethane and dopamine hydrochloride carry out mixing coating reaction, on the basis of the meso-hole structure that solid product one is constructed One layer of microcellular structure is coated, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide template is removed with acid, is obtained Three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate potassium, three The mass ratio of hydroxymethyl aminomethane and dopamine hydrochloride is 10:(1-2):(4-5):(9-11)；
（3）Compound coating
The three-dimensional flower-shaped carbon material of gained and the ferrous metasilicate lithium material are combined, compound condition is：Under a nitrogen atmosphere, 150-200 DEG C is heated to, 20-24h is incubated, is then purged, the ferrous metasilicate lithium material being not filled by into duct is removed, carbon is multiple Mould assembly ferrosilicon silicate of lithium composite.
2. the method as described in right will go 1, it is characterised in that the step（2）In, hydrothermal temperature is 80-90 DEG C, instead It is 30-50min between seasonable, the temperature of the mixing coating reaction is 25-40 DEG C, and the time is 6-8h.
CN201710449433.9A 2017-06-14 2017-06-14 A kind of preparation method of carbon composite silica ferrous silicate lithium composite Pending CN107093736A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020016899A1 (en) * 2018-07-18 2020-01-23 Technion Research & Development Foundation Limited Electrocatalysts with branched-type porosity

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102208647A (en) * 2011-05-13 2011-10-05 天津大学 Lithium ferrous silicate anode material coated with crystalline carbon and preparation method thereof
CN102664262A (en) * 2012-05-18 2012-09-12 哈尔滨工业大学 Method for preparing lithium ferrous silicate or carbon ferrous silicate cathode material for lithium ion battery
CN103474616A (en) * 2013-08-29 2013-12-25 合肥国轩高科动力能源股份公司 Sol precipitation preparation method for carbon-coated lithium iron silicate cathode material
CN103515590A (en) * 2013-09-23 2014-01-15 北京鼎能开源电池科技股份有限公司 Preparation method of ternary anode material of lithium ion battery
CN103887510A (en) * 2014-03-27 2014-06-25 电子科技大学 Preparation method of carbon-coated lithium ferrous silicate compound positive electrode material
CN106654231A (en) * 2017-01-23 2017-05-10 武汉理工大学 Anode material for lithium sulfur batteries and method for preparing anode material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102208647A (en) * 2011-05-13 2011-10-05 天津大学 Lithium ferrous silicate anode material coated with crystalline carbon and preparation method thereof
CN102664262A (en) * 2012-05-18 2012-09-12 哈尔滨工业大学 Method for preparing lithium ferrous silicate or carbon ferrous silicate cathode material for lithium ion battery
CN103474616A (en) * 2013-08-29 2013-12-25 合肥国轩高科动力能源股份公司 Sol precipitation preparation method for carbon-coated lithium iron silicate cathode material
CN103515590A (en) * 2013-09-23 2014-01-15 北京鼎能开源电池科技股份有限公司 Preparation method of ternary anode material of lithium ion battery
CN103887510A (en) * 2014-03-27 2014-06-25 电子科技大学 Preparation method of carbon-coated lithium ferrous silicate compound positive electrode material
CN106654231A (en) * 2017-01-23 2017-05-10 武汉理工大学 Anode material for lithium sulfur batteries and method for preparing anode material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020016899A1 (en) * 2018-07-18 2020-01-23 Technion Research & Development Foundation Limited Electrocatalysts with branched-type porosity
US11784321B2 (en) 2018-07-18 2023-10-10 Technion Research & Development Foundation Limited Electrocatalysts with branched-type porosity

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