CN107959024A - A kind of sodium-ion battery anode sheet Sb2Se3Nanocrystalline preparation method - Google Patents

A kind of sodium-ion battery anode sheet Sb2Se3Nanocrystalline preparation method Download PDF

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CN107959024A
CN107959024A CN201711085707.7A CN201711085707A CN107959024A CN 107959024 A CN107959024 A CN 107959024A CN 201711085707 A CN201711085707 A CN 201711085707A CN 107959024 A CN107959024 A CN 107959024A
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sodium
solution
ion battery
battery anode
anode sheet
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CN107959024B (en
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曹丽云
郭玲
李嘉胤
黄剑锋
程娅伊
齐慧
李倩颖
仵婉晨
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Shaanxi University of Science and Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/581Chalcogenides or intercalation compounds thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/054Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

A kind of sodium-ion battery anode sheet Sb2Se3Nanocrystalline preparation method, polyvinylpyrrolidone and tartaric acid are added in deionized water and obtain solution A 1, and potassium antimony tartrate then is added solution A 1 obtains solution A 2;Solution B is obtained in the hydrazine hydrate that sodium selenite is added to;Solution B is added dropwise in solution A 2 and obtains mixed liquor C;Mixed liquor C is transferred to polytetrafluoroethyllining lining, is put into homogeneous reaction instrument, room temperature is cooled to the furnace after 100~150 DEG C of reactions, washs precipitation and separation repeatedly with deionized water and absolute ethyl alcohol, freeze-drying obtains sodium-ion battery anode sheet Sb2Se3It is nanocrystalline.The present invention uses one step hydro thermal method, and equipment is simple, green safe, and reaction temperature is relatively low, reproducible, is adapted to large-scale production;The characteristics of product morphology structure easy to control using liquid phase environment, under the action of polyvinylpyrrolidone and tartaric acid, induced crystal development, successfully prepares sheet pure phase Sb2Se3It is nanocrystalline.

Description

A kind of sodium-ion battery anode sheet Sb2Se3Nanocrystalline preparation method
Technical field
The invention belongs to electrochemical energy storage field, and in particular to a kind of sodium-ion battery anode sheet Sb2Se3It is nanocrystalline Preparation method.
Background technology
The development of lithium ion battery starts from about 1980, with continuous progressive, the scientific and technical continuous development of society, section Scholars also gradually recognize the restriction that lithium resource shortage develops for lithium ion battery.Therefore, and its same main group and store up The abundant sodium-ion battery with similar electrochemical behavior of amount gradually causes the concern of numerous researchers.Antimony base selenides sodium from Sub- cell negative electrode material Sb2Se3, a kind of V-VI compounds of group with layer structure, as anode material of lithium-ion battery, The Sb2Se3 of 1mol can be embedded in the Na+ of 12mol, and the conversion reaction occurred is a reversible process, these all promote Sb2Se3With good chemical property, such as high theoretical capacity:678mAh·g-1.But apart from practical application, its electrification Performance is learned to need to be improved.
According to the literature, the nano material for preparing two-dimensional sheet structure be improve chemical property most efficient method it One, it can not only shorten ion and electric transmission path, but also the contact after material nano with electrolyte in a thickness direction Area can also increase, simultaneously for the larger negative material of some bulk effects such as Sb2Se3, can effectively alleviate material after nanosizing Structural damage and dusting, significantly improve chemical property during sodium ion deintercalation.At present, for two-dimensional sheet Sb2Se3Nanocrystalline report as anode material of lithium-ion battery or fewer.Song H et al. are using hydrone intercalation Method prepares two-dimensional slice shape Sb2Se3(Song H,et al.,Highly Anisotropic Sb2Se3Nanosheets: Gentle Exfoliation from theBulk Precursors Possessing 1D Crystal Structure.Adv Mater, 2017.) Jin, R et al. prepares nanometer sheet assembling vermiform using the method for solvent heat Sb2Se3With good hydrogen storage property.(Jin,R.;Chen,G.;Wang,Q.;Sun,J.;Wang,Y.,A facile solvothermal synthesis of hierarchical Sb2Se3nanostructures with high electrochemical hydrogen storage ability.Journal of Materials Chemistry 2011, 21 (18), 6628.) therefore, a kind of open simple preparation sheet Sb2Se3Method and its as anode material of lithium-ion battery Partial test is the result is that significantly.
The content of the invention
It is an object of the invention to propose a kind of sodium-ion battery anode sheet Sb2Se3Nanocrystalline preparation method, institute The Sb of preparation2Se3It is nanocrystalline that there is two-dimensional sheet structure, and Nano grade is in a thickness direction, as sodium-ion battery Negative material shows excellent cyclical stability and high rate performance.
To reach above-mentioned purpose, the technical solution adopted by the present invention is:
1) (0.001g~0.005g) is pressed:(0.2g~2g):The mass ratio of (0.169g~1.0139g) takes polyvinyl pyrrole Alkanone, tartaric acid and potassium antimony tartrate, polyvinylpyrrolidone and tartaric acid are added in the deionized water of 25~70ml, stirring It is completely dissolved to obtain clear solution A1 to it, then potassium antimony tartrate is added in solution A 1 and persistently stirs to obtain clear solution A2;
2) it is 1 by potassium antimony tartrate and sodium selenite:Sodium selenite is added to the water of 3~10mL by the molar ratio of (1~3) Close stirring in hydrazine and obtain claret solution B;Solution B is quickly added dropwise in solution A 2 under stirring after being dispersed with stirring uniformly and obtained Mixed liquor C;
3) mixed liquor C is transferred to polytetrafluoroethyllining lining, is put into homogeneous reaction instrument, in 100~150 DEG C of insulation reactions 1 After~12h, cool to room temperature with the furnace, precipitation and separation washed repeatedly with deionized water and absolute ethyl alcohol, freeze-drying gained sodium from Sub- battery cathode sheet Sb2Se3It is nanocrystalline.
Polyvinylpyrrolidonemolecules molecules amount is 30000 in the step 1).
Stirring uses magnetic stirring apparatus in the step 1), step 2), and speed of agitator is 500~800r/min.
The mass percent of hydrazine hydrate is 50% in the step 2).
The packing ratio that the mixed liquor C of the step 3) is transferred to polytetrafluoroethyllining lining is 30%~80%.
Step 3) the freeze-drying temperature is -40 DEG C, pressure 60Pa.
Relative to the prior art, the present invention has following beneficial effect:
First, the present invention uses one step hydro thermal method, and equipment is simple, green safe, and reaction temperature is relatively low, repeatability It is good, it is adapted to large-scale production;Further, the characteristics of product morphology structure easy to control using liquid phase environment, in polyvinyl pyrrole Under the action of alkanone and tartaric acid, induced crystal development, successfully prepares sheet pure phase Sb2Se3Nanocrystalline, the thickness of piece is about 10nm, is stacked, and leaves gap.By prepared Sb2Se3It is nanocrystalline to be used as active material, by 8:1:(0.5:0.5) Mass ratio by active material and binding agent (Kynoar PVDF), conductive agent (conductive black and electrically conductive graphite) in solvent In (N-methyl pyrrolidones) by grinding, slurry coating, drying, section after as anode in the glove box full of argon gas group Dress up button-shaped sodium-ion battery.Primary Study is carried out to its electrochemical behavior as anode material of lithium-ion battery, is found Sheet Sb prepared by the present invention2Se3Anode material of lithium-ion battery, in 0.1A g-1、0.2A g-1、0.5A g-1、1.0A g-1、2.0A g-1Current density under, discharge capacity is 550mAh g-1、400mAh g-1、350mAh g-1、300mAh g-1、 200mAh g-1, when current density turns again to 0.1A g-1When, capacity can also be maintained at 350mAh g-1, show excellent times Rate performance;And good cyclical stability is showed under high current.
Brief description of the drawings
Fig. 1 is the sodium-ion battery anode sheet Sb prepared by the embodiment of the present invention 32Se3Nanocrystalline X-ray diffraction (XRD) collection of illustrative plates;
Fig. 2 is the sodium-ion battery anode sheet Sb prepared by embodiment 32Se3Nanocrystalline scanning electron microscope (SEM) is shone Piece;
Fig. 3 is the sodium-ion battery anode sheet Sb prepared by embodiment 32Se3Nanocrystalline multiplying power figure;Wherein, Cycle number:Cycle-index;Capacity:Capacity.
Embodiment:
Embodiment 1:
1) tartaric acid of the polyvinylpyrrolidone of 0.001g and 0.2g are added in the deionized water of 25ml, in 500r/ Magnetic agitation is completely dissolved to obtain clear solution A1 to it under min, then adds the potassium antimony tartrate of 0.169g in solution A 1 Clear solution A2 is persistently stirred to obtain, wherein polyvinylpyrrolidonemolecules molecules amount is 30000;
2) it is 1 by potassium antimony tartrate and sodium selenite:Sodium selenite is added to the mass percent of 3mL by 1 molar ratio For magnetic agitation obtains claret solution B under 500r/min in 50% hydrazine hydrate;Solution B is quickly added dropwise under stirring Mixed liquor C is obtained after being dispersed with stirring in solution A 2 uniformly;
3) mixed liquor C is transferred in polytetrafluoroethyllining lining by 30% packing ratio, homogeneous reaction instrument is put into, 100 After DEG C insulation reaction 12h, cool to room temperature with the furnace, precipitation and separation is washed repeatedly with deionized water and absolute ethyl alcohol, at -40 DEG C, Freeze-drying obtains sodium-ion battery anode sheet Sb under 60Pa2Se3It is nanocrystalline.
Embodiment 2:
1) tartaric acid of the polyvinylpyrrolidone of 0.002g and 0.5g are added in the deionized water of 45ml, in 600r/ Magnetic agitation is completely dissolved to obtain clear solution A1 to it under min, then adds the potassium antimony tartrate of 0.338g in solution A 1 Clear solution A2 is persistently stirred to obtain, wherein polyvinylpyrrolidonemolecules molecules amount is 30000;
2) it is 1 by potassium antimony tartrate and sodium selenite:Sodium selenite is added to the quality percentage of 5mL by 1.5 molar ratio Number is magnetic agitation obtains claret solution B under 600r/min in 50% hydrazine hydrate;Solution B is quickly added dropwise under stirring Enter and obtain mixed liquor C after being dispersed with stirring in solution A 2 uniformly;
3) mixed liquor C is transferred in polytetrafluoroethyllining lining by 50% packing ratio, homogeneous reaction instrument is put into, 120 After DEG C insulation reaction 8h, cool to room temperature with the furnace, precipitation and separation is washed repeatedly with deionized water and absolute ethyl alcohol, at -40 DEG C, Freeze-drying obtains sodium-ion battery anode sheet Sb under 60Pa2Se3It is nanocrystalline.
Embodiment 3:
1) tartaric acid of the polyvinylpyrrolidone of 0.003g and 1.0g are added in the deionized water of 53ml, in 500r/ Magnetic agitation is completely dissolved to obtain clear solution A1 to it under min, then adds the potassium antimony tartrate of 0.6759g in solution A 1 Clear solution A2 is persistently stirred to obtain, wherein polyvinylpyrrolidonemolecules molecules amount is 30000;
2) it is 1 by potassium antimony tartrate and sodium selenite:Sodium selenite is added to the mass percent of 7mL by 2 molar ratio For magnetic agitation obtains claret solution B under 500r/min in 50% hydrazine hydrate;Solution B is quickly added dropwise under stirring Mixed liquor C is obtained after being dispersed with stirring in solution A 2 uniformly;
3) mixed liquor C is transferred in polytetrafluoroethyllining lining by 60% packing ratio, homogeneous reaction instrument is put into, 130 After DEG C insulation reaction 6h, cool to room temperature with the furnace, precipitation and separation is washed repeatedly with deionized water and absolute ethyl alcohol, at -40 DEG C, Freeze-drying obtains sodium-ion battery anode sheet Sb under 60Pa2Se3It is nanocrystalline.
With Rigaku D/max2000PCX- x ray diffractometer xs analysis sample (Sb2Se3Powder), find sample and JCPDS The Sb for the rhombic system that numbering is 15-08612Se3Structure is consistent and (Fig. 1) occurs without other miscellaneous peaks;By sample U.S. FEI The field emission scanning electron microscope (FESEM) of company's S-4800 types is observed, it can be seen that prepared pure phase Sb2Se3Receive Meter Jing Wei two-dimensional sheet structures, thickness are about 10nm, and piece is stacked with piece, and leaves gap.(Fig. 2).
By prepared two-dimensional sheet pure phase Sb2Se3Nanocrystalline and binding agent Kynoar PVDF, conductive agent conduction charcoal Black and electrically conductive graphite, mass ratio is according to 8:1:0.5:0.5, under conditions of N-methyl pyrrolidone as solvent, ground, slurry Button-shaped sodium-ion battery is assembled into the glove box full of argon gas as anode after body coating, drying, section, shelves 48h Afterwards, electrochemical property test is carried out using blue electric tester.In 0.1A g-1、0.2A g-1、0.5A g-1、1.0A g-1、2.0A g-1Current density under, discharge capacity is 550mAh g-1、400mAh g-1、350mAh g-1、300mAh g-1、200mAh g-1, When current density turns again to 0.1A g-1When, capacity can also be maintained at 350mAh g-1, show excellent high rate performance;And And good cyclical stability (Fig. 3) is showed under high current.
Embodiment 4:
1) tartaric acid of the polyvinylpyrrolidone of 0.004g and 1.5g are added in the deionized water of 61ml, in 800r/ Magnetic agitation is completely dissolved to obtain clear solution A1 to it under min, then adds the potassium antimony tartrate of 0.8848g in solution A 1 Clear solution A2 is persistently stirred to obtain, wherein polyvinylpyrrolidonemolecules molecules amount is 30000;
2) it is 1 by potassium antimony tartrate and sodium selenite:Sodium selenite is added to the quality percentage of 9mL by 2.5 molar ratio Number is magnetic agitation obtains claret solution B under 800r/min in 50% hydrazine hydrate;Solution B is quickly added dropwise under stirring Enter and obtain mixed liquor C after being dispersed with stirring in solution A 2 uniformly;
3) mixed liquor C is transferred in polytetrafluoroethyllining lining by 70% packing ratio, homogeneous reaction instrument is put into, 140 After DEG C insulation reaction 4h, cool to room temperature with the furnace, precipitation and separation is washed repeatedly with deionized water and absolute ethyl alcohol, at -40 DEG C, Freeze-drying obtains sodium-ion battery anode sheet Sb under 60Pa2Se3It is nanocrystalline.
Embodiment 5:
1) tartaric acid of the polyvinylpyrrolidone of 0.005g and 2g are added in the deionized water of 70ml, in 700r/min Lower magnetic agitation is completely dissolved to obtain clear solution A1 to it, then adds in solution A 1 potassium antimony tartrate of 1.0139g and holds Continuous to stir to obtain clear solution A2, wherein polyvinylpyrrolidonemolecules molecules amount is 30000;
2) it is 1 by potassium antimony tartrate and sodium selenite:Sodium selenite is added to the mass percent of 10mL by 3 molar ratio For magnetic agitation obtains claret solution B under 700r/min in 50% hydrazine hydrate;Solution B is quickly added dropwise under stirring Mixed liquor C is obtained after being dispersed with stirring in solution A 2 uniformly;
3) mixed liquor C is transferred in polytetrafluoroethyllining lining by 80% packing ratio, homogeneous reaction instrument is put into, 150 After DEG C insulation reaction 1h, cool to room temperature with the furnace, precipitation and separation is washed repeatedly with deionized water and absolute ethyl alcohol, at -40 DEG C, Freeze-drying obtains sodium-ion battery anode sheet Sb under 60Pa2Se3It is nanocrystalline.

Claims (6)

  1. A kind of 1. sodium-ion battery anode sheet Sb2Se3Nanocrystalline preparation method, it is characterised in that comprise the following steps:
    1) (0.001g~0.005g) is pressed:(0.2g~2g):The mass ratio of (0.169g~1.0139g) takes polyvinylpyrrolidine Ketone, tartaric acid and potassium antimony tartrate, polyvinylpyrrolidone and tartaric acid are added in the deionized water of 25~70ml, and stirring is extremely It is completely dissolved to obtain clear solution A1, then adds in solution A 1 potassium antimony tartrate and persistently stirs to obtain clear solution A2;
    2) it is 1 by potassium antimony tartrate and sodium selenite:Sodium selenite is added to the hydrazine hydrate of 3~10mL by the molar ratio of (1~3) Middle stirring obtains claret solution B;Solution B is quickly added dropwise in solution A 2 under stirring after being dispersed with stirring uniformly and mixed Liquid C;
    3) mixed liquor C is transferred to polytetrafluoroethyllining lining, is put into homogeneous reaction instrument, in 100~150 DEG C of 1~12h of insulation reaction Afterwards, cool to room temperature with the furnace, wash precipitation and separation repeatedly with deionized water and absolute ethyl alcohol, freeze-drying obtains sodium-ion battery Anode sheet Sb2Se3It is nanocrystalline.
  2. 2. sodium-ion battery anode sheet Sb according to claim 12Se3Nanocrystalline preparation method, its feature exist In:Polyvinylpyrrolidonemolecules molecules amount is 30000 in the step 1).
  3. 3. sodium-ion battery anode sheet Sb according to claim 12Se3Nanocrystalline preparation method, its feature exist In:Stirring uses magnetic stirring apparatus in the step 1), step 2), and speed of agitator is 500~800r/min.
  4. 4. sodium-ion battery anode sheet Sb according to claim 12Se3Nanocrystalline preparation method, its feature exist In:The mass percent of hydrazine hydrate is 50% in the step 2).
  5. 5. sodium-ion battery anode sheet Sb according to claim 12Se3Nanocrystalline preparation method, its feature exist In:The packing ratio that the mixed liquor C of the step 3) is transferred to polytetrafluoroethyllining lining is 30%~80%.
  6. 6. sodium-ion battery anode sheet Sb according to claim 12Se3Nanocrystalline preparation method, its feature exist In:Step 3) the freeze-drying temperature is -40 DEG C, pressure 60Pa.
CN201711085707.7A 2017-11-07 2017-11-07 Flaky Sb for sodium ion battery cathode2Se3Method for preparing nanocrystalline Active CN107959024B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108963237A (en) * 2018-08-07 2018-12-07 河北工业大学 A kind of preparation method of anode material of lithium-ion battery
CN109037670A (en) * 2018-07-10 2018-12-18 湖南鸿捷新材料有限公司 A kind of method of continuity preparation little particle ternary precursor material
CN113023706A (en) * 2021-03-10 2021-06-25 陕西科技大学 Carbon-coated antimony selenide/graphene composite material and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102583272A (en) * 2012-01-21 2012-07-18 哈尔滨工业大学 Vermicular Sb2Se3 hydrogen storage material and preparation method thereof
CN102897723A (en) * 2012-08-29 2013-01-30 江苏大学 Hydrothermal method for preparing selenium-copper-based nano-crystals
CN107055489A (en) * 2017-05-27 2017-08-18 陕西科技大学 It is a kind of to prepare the method that nano wire weaves spherical antimony selenide anode material of lithium-ion battery

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102583272A (en) * 2012-01-21 2012-07-18 哈尔滨工业大学 Vermicular Sb2Se3 hydrogen storage material and preparation method thereof
CN102897723A (en) * 2012-08-29 2013-01-30 江苏大学 Hydrothermal method for preparing selenium-copper-based nano-crystals
CN107055489A (en) * 2017-05-27 2017-08-18 陕西科技大学 It is a kind of to prepare the method that nano wire weaves spherical antimony selenide anode material of lithium-ion battery

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109037670A (en) * 2018-07-10 2018-12-18 湖南鸿捷新材料有限公司 A kind of method of continuity preparation little particle ternary precursor material
CN108963237A (en) * 2018-08-07 2018-12-07 河北工业大学 A kind of preparation method of anode material of lithium-ion battery
CN108963237B (en) * 2018-08-07 2021-03-16 河北工业大学 Preparation method of sodium ion battery negative electrode material
CN113023706A (en) * 2021-03-10 2021-06-25 陕西科技大学 Carbon-coated antimony selenide/graphene composite material and preparation method and application thereof
CN113023706B (en) * 2021-03-10 2022-10-14 陕西科技大学 Carbon-coated antimony selenide/graphene composite material and preparation method and application thereof

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