CN107482201A - A kind of SnSe/ carbon cloths flexibility negative material and preparation method thereof - Google Patents
A kind of SnSe/ carbon cloths flexibility negative material and preparation method thereof Download PDFInfo
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- CN107482201A CN107482201A CN201710697912.2A CN201710697912A CN107482201A CN 107482201 A CN107482201 A CN 107482201A CN 201710697912 A CN201710697912 A CN 201710697912A CN 107482201 A CN107482201 A CN 107482201A
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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
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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
- 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
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
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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
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- 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
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Abstract
The invention discloses a kind of SnSe/ carbon cloths flexibility negative material and preparation method thereof, belong to electrochemistry and new energy materialses field.The present invention prepares SnSe/ carbon cloth flexibility negative materials using straightforward procedure.Stannous oxide, citric acid are well mixed back loading to carbon cloth in deionized water with selenium powder, calcining obtains SnSe/ carbon cloth flexibility negative materials in atmosphere furnace after drying.SnSe is equably supported on carbon fiber surface, drastically increases the cyclical stability and electric transmission speed of material.SnSe has higher specific capacity, and flexible fiber carbon cloth improves the electric conductivity of material as matrix.The SnSe/ carbon fiber cloth electrodes material is, can be directly as flexible electrode material without using bonding agent as collector with good pliability, carbon fiber.SnSe/ carbon fiber cloth electrodes material shows higher specific capacity and excellent stable circulation performance as lithium ion battery negative material.
Description
Technical field
The invention discloses a kind of SnSe/ carbon cloths flexibility negative material and preparation method thereof, belong to electrochemistry and new
Field of energy source materials.
Background technology
Tin base cathode material is due to its higher theoretical capacity（990 mAh/g）, have become in field of lithium ion battery
Study hotspot.SnSe is a kind of IV-VI type compound semiconductor, and its structure is advantageous to strengthen between two and three dimensions
The transmission speed of lithium ion.Energy gap width relatively low SnSe（0.9 eV）Theoretical foundation is provided for its good electric conductivity, its
Huge potential is shown as lithium ion battery negative material.The SnSe/C that Zhang Zhi's peace et al. is prepared by ball-milling method is compound
Material shows excellent chemical property as lithium ion battery negative material, is circulated under 500 mA/g current density
Its reversible capacity still has 325 mAh/g after 200 circles（Electrochimica Acta, 2015, 9, 1296-1301）.These
Research further demonstrate application values of the SnSe as lithium ion battery negative material.CN105633483A patents disclose one
Kind SnSe/Graphene composite material preparation methods.Using water as solvent, SnCl2·2H2O is as raw material, oxidation
Graphene is as carbon base body, using the previously prepared SnO of hydro-thermal method2/ Graphene composites, then by SnO2/ Graphene is multiple
After condensation material and selenium powder ground and mixed are uniform, it is placed in vacuum tube furnace and in calcining, obtains the SnSe/Graphene of pure phase and answer
Condensation material, the material show preferable chemical property as anode material of lithium-ion battery.CN106744728A patents are public
The preparation method of SnSe micron balls has been opened, selenium powder has been dissolved in hydrazine hydrate, has then added SnCl2·2H2O, after stirring, drying
Obtain SnSe micron balls.
Carbon cloth has preferable electric conductivity and mechanics pliability, and SnSe active materials are supported on carbon fiber, can
To avoid the addition of binding agent, while carbon fiber can also provide portion capacity.Led with reference to SnSe high power capacity and carbon fiber height
The characteristics of electrical and stability, both combinations can be played into the advantage respectively as electrochemical material.The SnSe that the method is prepared
Carbon fiber surface is equably supported on, carbon fiber is crosslinked together to form stable three-dimensional conductive network, improves material
Cyclical stability and electric transmission speed.In addition, the electrode material is binder free, conductive agent self-supporting flexible electrode material,
The chemical property under the energy density and bending condition of material can further be improved.
To sum up analyze, with reference to both SnSe and flexible carbon fibre cloth advantage, the two is organically combined to be formed
SnSe/ carbon cloth flexible electrodes, the electrode material have higher potential using value as lithium ion battery negative material.
The content of the invention
It is an object of the invention to provide a kind of preparation method of SnSe/ carbon cloths flexibility negative material.This method is
Stannous oxide, selenium powder are well mixed back loading to carbon cloth in deionized water with citric acid, in atmosphere furnace after drying
Middle calcining obtains SnSe/ carbon cloth flexibility negative materials.
The object of the present invention is achieved like this：A kind of preparation method of SnSe/ carbon cloths flexibility negative material, it has
Body technology step is as follows：
（1）Be well mixed in deionized water using stannous oxide, selenium powder with citric acid as presoma, stannous oxide, selenium powder with
The mass ratio of citric acid is 1.2 ~ 2.0：1：2.5~13.5；
（2）Forerunner's liquid suspension is supported on carbon cloth, 50 DEG C of dry 5h；
（3）The carbon cloth for loading SnSe is calcined under argon/hydrogen protective atmosphere, it is 600-900 DEG C to burn temperature, and calcination time is
2-20h。
SnSe/ carbon cloths flexibility negative material provided by the invention, possesses following beneficial effect：
（1）SnSe/ carbon cloth flexibility negative material experimental procedures prepared by the method are simple, and SnSe/ is prepared by high-temperature calcination
Carbon cloth flexibility negative material；
（2）The electrode material can effectively improve the electric conductivity and cyclical stability of material using carbon cloth as matrix；
（3）Electrode material prepared by the method is the energy density that material can be improved without binding agent and conductive agent；
（4）Electrode material prepared by the method has good mechanics pliability.
The present invention prepares SnSe/ carbon cloth flexibility negative materials using a kind of straightforward procedure, and the electrode material has good
Good mechanics pliability, higher specific capacity and preferable stable circulation performance are shown as lithium ion battery negative material.
Stannous oxide, selenium powder are well mixed as forerunner by the present invention in deionized water using carbon cloth as matrix with citric acid
Body is loaded on carbon cloth, and calcining obtains SnSe/ carbon cloth flexibility negative materials in nitrogen atmosphere after drying.This
Kind method is there is not yet any document and patent report.
Brief description of the drawings
Fig. 1 is the photo of SnSe/ carbon cloth flexibility negative materials prepared by the embodiment of the present invention 1.
Fig. 2 is the X-ray diffraction of SnSe/ carbon cloth flexibility negative materials prepared by the embodiment of the present invention 1（XRD）Figure
Spectrum.
Fig. 3 is the stereoscan photograph (SEM) of SnSe/ carbon cloth flexibility negative materials prepared by the embodiment of the present invention 1,
Wherein a is the accompanying drawing of 500 multiplying powers of amplification, and b is the accompanying drawing of 2000 multiplying powers of amplification.
Fig. 4 is the 3 times charging and discharging curve of SnSe/ carbon cloth flexibility negative materials prepared by the embodiment of the present invention 1.
Fig. 5 is the stable circulation performance of SnSe/ carbon cloth flexibility negative materials prepared by the embodiment of the present invention 1.
Embodiment
With reference to instantiation, the present invention is further described.
Embodiment 1：SnSe/ carbon cloth flexibilities negative material I
By stannous oxide（0.27g）, Se powder（0.158g）, citric acid（1.68g）It is placed in 20mL deionized water solutions and stirs 20
Minute, it is then ultrasonic 20 minutes.By above-mentioned suspension coated on carbon cloth, it is placed in 50 DEG C of baking ovens and dries 5h.Then will
The carbon cloth for being loaded with presoma is placed in tube furnace under argon/nitrogen atmosphere and calcined, and calcining heat is 700 DEG C, calcination time
For 12h.Obtain SnSe/ carbon cloth flexibility negative materials.Fig. 1 is the SnSe/ carbon cloth flexibility negative materials prepared
Photo, from photo it can be seen that the material has good mechanics pliability.Fig. 2 is that the SnSe/ carbon cloths prepared are flexible negative
The XRD spectrum of pole material, it can be seen that the XRD diffraction maximums of prepared material and SnSe base peak fit like a glove, corresponding to card
Piece 14-0159, it was demonstrated that the material prepared by the method is SnSe.Do not occur the diffraction maximum of carbon in XRD spectrum, illustrate carbon fibre
Wei Bu is impalpable structure.Fig. 3 is the SEM photograph of the SnSe/ carbon cloth flexibility negative materials prepared, it can be seen that SnSe
Grain be evenly distributed on carbon fiber, carbon fiber is cross-linked forms three-dimensional conductive network together, be electronics transmission and
The diffusion of ion provides good passage.Prepared SnSe/ carbon cloths are shown as lithium ion battery negative material
Higher specific capacity and excellent stable circulation performance.By the electrode directly as working electrode, lithium piece is to electrode, electrolyte
For the general M LiPF of lithium-ion battery electrolytes 16/DMC: EC=1:1,2025 type button cells are prepared, with 100 mA g-1
Current density discharge and recharge.The 3 times charging and discharging curve of the electrode is as shown in Figure 4, it can be seen that the electric discharge first of the material is held
Measure as 1330 mAh g-1, reversible charging capacity is 983 mAh g first-1, second of reversible capacity is 809 mAh g-1.Follow
Ring stability is as shown in figure 5, in 100 mA g-1Under current density after 70 circulations, reversible capacity also has 658 mAh g-1, the electrode material shows higher capacity and preferable stable circulation performance.
The SnSe/ carbon cloth flexibilities negative material II of embodiment 2
By stannous oxide（0.27g）, Se powder（0.158g）, citric acid（1.26g）It is placed in 20mL deionized water solutions and stirs 20
Minute, it is then ultrasonic 20 minutes.By above-mentioned suspension coated on carbon cloth, it is placed in 50 DEG C of baking ovens and dries 5h.It is placed in 50
5h is dried in DEG C baking oven.Then the carbon cloth for being loaded with presoma is placed in tube furnace under argon/nitrogen atmosphere and calcined, is calcined
Temperature is 700 DEG C, calcination time 12h.SnSe/ carbon cloth flexibility negative materials are obtained after calcining.The electrode material is surveyed
Strip part as described in example 1 above, as lithium ion battery negative material, with 100 mA g-1Current density carries out discharge and recharge, first
Secondary reversible capacity is 1030 mAh g-1, the reversible capacity after 70 circulations is 630 mAh g-1。
The SnSe/ carbon cloth flexibilities negative material III of embodiment 3
By stannous oxide（0.27g）, Se powder（0.158g）, citric acid（2.1g）It is placed in 20mL deionized water solutions and stirs 20 points
Clock, it is then ultrasonic 20 minutes.By above-mentioned suspension coated on carbon cloth, it is placed in 50 DEG C of baking ovens and dries 5h.Then will be negative
The carbon cloth for being loaded with presoma is placed in tube furnace under argon/nitrogen atmosphere and calcined, and calcining heat is 700 DEG C, and calcination time is
12h.SnSe/ carbon cloth flexibility negative materials are obtained after calcining.The electrode material test condition as described in example 1 above,
As lithium ion battery negative material, with 100 mA g-1Current density carries out discharge and recharge, and reversible capacity is 920 mAh g first-1, the reversible capacity after 70 circulations is 560 mAh g-1。
The SnSe/ carbon cloth flexibilities negative material IV of embodiment 4
By stannous oxide（0.27g）, Se powder（0.158g）, citric acid（1.68g）It is placed in 20mL deionized water solutions and stirs 20
Minute, it is then ultrasonic 20 minutes.By above-mentioned suspension coated on carbon cloth, it is placed in 50 DEG C of baking ovens and dries 5h.Then will
The carbon cloth for being loaded with presoma is placed in tube furnace under argon/nitrogen atmosphere and calcined, and calcining heat is 600 DEG C, calcination time
For 12h.SnSe/ carbon cloth flexibility negative materials are obtained after calcining.Institute in the electrode material test condition such as embodiment 1
State, as lithium ion battery negative material, with 100 mA g-1Current density carries out discharge and recharge, and reversible capacity is 860 mAh first
g-1, the reversible capacity after 70 circulations is 530 mAh g-1。
The SnSe/ carbon cloth flexibilities negative material V of embodiment 5
By stannous oxide（0.27g）, Se powder（0.158g）, citric acid（1.68g）It is placed in 20mL deionized water solutions and stirs 20
Minute, it is then ultrasonic 20 minutes.By above-mentioned suspension coated on carbon cloth, it is placed in 50 DEG C of baking ovens and dries 5h.Then will
The carbon cloth for being loaded with presoma is placed in tube furnace under argon/nitrogen atmosphere and calcined, and calcining heat is 900 DEG C, calcination time
For 12h.SnSe/ carbon cloth flexibility negative materials are obtained after calcining.Institute in the electrode material test condition such as embodiment 1
State, as lithium ion battery negative material, with 100 mA g-1Current density carries out discharge and recharge, and reversible capacity is 1100 first
mAh g-1, the reversible capacity after 70 circulations is 609 mAh g-1。
Claims (4)
- A kind of 1. preparation method of SnSe/ carbon cloths flexibility negative material, it is characterised in that：By stannous oxide, selenium powder and lemon Lemon acid is loaded on carbon cloth after being well mixed in deionized water as presoma, and calcining obtains in atmosphere furnace after drying SnSe/ carbon cloth flexibility negative materials.
- 2. the preparation method of SnSe/ carbon cloths flexibility negative material as claimed in claim 1, it is characterised in that：Presoma The mass ratio of middle stannous oxide, selenium powder and citric acid is 1.2 ~ 2.0：1：2.5~13.5.
- 3. the preparation method of SnSe/ carbon cloths flexibility negative material as claimed in claim 1, it is characterised in that：SnSe with Carbon cloth mass ratio is 1: 2~ 10.
- 4. the preparation method of SnSe/ carbon cloths flexibility negative material as claimed in claim 1, it is characterised in that：It is loaded with The carbon cloth of presoma is calcined in a nitrogen atmosphere after drying, and calcining heat is 600 ~ 900 DEG C, and calcination time is 2 ~ 20h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110299512A (en) * | 2019-06-25 | 2019-10-01 | 西安交通大学 | A kind of preparation method of the lithium metal battery cathode of carbon/tin multiple base support |
| CN110767902A (en) * | 2019-10-14 | 2020-02-07 | 山东理工大学 | Preparation method of SnSe/graphene-coated cotton carbon fiber self-supporting material |
| CN113097486A (en) * | 2021-04-01 | 2021-07-09 | 陕西科技大学 | SnSe quantum dot/CFF compound and preparation method and application thereof |
| CN114583160A (en) * | 2022-03-09 | 2022-06-03 | 广东工业大学 | Tin selenide nanosheet array/carbon cloth composite cathode material structure for sodium ion battery |
| CN114665080A (en) * | 2022-04-18 | 2022-06-24 | 齐鲁工业大学 | SnSe2-NiSe2Negative electrode material of/CNT (carbon nanotube) sodium ion battery and preparation method thereof |
| CN114843464A (en) * | 2022-04-21 | 2022-08-02 | 陕西科技大学 | Three-dimensional cross-linked structure SnSe/3D r-GO composite material and preparation method and application thereof |
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| CN105633483A (en) * | 2016-03-29 | 2016-06-01 | 陕西科技大学 | Preparation method of SnSe/Graphene composite electrode material for negative electrode of sodium-ion battery |
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| CN105633483A (en) * | 2016-03-29 | 2016-06-01 | 陕西科技大学 | Preparation method of SnSe/Graphene composite electrode material for negative electrode of sodium-ion battery |
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Non-Patent Citations (2)
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| WANGWANG XU等: ""SnS2@Graphene nanosheet arrays grown on carbon cloth as freestanding binder-free flexible anodes for advanced sodium batteries"", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110299512A (en) * | 2019-06-25 | 2019-10-01 | 西安交通大学 | A kind of preparation method of the lithium metal battery cathode of carbon/tin multiple base support |
| CN110767902A (en) * | 2019-10-14 | 2020-02-07 | 山东理工大学 | Preparation method of SnSe/graphene-coated cotton carbon fiber self-supporting material |
| CN113097486A (en) * | 2021-04-01 | 2021-07-09 | 陕西科技大学 | SnSe quantum dot/CFF compound and preparation method and application thereof |
| CN114583160A (en) * | 2022-03-09 | 2022-06-03 | 广东工业大学 | Tin selenide nanosheet array/carbon cloth composite cathode material structure for sodium ion battery |
| CN114583160B (en) * | 2022-03-09 | 2024-04-26 | 广东工业大学 | Tin selenide nano-sheet array/carbon cloth composite anode material structure for sodium ion battery |
| CN114665080A (en) * | 2022-04-18 | 2022-06-24 | 齐鲁工业大学 | SnSe2-NiSe2Negative electrode material of/CNT (carbon nanotube) sodium ion battery and preparation method thereof |
| CN114843464A (en) * | 2022-04-21 | 2022-08-02 | 陕西科技大学 | Three-dimensional cross-linked structure SnSe/3D r-GO composite material and preparation method and application thereof |
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