CN107934923A - A kind of nanometer sheet self assembly flower ball-shaped Sb2Se3The preparation method of anode material of lithium-ion battery - Google Patents
A kind of nanometer sheet self assembly flower ball-shaped Sb2Se3The preparation method of anode material of lithium-ion battery Download PDFInfo
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- CN107934923A CN107934923A CN201711085729.3A CN201711085729A CN107934923A CN 107934923 A CN107934923 A CN 107934923A CN 201711085729 A CN201711085729 A CN 201711085729A CN 107934923 A CN107934923 A CN 107934923A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- 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
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- C01P2004/32—Spheres
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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
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- H—ELECTRICITY
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- H01M4/00—Electrodes
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- 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
A kind of nanometer sheet self assembly flower ball-shaped Sb2Se3The preparation method of anode material of lithium-ion battery, the present invention reduce production cost using the common cheap thing such as antimony trichloride, selenium powder, sodium borohydride and ethanol as raw material；The characteristics of product structure easy to control using solvent thermal environment, successfully prepare nanometer sheet self assembly single dispersing flower ball-shaped pure phase Sb under the action of polyvinylpyrrolidone2Se3It is nanocrystalline, and reaction temperature is relatively low, it is reproducible, meet that large-scale production requires.Finally, by prepared Sb2Se3A series of processes such as nanocrystalline ground, slurrying, coating, drying, are assembled into button-shaped sodium-ion battery, carry out Primary Study to its electrochemical behavior as anode material of lithium-ion battery, find the nanometer sheet self assembly flower ball-shaped Sb prepared by the present invention2Se3Discharge capacity is 780mA h g to anode material of lithium-ion battery first‑1, higher than theoretical capacity, the circle capacity of circulation 50 is maintained at 300mA h g‑1, there is good cyclical stability, while high rate performance is also preferable.
Description
Technical field
The invention belongs to electrochemical energy storage field, and in particular to a kind of nanometer sheet self assembly flower ball-shaped Sb2Se3Sodium ion electricity
The preparation method of pond negative material.
Background technology
Electrochemical energy storage is one of major way of today's society energy storage, and electrochemical energy storage mainly has solar-electricity
Pond, lead accumulator, lithium ion battery and sodium-ion battery etc..Wherein, there is storage capacity to enrich, pollute less, compare for sodium-ion battery
Energy is big, the advantages that having extended cycle life, and is one of the research hotspot in current electrochemical energy storage field.Antimony base selenides Sb2Se3Make
For anode material of lithium-ion battery, its typical layer structure is conducive to Na+Transmission, and 1moL Sb2Se3Can be with
The Na of 12moL+Reaction, so as to result in high theoretical capacity 670mA h g-1, causes the extensive concern of numerous researchers.
According to the literature, currently as anode material of lithium-ion battery Sb2Se3 mainly based on one-dimentional structure.Such as,
Xing Qu et al. synthesize nano bar-shape Sb2Se3/rGO composite materials using the method for solvent heat, in the electric current of 1.0A g-1
Under density, capacity is maintained at 471mA h g-1 (Ou X, Yang C, Xiong X, et al.A New after circulating 500 times
rGO‐Overcoated Sb2Se3Nanorods Anode for Na+Battery:In Situ X‐Ray Diffraction
Study on a Live Sodiation/Desodiation Process[J].Advanced Functional
Materials,2017.).It is compound to prepare nano bar-shape Sb2Se3/N-GO using the method for " treating different things alike " by Wenxi Zhao etc.
Material, under the current density of 0.1A g-1, discharge capacity is 1000mA h g-1 first, and capacity is maintained at after circulating 50 times
560mA h g-1(Zhao W,Li C M.Mesh-structured N-doped graphene@Sb2Se3hybrids as
an anode for large capacity sodium-ion batteries.[J].Journal of Colloid&
Interface Science,2016,488:356-364).One-dimensional Sb2Se3 nano materials are prepared into film by Luo W etc., and
As anode material of lithium-ion battery, under the current density in 0.1A g-1, capacity stabilization is in 300mA after the circle of circulation 50
h g-1。(Luo W,Calas A,Tang C,et al.Ultralong Sb2Se3Nanowire-Based Free-
Standing Membrane Anode for Lithium/Sodium Ion Batteries[J].2016).For other shapes
Looks Sb2Se3 nano materials are less as the report of sodium-ion battery anode, hinder numerous researchers to different-shape Sb2Se3
Research as anode material of lithium-ion battery electrochemical behavior.
The content of the invention
It is an object of the invention to provide a kind of nanometer sheet self assembly flower ball-shaped Sb2Se3The system of anode material of lithium-ion battery
Preparation Method, prepared Sb2Se3Nano material not only has the flower ball-shaped special construction being self-assembly of by thin slice, but also conduct
Anode material of lithium-ion battery has high charge/discharge capacity, good cyclical stability and excellent high rate performance.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
1) antimony trichloride of the polyvinylpyrrolidone of 0.005~0.05g and 0.5~2mmol is added to 35~75ml
Ethanol in, stirring obtains clear solution A, take 0.75~3mmol selenium powder add the concentration of 2-15ml for 0.075~
In 0.9moL/L sodium borohydride aqueous solutions, stirring obtains clear solution B, solution B is added dropwise in solution A stirs under agitation
Mix and black mixed liquor C is obtained after being uniformly dispersed；
2) mixed liquor C is transferred to polytetrafluoroethyllining lining, is put into homogeneous reaction instrument, at 150~200 DEG C, reaction 18~
After 30h, room temperature is cooled to the furnace, wash precipitation and separation repeatedly with deionized water and absolute ethyl alcohol, gained black gray expandable powder is
Nanometer sheet self assembly flower ball-shaped Sb2Se3Anode material of lithium-ion battery.
Polyvinylpyrrolidone average molecular weight 30000 in the step 1).
Stirring use magnetic stirring apparatus in the step 1), and speed of agitator is 500~800r/min, and mixing time is 10~
60min。
The packing ratio that step 2) the mixed liquor C is transferred to polytetrafluoroethyllining lining is 50%~80%.
Step 2) the freeze-drying temperature is -40 DEG C, pressure 60Pa.
Relative to the prior art, first, the present invention is common with antimony trichloride, selenium powder, sodium borohydride and ethanol etc. by the present invention
Cheap thing reduces production cost as raw material；Further, the characteristics of product structure easy to control using solvent thermal environment, poly-
Nanometer sheet self assembly single dispersing flower ball-shaped pure phase Sb is successfully prepared under the action of vinylpyrrolidone2Se3It is nanocrystalline, nanometer sheet
Thickness is about 10nm, and bouquet diameter is about 1 μm, and reaction temperature is relatively low, reproducible, meets that large-scale production requires.Most
Afterwards, by prepared Sb2Se3A series of processes such as nanocrystalline ground, slurrying, coating, drying, are assembled into button-shaped sodium ion
Battery, carries out Primary Study to its electrochemical behavior as anode material of lithium-ion battery, finds receiving prepared by the present invention
Rice piece self assembly flower ball-shaped Sb2Se3Discharge capacity is 780mA h g to anode material of lithium-ion battery first-1, hold higher than theory
Amount, the circle capacity of circulation 50 are maintained at 300mA h g-1, there is good cyclical stability, while high rate performance is also preferable.
Brief description of the drawings
Fig. 1 is Sb prepared by the embodiment of the present invention 12Se3X-ray diffraction (XRD) collection of illustrative plates of electrode material；
Fig. 2 is Sb prepared by the embodiment of the present invention 12Se3Scanning electron microscope (SEM) photo of electrode material；
Fig. 3 is Sb prepared by the embodiment of the present invention 12Se3The cycle performance figure of electrode material；Wherein, Cycle number：
Cycle-index；Capacity：Capacity；
Fig. 4 is Sb prepared by the embodiment of the present invention 62Se3X-ray diffraction (XRD) collection of illustrative plates of electrode material；
Fig. 5 is Sb prepared by the embodiment of the present invention 62Se3Scanning electron microscope (SEM) photo of electrode material；
Fig. 6 is Sb prepared by the embodiment of the present invention 62Se3The high rate performance figure of electrode material；Wherein, Cycle number：
Cycle-index；Capacity：Capacity
Embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1：
1) antimony trichloride of the polyvinylpyrrolidone of 0.005g and 0.5mmol is added in the ethanol of 35ml, stirred
Clear solution A is obtained, the concentration for taking the selenium powder addition 15ml of 0.75mmol is stirring in 0.075moL/L sodium borohydride aqueous solutions
Clear solution B is obtained, solution B is added dropwise in solution A under agitation after being dispersed with stirring uniformly and obtains black mixed liquor C；
Stirring uses magnetic stirring apparatus, speed of agitator 500r/min, mixing time 60min above；
2) mixed liquor C is transferred to polytetrafluoroethyllining lining by 50% packing ratio, is put into homogeneous reaction instrument, at 150 DEG C,
After reacting 30h, cool to room temperature with the furnace, precipitation and separation is washed repeatedly with deionized water and absolute ethyl alcohol, under -40 DEG C, 60Pa
Be freeze-dried black gray expandable powder is nanometer sheet self assembly flower ball-shaped Sb2Se3Anode material of lithium-ion battery.
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 Cheng nanometer sheet self assembly single dispersing flower ball-shapeds, nanometer sheet thickness are about 10nm, and bouquet diameter is about 1 μm (Fig. 2).
Using above-mentioned black gray expandable powder as active material, with conductive agent Super-p, I CMC of binding agent hydroxymethyl cellulose,
Polyacrylic acid PAA presses 7:2:0.5:0.5 mass ratio is made after grinding, slurry coating, drying, section in deionized water
Button-shaped sodium-ion battery is assembled into the glove box full of argon gas for anode, after shelving 48h, is carried out using blue electric tester
Electrochemical property test.In 0.1A g-1Current density under, discharge capacity is 780mA h g first-1, higher than theoretical capacity,
The circle capacity of circulation 50 is maintained at 300mA h g-1, there is good cyclical stability (Fig. 3).
Embodiment 2：
1) antimony trichloride of the polyvinylpyrrolidone of 0.01g and 0.75mmol is added in the ethanol of 42ml, stirred
Clear solution A is obtained, the concentration for taking the selenium powder addition 13ml of 1.125mmol is in 0.129moL/L sodium borohydride aqueous solutions, is stirred
Mix to obtain clear solution B, solution B is added dropwise in solution A under agitation after being dispersed with stirring uniformly and obtains black mixed liquor
C；
Stirring uses magnetic stirring apparatus, speed of agitator 800r/min, mixing time 10min above；
2) mixed liquor C is transferred to polytetrafluoroethyllining lining by 55% packing ratio, is put into homogeneous reaction instrument, at 160 DEG C,
After reacting 28h, cool to room temperature with the furnace, precipitation and separation is washed repeatedly with deionized water and absolute ethyl alcohol, under -40 DEG C, 60Pa
Be freeze-dried black gray expandable powder is nanometer sheet self assembly flower ball-shaped Sb2Se3Anode material of lithium-ion battery.
Embodiment 3：
1) antimony trichloride of the polyvinylpyrrolidone of 0.02g and 1mmol is added in the ethanol of 49ml, stirring obtains
Clear solution A, takes the selenium powder of 1.5mmol to add the concentration of 11ml as in 0.204moL/L sodium borohydride aqueous solutions, stirring obtains
Solution B, is added dropwise in solution A after being dispersed with stirring uniformly and obtains black mixed liquor C by clear solution B under agitation；
Stirring uses magnetic stirring apparatus, speed of agitator 600r/min, mixing time 40min above；
2) mixed liquor C is transferred to polytetrafluoroethyllining lining by 60% packing ratio, is put into homogeneous reaction instrument, at 170 DEG C,
After reacting 24h, cool to room temperature with the furnace, precipitation and separation is washed repeatedly with deionized water and absolute ethyl alcohol, under -40 DEG C, 60Pa
Be freeze-dried black gray expandable powder is nanometer sheet self assembly flower ball-shaped Sb2Se3Anode material of lithium-ion battery.
Embodiment 4：
1) antimony trichloride of the polyvinylpyrrolidone of 0.03g and 1.25mmol is added in the ethanol of 56ml, stirred
Clear solution A is obtained, the concentration for taking the selenium powder addition 9ml of 1.875mmol is stirring in 0.312moL/L sodium borohydride aqueous solutions
Clear solution B is obtained, solution B is added dropwise in solution A under agitation after being dispersed with stirring uniformly and obtains black mixed liquor C；
Stirring uses magnetic stirring apparatus, speed of agitator 700r/min, mixing time 30min above；
2) mixed liquor C is transferred to polytetrafluoroethyllining lining by 65% packing ratio, is put into homogeneous reaction instrument, at 180 DEG C,
After reacting 22h, cool to room temperature with the furnace, precipitation and separation is washed repeatedly with deionized water and absolute ethyl alcohol, under -40 DEG C, 60Pa
Be freeze-dried black gray expandable powder is nanometer sheet self assembly flower ball-shaped Sb2Se3Anode material of lithium-ion battery.
Embodiment 5：
1) antimony trichloride of the polyvinylpyrrolidone of 0.04g and 1.5mmol is added in the ethanol of 63ml, stirred
To clear solution A, the selenium powder of 2.25mmol is taken to add the concentration of 7ml as in 0.48moL/L sodium borohydride aqueous solutions, stirring obtains
Solution B, is added dropwise in solution A after being dispersed with stirring uniformly and obtains black mixed liquor C by clear solution B under agitation；
Stirring uses magnetic stirring apparatus, speed of agitator 650r/min, mixing time 50min above；
2) mixed liquor C is transferred to polytetrafluoroethyllining lining by 70% packing ratio, is put into homogeneous reaction instrument, at 190 DEG C,
After reacting 320h, cool to room temperature with the furnace, precipitation and separation is washed repeatedly with deionized water and absolute ethyl alcohol, under -40 DEG C, 60Pa
Be freeze-dried black gray expandable powder is nanometer sheet self assembly flower ball-shaped Sb2Se3Anode material of lithium-ion battery.
Embodiment 6：
1) antimony trichloride of the polyvinylpyrrolidone of 0.05g and 2mmol is added in the ethanol of 75ml, stirring obtains
Clear solution A, takes the selenium powder of 3mmol to add the concentration of 5ml as in 0.9moL/L sodium borohydride aqueous solutions, stirring obtains transparent molten
Solution B, is added dropwise in solution A after being dispersed with stirring uniformly and obtains black mixed liquor C by liquid B under agitation；
Stirring uses magnetic stirring apparatus, speed of agitator 750r/min, mixing time 20min above；
2) mixed liquor C is transferred to polytetrafluoroethyllining lining by 80% packing ratio, is put into homogeneous reaction instrument, at 200 DEG C,
After reacting 18h, cool to room temperature with the furnace, precipitation and separation is washed repeatedly with deionized water and absolute ethyl alcohol, under -40 DEG C, 60Pa
Be freeze-dried black gray expandable powder is nanometer sheet self assembly flower ball-shaped Sb2Se3Anode material of lithium-ion battery.
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. 4) 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 is nanometer sheet self assembly single dispersing flower ball-shaped, and nanometer sheet diameter is about 10nm, and bouquet diameter is about 1 μm (Fig. 5).
Using above-mentioned black gray expandable powder as active material, with conductive agent Super-p, I CMC of binding agent hydroxymethyl cellulose,
Polyacrylic acid PAA presses 7:2:0.5:0.5 mass ratio is made after grinding, slurry coating, drying, section in deionized water
Button-shaped sodium-ion battery is assembled into the glove box full of argon gas for anode, after shelving 48h, is carried out using blue electric tester
Electrochemical property test.In 0.1A g-1Current density under, discharge capacity is 767mA h g first-1, higher than theoretical capacity,
High rate performance is also preferable (Fig. 6) at the same time.
Claims (5)
- A kind of 1. nanometer sheet self assembly flower ball-shaped Sb2Se3The preparation method of anode material of lithium-ion battery, it is characterised in that：1) antimony trichloride of the polyvinylpyrrolidone of 0.005~0.05g and 0.5~2mmol is added to the second of 35~75ml In alcohol, stirring obtains clear solution A, and the concentration for taking the selenium powder addition 2-15ml of 0.75~3mmol is 0.075~0.9moL/L boron In sodium hydride aqueous solution, stirring obtains clear solution B, solution B is added dropwise in solution A is dispersed with stirring uniformly under agitation After obtain black mixed liquor C；2) mixed liquor C is transferred to polytetrafluoroethyllining lining, is put into homogeneous reaction instrument, at 150~200 DEG C, react 18~30h Afterwards, cool to room temperature with the furnace, wash precipitation and separation repeatedly with deionized water and absolute ethyl alcohol, gained black gray expandable powder is nanometer Piece self assembly flower ball-shaped Sb2Se3Anode material of lithium-ion battery.
- 2. nanometer sheet self assembly flower ball-shaped Sb according to claim 12Se3The preparation method of anode material of lithium-ion battery, It is characterized in that：Polyvinylpyrrolidone average molecular weight 30000 in the step 1).
- 3. nanometer sheet self assembly flower ball-shaped Sb according to claim 12Se3The preparation method of anode material of lithium-ion battery, It is characterized in that：Stirring uses magnetic stirring apparatus in the step 1), and speed of agitator is 500~800r/min, and mixing time is 10~60min.
- 4. nanometer sheet self assembly flower ball-shaped Sb according to claim 12Se3The preparation method of anode material of lithium-ion battery, It is characterized in that：The packing ratio that step 2) the mixed liquor C is transferred to polytetrafluoroethyllining lining is 50%~80%.
- 5. nanometer sheet self assembly flower ball-shaped Sb according to claim 12Se3The preparation method of anode material of lithium-ion battery, It is characterized in that：Step 2) the freeze-drying temperature is -40 DEG C, pressure 60Pa.
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Cited By (4)
| 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 |
| CN110042506A (en) * | 2019-04-30 | 2019-07-23 | 湘潭大学 | A kind of flexibility Sb2Se3The electrostatic spinning preparation method of/C nano fiber |
| CN113263184A (en) * | 2021-04-13 | 2021-08-17 | 上海大学 | Selenium-doped nano antimony, preparation method and application thereof |
| CN114188506A (en) * | 2021-12-01 | 2022-03-15 | 合肥国轩高科动力能源有限公司 | Modified NCM622 lithium ion battery anode material and preparation and application thereof |
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| CN102328960A (en) * | 2011-09-02 | 2012-01-25 | 上海大学 | Synthesis method of trimanganese tetroxide material with 3D (three-dimensional) flower-shaped structure |
| CN106848386A (en) * | 2017-01-23 | 2017-06-13 | 陕西科技大学 | A kind of sodium-ion battery negative pole nest like Sb2Se3The preparation method of electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| CN110042506A (en) * | 2019-04-30 | 2019-07-23 | 湘潭大学 | A kind of flexibility Sb2Se3The electrostatic spinning preparation method of/C nano fiber |
| CN113263184A (en) * | 2021-04-13 | 2021-08-17 | 上海大学 | Selenium-doped nano antimony, preparation method and application thereof |
| CN114188506A (en) * | 2021-12-01 | 2022-03-15 | 合肥国轩高科动力能源有限公司 | Modified NCM622 lithium ion battery anode material and preparation and application thereof |
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| CN107934923B (en) | 2020-05-12 |
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