CN108807987A - A kind of preparation method of carbon coating selenizing tin negative pole material - Google Patents

A kind of preparation method of carbon coating selenizing tin negative pole material Download PDF

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Publication number
CN108807987A
CN108807987A CN201810740659.9A CN201810740659A CN108807987A CN 108807987 A CN108807987 A CN 108807987A CN 201810740659 A CN201810740659 A CN 201810740659A CN 108807987 A CN108807987 A CN 108807987A
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weight
parts
stannic selenide
snse
solution
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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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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
    • H01M4/62—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
    • H01M4/36—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
    • 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 discloses a kind of preparation methods of carbon coating selenizing tin negative pole material, and preparation method of the present invention is simple, and experimental repeatability is high, the period is short, and the needs for being suitble to large-scale production to prepare have significant scientific meaning in terms of lithium ion battery applications；The stannic selenide that the method uses is covered with uniform through hole for nano-scale fiber shape on single fiber, and the volume expansion for effectively inhibiting stannic selenide is shunk；The present invention is compound by carbon nitrogen, improves the electric conductivity of active material, in addition, the cavity between the carbon-coating and stannic selenide of N doping for active material Li insertion extraction when volume expansion provide the useful space, it is therefore prevented that the dusting of stannic selenide is reunited.

Description

A kind of preparation method of carbon coating selenizing tin negative pole material
Technical field
The present invention relates to battery material fields, and in particular to a kind of preparation method of carbon coating selenizing tin negative pole material.
Background technology
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 films are generated in discharge process for the first time, cause irreversible capacity loss, or even cause 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 larger development potentiality.
Have studies have shown that the oxidation of nanometer transition metal has higher theoretical specific capacity, and capacity retention ratio is high.Especially It is tin base cathode material, because tin base cathode not only has higher theoretical capacity, but also is easy to the member with the Vth main group Element and the element of the VIth main group form the alloy cpd of two-phase.In recent years, for SnSb, Sn3P4、SnO2、SnS2The conjunction of equal tin The report of gold compound is relatively more, but for SnSe2Report it is fewer.SnSe2For the layer structure of hexagonal phase, layer and layer Between combination it is weaker, be conducive to the insertion and abjection of lithium ion, as negative material have larger development space.But By SnSe2Negative material is applied in practice, and it still needs further improvement for chemical property.
Invention content
The present invention provides a kind of preparation method of carbon coating selenizing tin negative pole material, preparation method letter of the present invention Single, experimental repeatability is high, the period is short, the needs for being suitble to large-scale production to prepare, and has in terms of lithium ion battery applications notable Scientific meaning；The stannic selenide that the method uses is covered with uniform through hole on single fiber, has for nano-scale fiber shape Effect ground inhibits the volume expansion of stannic selenide to shrink；The present invention is compound by carbon nitrogen, improves the electric conductivity of active material, separately Outside, the cavity between the carbon-coating and stannic selenide of N doping for active material Li insertion extraction when volume expansion provide the useful space, The dusting of stannic selenide is prevented to reunite.
To achieve the goals above, the present invention provides a kind of preparation method of carbon coating selenizing tin negative pole material, this method Include the following steps：
（1）Prepare porous selenizing tin material
Stannic chloride is taken to be add to deionized water, stirring to form solution one to being completely dissolved；Selenium powder is weighed, hydrazine hydrate is added to In, stirring to form solution two to being completely dissolved；Then solution two is added dropwise to formation mixed solution three in solution one, and stirred It mixes uniformly；Wherein, the molar ratio of tin ion and selenium atom is 1：(2-3)；
Above-mentioned mixed liquor three is transferred in water heating kettle, water heating kettle is then placed in hydro-thermal reaction instrument in 220-230 DEG C of reaction, instead It cools to room temperature after answering with the furnace, is then washed respectively with deionized water and absolute ethyl alcohol, centrifuges and obtain the powder of black, it will Isolated powder dries to obtain SnSe2It is nanocrystalline.
By powdered potassium chloride and SnSe2It is nanocrystalline with mass ratio 10：（150-200）It is uniformly mixed, is then fed into spiral shell The temperature of bar extruder, setting Screw Extrusion press is 340-350 DEG C, so that potassium chloride is ground by the rotational shear of screw rod, dispersion Mill forms crystal grain and is dispersed in the SnSe of semi-molten state2It is nanocrystalline；
By to SnSe2Nanocrystalline to be sent into high temperature and pressure homogenizer while hot, setting temperature is 450-460 DEG C, and high pressure gas is nitrogen Gas makes doped tin form injection stream and enters high voltage electrostatic spinning, obtain radial SnSe by homogenizer high temperature and pressure2Nanometer Line；
The radial SnSe that will be obtained2Nano wire is cleaned with deionized water, removes remaining potassium chloride, and drying, refinement obtain porous Stannic selenide；
（2）Prepare silica cladding stannic selenide presoma
By the porous stannic selenide 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 are being added just under agitation Tetraethyl orthosilicate continues to stir 8-14h, centrifugation, washing obtain silica and coat stannic selenide presoma；
（3）The silica cladding stannic selenide 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；
Silica cladding stannic selenide presoma after washing is scattered in 80 parts by weight of deionized water, 0.3-0.35 weights are then added Part pyrrole monomer, ultrasonic 45-50min are measured, then drawing for a concentration of 20-25mmol/L of 50 parts by weight is added dropwise under agitation Send out agent solution, last polymerisation 4-12h, centrifugation, washing, drying；
（4）Product after the drying is placed in atmosphere of inert gases, 570 are warming up to 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 stannic selenide Pole material.
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 stannic selenide 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 stannic selenide processed is shunk, and under equal conditions, can be embedded in more lithium ion, be improved the energy density of battery；
（2）The present invention is compound by carbon nitrogen, improves the electric conductivity of active material, in addition, the carbon-coating and stannic selenide 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 stannic selenide is reunited；
（3）Preparation method of the present invention is simple, and experimental repeatability is high, the period is short, the need for being suitble to large-scale production to prepare It wants, there is significant scientific meaning in terms of lithium ion battery applications.
Specific implementation mode
Embodiment one
Stannic chloride is taken to be add to deionized water, stirring to form solution one to being completely dissolved；Selenium powder is weighed, hydrazine hydrate is added to In, stirring to form solution two to being completely dissolved；Then solution two is added dropwise to formation mixed solution three in solution one, and stirred It mixes uniformly；Wherein, the molar ratio of tin ion and selenium atom is 1：2；Above-mentioned mixed liquor three is transferred in water heating kettle, then by water Hot kettle is placed in hydro-thermal reaction instrument in 220 DEG C of reactions, cools to room temperature with the furnace after reaction, then uses deionized water and anhydrous second Alcohol washs respectively, centrifuges and obtains the powder of black, dries isolated powder to obtain SnSe2It is nanocrystalline.It will be powdered Potassium chloride and SnSe2It is nanocrystalline with mass ratio 10：150 are uniformly mixed, and are then fed into screw extruder, and Screw Extrusion press is arranged Temperature be 340 DEG C, make potassium chloride grind to form crystal grain and be dispersed in semi-molten shape by the rotational shear of screw rod, dispersion The SnSe of state2It is nanocrystalline.
By to SnSe2Nanocrystalline to be sent into high temperature and pressure homogenizer while hot, setting temperature is 450-460 DEG C, high pressure gas So that doped tin is formed injection stream by homogenizer high temperature and pressure for nitrogen and enter high voltage electrostatic spinning, obtain radial SnSe2 Nano wire；The radial SnSe that will be obtained2Nano wire is cleaned with deionized water, removes remaining potassium chloride, and drying, refinement obtain Porous stannic selenide.
By the porous stannic selenide 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 obtain silica and coat stannic selenide presoma.
The silica cladding stannic selenide 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；Silica cladding stannic selenide presoma after washing is scattered in 80 weight 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 of a concentration of 20mmol/L of part, last polymerisation 4h, centrifugation, washing, drying；By the product after the drying It is placed in atmosphere of inert gases, 570 DEG C is warming up to 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 SiO2To get to carbon coating selenizing tin negative pole material.
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
Stannic chloride is taken to be add to deionized water, stirring to form solution one to being completely dissolved；Selenium powder is weighed, hydrazine hydrate is added to In, stirring to form solution two to being completely dissolved；Then solution two is added dropwise to formation mixed solution three in solution one, and stirred It mixes uniformly；Wherein, the molar ratio of tin ion and selenium atom is 1：3；Above-mentioned mixed liquor three is transferred in water heating kettle, then by water Hot kettle is placed in hydro-thermal reaction instrument in 230 DEG C of reactions, cools to room temperature with the furnace after reaction, then uses deionized water and anhydrous second Alcohol washs respectively, centrifuges and obtains the powder of black, dries isolated powder to obtain SnSe2It is nanocrystalline.It will be powdered Potassium chloride and SnSe2It is nanocrystalline with mass ratio 10：200 are uniformly mixed, and are then fed into screw extruder, and Screw Extrusion press is arranged Temperature be 350 DEG C, make potassium chloride grind to form crystal grain and be dispersed in semi-molten shape by the rotational shear of screw rod, dispersion The SnSe of state2It is nanocrystalline.
By to SnSe2Nanocrystalline to be sent into high temperature and pressure homogenizer while hot, setting temperature is 460 DEG C, and high pressure gas is nitrogen Gas makes doped tin form injection stream and enters high voltage electrostatic spinning, obtain radial SnSe by homogenizer high temperature and pressure2Nanometer Line；The radial SnSe that will be obtained2Nano wire is cleaned with deionized water, removes remaining potassium chloride, and drying, refinement obtain porous Stannic selenide.
By the porous stannic selenide 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 obtain silica and coat stannic selenide presoma.
The silica cladding stannic selenide 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；Silica cladding stannic selenide presoma after washing is scattered in 80 weight 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 of a concentration of 25mmol/L of part, last polymerisation 12h, centrifugation, washing, drying；After the drying Product is placed in atmosphere of inert gases, and 630 DEG C are warming up to 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 SiO2To get to carbon coating selenizing tin negative pole material.
Wherein, the high molecular surfactant is polyoxyethylene analog copolymer；The initiator is Potassiumiodate.
Using above-described embodiment one, two products therefrom materials as cathode of lithium battery is used for, with just extremely LiFePO 4 material The test battery pack of composition carries out cyclical stability test, and discharge capacity is respectively 773mAh/g and 761mAh/g, cycle for the first time Capacity is 738mAh/g and 715mAh/g after 200 times, has good cyclical stability.

Claims (2)

1. a kind of preparation method of carbon coating selenizing tin negative pole material, this method comprises the following steps：
（1）Prepare porous selenizing tin material
Stannic chloride is taken to be add to deionized water, stirring to form solution one to being completely dissolved；Selenium powder is weighed, hydrazine hydrate is added to In, stirring to form solution two to being completely dissolved；Then solution two is added dropwise to formation mixed solution three in solution one, and stirred It mixes uniformly；Wherein, the molar ratio of tin ion and selenium atom is 1：(2-3)；
Above-mentioned mixed liquor three is transferred in water heating kettle, water heating kettle is then placed in hydro-thermal reaction instrument in 220-230 DEG C of reaction, instead It cools to room temperature after answering with the furnace, is then washed respectively with deionized water and absolute ethyl alcohol, centrifuges and obtain the powder of black, it will Isolated powder dries to obtain SnSe2It is nanocrystalline；
By powdered potassium chloride and SnSe2It is nanocrystalline with mass ratio 10：（150-200）It is uniformly mixed, is then fed into screw extruding The temperature of machine, setting Screw Extrusion press is 340-350 DEG C, makes potassium chloride grind to be formed by the rotational shear of screw rod, dispersion Crystal grain and the SnSe for being dispersed in semi-molten state2It is nanocrystalline；
By to SnSe2Nanocrystalline to be sent into high temperature and pressure homogenizer while hot, setting temperature is 450-460 DEG C, and high pressure gas is nitrogen Gas makes doped tin form injection stream and enters high voltage electrostatic spinning, obtain radial SnSe by homogenizer high temperature and pressure2Nanometer Line；
The radial SnSe that will be obtained2Nano wire is cleaned with deionized water, removes remaining potassium chloride, and drying, refinement obtain porous Stannic selenide；
（2）Prepare silica cladding stannic selenide presoma
By the porous stannic selenide 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 are being added just under agitation Tetraethyl orthosilicate continues to stir 8-14h, centrifugation, washing obtain silica and coat stannic selenide presoma；
（3）The silica cladding stannic selenide 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；
Silica cladding stannic selenide presoma after washing is scattered in 80 parts by weight of deionized water, 0.3-0.35 weights are then added Part pyrrole monomer, ultrasonic 45-50min are measured, then drawing for a concentration of 20-25mmol/L of 50 parts by weight is added dropwise under agitation Send out agent solution, last polymerisation 4-12h, centrifugation, washing, drying；
（4）Product after the drying is placed in atmosphere of inert gases, 570 are warming up to 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 to carbon coating stannic selenide cathode Material.
2. the method as described in claim 1, which is characterized in that the high molecular surfactant is poly amic acid, hydroxyl second At least one of base cellulose and polyoxyethylene analog copolymer；The initiator is ammonium persulfate, potassium bichromate and Potassiumiodate At least one of.
CN201810740659.9A 2018-07-07 2018-07-07 A kind of preparation method of carbon coating selenizing tin negative pole material Pending CN108807987A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111573633A (en) * 2020-05-28 2020-08-25 哈尔滨工业大学 Preparation method and application of carbon-coated tin selenide negative electrode material
CN114988419A (en) * 2022-05-25 2022-09-02 陕西科技大学 SiO (silicon dioxide) 2 SnSe/C nanosphere and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106784598A (en) * 2016-12-19 2017-05-31 陕西科技大学 A kind of used as negative electrode of Li-ion battery flake SnSe2Nanocrystalline preparation method
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106784598A (en) * 2016-12-19 2017-05-31 陕西科技大学 A kind of used as negative electrode of Li-ion battery flake SnSe2Nanocrystalline preparation method
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

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111573633A (en) * 2020-05-28 2020-08-25 哈尔滨工业大学 Preparation method and application of carbon-coated tin selenide negative electrode material
CN114988419A (en) * 2022-05-25 2022-09-02 陕西科技大学 SiO (silicon dioxide) 2 SnSe/C nanosphere and preparation method thereof
CN114988419B (en) * 2022-05-25 2023-12-08 陕西科技大学 SiO (silicon dioxide) 2 SnSe/C nanospheres and preparation method thereof

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Application publication date: 20181113