CN108899491A - A kind of lithium battery aoxidizes the preparation method of tin negative pole material with carbon coating - Google Patents

A kind of lithium battery aoxidizes the preparation method of tin negative pole material with carbon coating Download PDF

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CN108899491A
CN108899491A CN201810631175.0A CN201810631175A CN108899491A CN 108899491 A CN108899491 A CN 108899491A CN 201810631175 A CN201810631175 A CN 201810631175A CN 108899491 A CN108899491 A CN 108899491A
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tin
weight
tin oxide
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aoxidizes
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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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  • General Chemical & Material Sciences (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of lithium battery preparation methods of carbon coating oxidation tin negative pole material, the tin oxide that the method uses is nano-scale fiber shape, it is covered with uniform through hole on its single fiber, the volume expansion for effectively inhibiting tin oxide is shunk, under equal conditions, embeddable more lithium ion, improves the energy density of battery；The present invention is compound by carbon nitrogen, improves the electric conductivity of active material, in addition, the expansion of volume provides the useful space when cavity between the carbon-coating and tin oxide of N doping is active material Li insertion extraction, it is therefore prevented that the dusting reunion of tin oxide.

Description

A kind of lithium battery aoxidizes the preparation method of tin negative pole material with carbon coating
Technical field
The present invention relates to battery material fields, and in particular to a kind of lithium battery aoxidizes the preparation of tin negative pole material with carbon coating Method.
Background technique
In recent years, domestic new-energy automobile industry development is rapid, and battery variety is rich and varied, demand of the market to battery and It is required that gradually increasing.Its most concerned key index is concentrated mainly on five broad aspects：Safety and stability performance, cycle life, resistance to width Warm nature, charging rate and energy density.
Now, effect of the lithium ion battery in social development is higher and higher.Therefore, high-performance, environmentally protective is developed Electrode material becomes the research hotspot of lithium ion battery.Lithium ion battery negative material is based on graphitized carbon material at present, but Carbon material has the following disadvantages：（1）SEI film is generated in discharge process for the first time, causes irreversible capacity loss, or even causes carbon electric Pole internal structure change and poor contact；（2）Because the decomposition of protective layer, leads to battery failure or cause safe sexual behavior when high temperature Therefore；（3）Unit volume capacity is relatively low.Since metal, metal oxide and its composite material have high specific capacity, They become the substitute of lithium ion battery negative material, have biggish development potentiality.
Existing research shows that nanometer transition metal aoxidizes theoretical specific capacity with higher, and capacity retention ratio is high, such as The oxide of silicon, titanium, tin etc. has become a hot topic of research.But this kind of transition metal oxide material lithium ion be embedded in and deviate from Biggish volume expansion and contraction change are had in the process, so as to cause the dusting of electrode material, and then lose electricity with collector Contact, the cycle performance of the such material of strong influence and application.
Summary of the invention
The present invention provides a kind of preparation method of lithium battery carbon coating oxidation tin negative pole material, the oxygen that the method uses Change tin is nano-scale fiber shape, is covered with uniform through hole on single fiber, and the volume expansion for effectively inhibiting tin oxide is received Contracting, under equal conditions, embeddable more lithium ion improves the energy density of battery；The present invention is compound by carbon nitrogen, mentions The high electric conductivity of active material, in addition, body when the cavity between the carbon-coating and tin oxide of N doping is active material Li insertion extraction Long-pending expansion provides the useful space, it is therefore prevented that the dusting of tin oxide is reunited.
To achieve the goals above, the present invention provides a kind of preparation side of lithium battery carbon coating oxidation tin negative pole material Method, this method comprises the following steps：
（1）Prepare porous oxidation tin material
By powdered potassium chloride and glass putty with mass ratio 10：（150-200）It is uniformly mixed, is then fed into screw extruder, if The temperature for setting Screw Extrusion press is 240-250 DEG C, grinds potassium chloride to form crystal grain simultaneously by the rotational shear of screw rod, dispersion It is dispersed in the tin of semi-molten state and forms doped tin；
By to doped tin be sent into high temperature and pressure homogenizer while hot, setting temperature is 350-360 DEG C, and high pressure gas is nitrogen, is led to Homogenizer high temperature and pressure is crossed, so that doped tin is formed injection stream and enters high voltage electrostatic spinning, obtains radial being receiving for Nano grade Rice noodles；
Obtained nano wire is sent into two stepwise fluidized beds, the first rank fluidized-bed temperature is set between 170-200 DEG C, by filling The air of foot aoxidizes nano wire quickly in complete suspended state lower surface, reacts 20-40s, forms the nano wire of surface oxidation； Subsequently into second-order fluidized bed, second-order fluidized-bed temperature is set between 820-840 DEG C, nanometer is made by sufficient air Line quickly aoxidizes under complete suspended state, and the potassium chloride crystal grain for being doped in tin with this condition melts to form crystal grain defective hole, Tin is oxidized simultaneously, so that tin oxide nano-wire is covered with uniform through hole；
Obtained material is cleaned with deionized water, removes remaining potassium chloride, drying, refinement obtain porous oxidation tin；
（2）Prepare silica cladding tin oxide presoma
By the porous oxidation tin of 60 parts by weight be dispersed in 150-180 parts by weight by ethylene glycol and water by volume 3:1 composition In mixed liquor, 10-60min is stirred by ultrasonic, 2-4 parts by weight ammonium hydroxide and 0.2-0.3 parts by weight then is being added just under agitation Tetraethyl orthosilicate continues to stir 8-14h, centrifugation, washing, i.e. acquisition silica coats tin oxide presoma；
（3）The silica cladding tin oxide presoma of acquisition is dispersed in 100 parts by weight of ethanol, 1-2 parts by weight are then added High molecular surfactant, stir 20-30h, centrifugation, washing；
It disperses silica cladding tin oxide presoma after washing in 80 parts by weight of deionized water, 0.3-0.35 weight is then added Part pyrrole monomer, ultrasonic 45-50min are measured, then it is drawing for 20-25mmol/L that 50 parts by weight concentration are added dropwise under agitation Send out agent solution, last polymerization reaction 4-12h, centrifugation, washing, drying；
（4）Product after the drying is placed in atmosphere of inert gases, is warming up to 570 with the heating rate of 5 DEG C -8 DEG C/min DEG C -630 DEG C, anneal 1-3h, and polypyrrole is made to be carbonized；
Product after the carbonization is put into alkaline solution and is performed etching, to remove SiO2To get negative to carbon coating tin oxide Pole material.
Preferably, the pressure of the high temperature and pressure homogenizer is set as 4-7MPa, is 20- in the reaction time of the first rank 25s。
Preferably, the high molecular surfactant is poly amic acid, hydroxyethyl cellulose and polyoxyethylene copolymerization At least one of object；The initiator is at least one of ammonium persulfate, potassium bichromate and Potassiumiodate.
The invention has the advantages that and remarkable result：
（1）The tin oxide that the method for stating uses is covered with uniform through hole on single fiber, effectively presses down for nano-scale fiber shape The volume expansion of oxygenerating tin is shunk, and under equal conditions, embeddable more lithium ion improves the energy density of battery；
（2）The present invention is compound by carbon nitrogen, the electric conductivity of active material is improved, in addition, the carbon-coating and tin oxide of N doping Between cavity for active material Li insertion extraction when volume expansion provide the useful space, it is therefore prevented that the dusting of tin oxide is reunited.
Specific embodiment
Embodiment one
By powdered potassium chloride and glass putty with mass ratio 10：150 are uniformly mixed, and are then fed into screw extruder, and screw rod is arranged The temperature for squeezing out press is 240 DEG C, grinds potassium chloride to form crystal grain and be dispersed in by the rotational shear of screw rod, dispersion Doped tin is formed in the tin of semi-molten state.
By to doped tin be sent into high temperature and pressure homogenizer while hot, setting temperature is 350 DEG C, and high pressure gas is nitrogen, is led to Homogenizer high temperature and pressure is crossed, so that doped tin is formed injection stream and enters high voltage electrostatic spinning, obtains radial being receiving for Nano grade Rice noodles.
Obtained nano wire is sent into two stepwise fluidized beds, the first rank fluidized-bed temperature is set between 170 DEG C, by filling The air of foot aoxidizes nano wire quickly in complete suspended state lower surface, reacts 20s, forms the nano wire of surface oxidation；So Enter second-order fluidized bed afterwards, second-order fluidized-bed temperature is set between 820 DEG C, makes nano wire complete by sufficient air It is quickly aoxidized under full suspended state, the potassium chloride crystal grain for being doped in tin with this condition melts to form crystal grain defective hole, while tin It is oxidized, so that tin oxide nano-wire is covered with uniform through hole.Obtained material is cleaned with deionized water, is removed residual Remaining potassium chloride, drying, refinement, obtains porous oxidation tin.
Wherein, the pressure of the high temperature and pressure homogenizer is set as 4MPa, is 20s in the reaction time of the first rank.
By the porous oxidation tin of 60 parts by weight be dispersed in 150 parts by weight by ethylene glycol and water by volume 3:1 composition In mixed liquor, 10min is stirred by ultrasonic, 2-4 parts by weight ammonium hydroxide and the positive silicic acid tetrem of 0.2 parts by weight are then added under agitation Ester continues to stir 8h, centrifugation, washing, i.e. acquisition silica coats tin oxide presoma.
The silica cladding tin oxide presoma of acquisition is dispersed in 100 parts by weight of ethanol, 1 parts by weight are then added High molecular surfactant stirs 20h, centrifugation, washing；80 weight are dispersed by silica cladding tin oxide presoma after washing In part deionized water, 0.3 parts by weight pyrrole monomer, ultrasonic 45min is then added, then 50 weight are added dropwise under agitation The initiator solution that part concentration is 20mmol/L, last polymerization reaction 4h, centrifugation, washing, drying；By the product after the drying It is placed in atmosphere of inert gases, is warming up to 570 DEG C with the heating rate of 5 DEG C/min, anneal 1h, and polypyrrole is made to be carbonized；It will be described Product after carbonization, which is put into alkaline solution, to be performed etching, to remove SiO2Tin negative pole material is aoxidized to get to carbon coating.
Wherein, the high molecular surfactant is poly amic acid, hydroxyethyl cellulose and polyoxyethylene analog copolymer At least one of；The initiator is at least one of ammonium persulfate, potassium bichromate and Potassiumiodate.
Embodiment two
By powdered potassium chloride and glass putty with mass ratio 10：200 are uniformly mixed, and are then fed into screw extruder, and screw rod is arranged The temperature for squeezing out press is 250 DEG C, grinds potassium chloride to form crystal grain and be dispersed in by the rotational shear of screw rod, dispersion Doped tin is formed in the tin of semi-molten state.
By to doped tin be sent into high temperature and pressure homogenizer while hot, setting temperature is 360 DEG C, and high pressure gas is nitrogen, is led to Homogenizer high temperature and pressure is crossed, so that doped tin is formed injection stream and enters high voltage electrostatic spinning, obtains radial being receiving for Nano grade Rice noodles.
Obtained nano wire is sent into two stepwise fluidized beds, the first rank fluidized-bed temperature is set between 200 DEG C, by filling The air of foot aoxidizes nano wire quickly in complete suspended state lower surface, reacts 40s, forms the nano wire of surface oxidation；So Enter second-order fluidized bed afterwards, second-order fluidized-bed temperature is set between 840 DEG C, makes nano wire complete by sufficient air It is quickly aoxidized under full suspended state, the potassium chloride crystal grain for being doped in tin with this condition melts to form crystal grain defective hole, while tin It is oxidized, so that tin oxide nano-wire is covered with uniform through hole.Obtained material is cleaned with deionized water, is removed residual Remaining potassium chloride, drying, refinement, obtains porous oxidation tin.
Wherein, the pressure of the high temperature and pressure homogenizer is set as 7MPa, is 25s in the reaction time of the first rank.
By the porous oxidation tin of 60 parts by weight be dispersed in 180 parts by weight by ethylene glycol and water by volume 3:1 composition In mixed liquor, 60min is stirred by ultrasonic, 4 parts by weight ammonium hydroxide and the positive silicic acid tetrem of 0.3 parts by weight are then added under agitation Ester continues to stir 14h, centrifugation, washing, i.e. acquisition silica coats tin oxide presoma.
The silica cladding tin oxide presoma of acquisition is dispersed in 100 parts by weight of ethanol, 2 parts by weight are then added High molecular surfactant stirs 30h, centrifugation, washing；80 weight are dispersed by silica cladding tin oxide presoma after washing In part deionized water, 0.35 parts by weight pyrrole monomer, ultrasonic 50min is then added, then 50 weights are added dropwise under agitation Measure the initiator solution that part concentration is 25mmol/L, last polymerization reaction 12h, centrifugation, washing, drying；After the drying Product is placed in atmosphere of inert gases, is warming up to 630 DEG C with the heating rate of 8 DEG C/min, and anneal 3h, and polypyrrole is made to be carbonized；It will Product after the carbonization, which is put into alkaline solution, to be performed etching, to remove SiO2Tin negative pole material is aoxidized to get to carbon coating.
Wherein, the high molecular surfactant is polyoxyethylene analog copolymer；The initiator is Potassiumiodate.
Using above-described embodiment one, two products therefrom materials as being used for cathode of lithium battery, with just extremely LiFePO 4 material The test battery pack of composition carries out cyclical stability test, and discharge capacity is respectively 725mAh/g and 731mAh/g, circulation for the first time Capacity is 688mAh/g and 690mAh/g after 200 times, has good cyclical stability.

Claims (3)

1. a kind of lithium battery aoxidizes the preparation method of tin negative pole material with carbon coating, this method comprises the following steps：
（1）Prepare porous oxidation tin material
By powdered potassium chloride and glass putty with mass ratio 10：（150-200）It is uniformly mixed, is then fed into screw extruder, if The temperature for setting Screw Extrusion press is 240-250 DEG C, grinds potassium chloride to form crystal grain simultaneously by the rotational shear of screw rod, dispersion It is dispersed in the tin of semi-molten state and forms doped tin；
By to doped tin be sent into high temperature and pressure homogenizer while hot, setting temperature is 350-360 DEG C, and high pressure gas is nitrogen, is led to Homogenizer high temperature and pressure is crossed, so that doped tin is formed injection stream and enters high voltage electrostatic spinning, obtains radial being receiving for Nano grade Rice noodles；
Obtained nano wire is sent into two stepwise fluidized beds, the first rank fluidized-bed temperature is set between 170-200 DEG C, by filling The air of foot aoxidizes nano wire quickly in complete suspended state lower surface, reacts 20-40s, forms the nano wire of surface oxidation； Subsequently into second-order fluidized bed, second-order fluidized-bed temperature is set between 820-840 DEG C, nanometer is made by sufficient air Line quickly aoxidizes under complete suspended state, and the potassium chloride crystal grain for being doped in tin with this condition melts to form crystal grain defective hole, Tin is oxidized simultaneously, so that tin oxide nano-wire is covered with uniform through hole；
Obtained material is cleaned with deionized water, removes remaining potassium chloride, drying, refinement obtain porous oxidation tin；
（2）Prepare silica cladding tin oxide presoma
By the porous oxidation tin of 60 parts by weight be dispersed in 150-180 parts by weight by ethylene glycol and water by volume 3:1 composition In mixed liquor, 10-60min is stirred by ultrasonic, 2-4 parts by weight ammonium hydroxide and 0.2-0.3 parts by weight then is being added just under agitation Tetraethyl orthosilicate continues to stir 8-14h, centrifugation, washing, i.e. acquisition silica coats tin oxide presoma；
（3）The silica cladding tin oxide presoma of acquisition is dispersed in 100 parts by weight of ethanol, 1-2 parts by weight are then added High molecular surfactant, stir 20-30h, centrifugation, washing；
It disperses silica cladding tin oxide presoma after washing in 80 parts by weight of deionized water, 0.3-0.35 weight is then added Part pyrrole monomer, ultrasonic 45-50min are measured, then it is drawing for 20-25mmol/L that 50 parts by weight concentration are added dropwise under agitation Send out agent solution, last polymerization reaction 4-12h, centrifugation, washing, drying；
（4）Product after the drying is placed in atmosphere of inert gases, is warming up to 570 with the heating rate of 5 DEG C -8 DEG C/min DEG C -630 DEG C, anneal 1-3h, and polypyrrole is made to be carbonized；
Product after the carbonization is put into alkaline solution and is performed etching, to remove SiO2To get arrive carbon coating tin oxide cathode Material.
2. the method as described in claim 1, which is characterized in that the pressure of the high temperature and pressure homogenizer is set as 4-7MPa, It is 20-25s in the reaction time of the first rank.
3. method according to claim 1 or 2, which is characterized in that the high molecular surfactant is poly amic acid, hydroxyl At least one of ethyl cellulose and polyoxyethylene analog copolymer；The initiator is ammonium persulfate, potassium bichromate and acid iodide At least one of potassium.
CN201810631175.0A 2018-06-19 2018-06-19 A kind of lithium battery aoxidizes the preparation method of tin negative pole material with carbon coating Pending CN108899491A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112086631A (en) * 2020-09-18 2020-12-15 合肥国轩电池材料有限公司 Preparation method of Sn-based negative electrode plate of lithium ion battery

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106816595A (en) * 2017-03-09 2017-06-09 合肥工业大学 A kind of lithium ion battery coats di-iron trioxide negative material and preparation method thereof with nitrogen-doped carbon
CN106867263A (en) * 2017-03-24 2017-06-20 浙江师范大学 ZnFe2O4@SiO2@RGO wave absorbing agents and its preparation technology
CN106946285A (en) * 2017-03-20 2017-07-14 成都新柯力化工科技有限公司 A kind of lithium battery fibrous porous oxidation tin negative pole material and preparation method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106816595A (en) * 2017-03-09 2017-06-09 合肥工业大学 A kind of lithium ion battery coats di-iron trioxide negative material and preparation method thereof with nitrogen-doped carbon
CN106946285A (en) * 2017-03-20 2017-07-14 成都新柯力化工科技有限公司 A kind of lithium battery fibrous porous oxidation tin negative pole material and preparation method
CN106867263A (en) * 2017-03-24 2017-06-20 浙江师范大学 ZnFe2O4@SiO2@RGO wave absorbing agents and its preparation technology

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112086631A (en) * 2020-09-18 2020-12-15 合肥国轩电池材料有限公司 Preparation method of Sn-based negative electrode plate of lithium ion battery

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