CN110190268A - A kind of SnSe2The preparation method of/CNTs composite lithium ion battery material - Google Patents
A kind of SnSe2The preparation method of/CNTs composite lithium ion battery material Download PDFInfo
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- CN110190268A CN110190268A CN201910547563.5A CN201910547563A CN110190268A CN 110190268 A CN110190268 A CN 110190268A CN 201910547563 A CN201910547563 A CN 201910547563A CN 110190268 A CN110190268 A CN 110190268A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
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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
- H01M4/362—Composites
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/387—Tin or alloys based on tin
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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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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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- 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 present invention discloses a kind of hydro-thermal method preparation SnSe2The method of/carbon nanotube composite lithium ion battery material, comprising: weigh a certain amount of SnCl2And SeO2；It is put into hydro-thermal reaction axe liner；Carbon nanotube is weighed to put into liner；Deionized water is added into liner, liner is put into reaction kettle after subsequent magnetic agitation and is sealed；Reaction kettle is put into drying box and carries out hydro-thermal reaction；Reaction product deionized water and dehydrated alcohol eccentric cleaning are dried afterwards several times after the reaction was completed.Operation of the present invention is simple, does not need complex device, synthesized nanoscale SnSe2/ CNTs composite material is applied to carry out electrochemical property test in lithium-ion battery system as negative electrode material, and in the electro-chemical test that current density is 0.1 C, the specific discharge capacity of preceding charge and discharge cycles three times is respectively 803.7 mAh g‑1, 521.3 mAh g‑1, 454.7 mAh g‑1, specific discharge capacity is 210.3 mAh g after 100 circulations‑1, in addition, charge and discharge discharge capacity remains to be maintained at 176.5 mAh g under the high current density of 0.5 C‑1。
Description
Technical field
The present invention relates to the stannides of lithium ion battery electrode material preparation more particularly to microcosmic nanostructure to adulterate carbon materials
Expect the electrode material field of lithium ion battery.
Background technique
Development cleaning and renewable energy are the Major Strategics of Chinese society economic development.In each layer of new energy technology
In secondary, electrochemical energy storage has the hot issue of extremely important status and contemporary scientific research.Lithium ion battery is because having
Many advantages, such as energy density is high, have extended cycle life, memory-less effect, it has also become the secondary electricity that the world today is most widely used
Pond.Lithium ion battery negative material as lithium ion battery energy is improved and an important factor for cycle life, in the nature of things at
For the emphasis of people's research.In recent years, with deepening continuously to Nanoalloy investigation of materials, Nanoalloy material is in lithium
Application in ion battery becomes noticeable research hotspot and achieves greater advance.Tin base alloy anode is as therein
Important a member has the features such as high-energy-density, high magnification, high safety performance, to also obtain in-depth study.
SnSe2As the important negative electrode material of lithium ion battery, 813 mAh g can be provided-1High theoretical specific capacity (base
In 426 mAh g of alloying reaction-1With 387 mAh g of conversion reaction-1), theoretical maximum is striven in spite of some documents
By: in view of inactive Li2Se, reversible memory capacity are 426 mAh g-1It irreversibly develops.With the present marketization
Carbon material lithium ion battery negative material, SnSe2There is some superiority on theoretical capacity.In addition, SnSe2Biggish interlayer
Away from will enable more lithium ions to be embedded in, and alleviate large volume variation during conversion and deintercalation.But SnSe2Make
For important a member of tin-based material, following problems are equally existed: SnSe2Biggish volume can be still generated in the reaction of embedding de- lithium
Expansion loses electrical contact inside active material, leads to SnSe as electrode material dusting easy to crack2Chemical property deteriorates.Benefit
With the volume expansion of the high resiliency buffering alloy lithiumation stone of carbon material, the electrical contact of alloying pellet is improved, is lithium ion and electronics
Diffusion admittance is provided, SnSe is prepared2Carbon composite can effectively solve SnSe2As existing for lithium ion battery electrode material
The above problem.
Carbon nanotube be as single-layer or multi-layer graphite flake around central axis by it is seamless made of certain helical angle winding, in
Empty " micro-pipe ", every layer of hexagon constituted after being bonded completely by sp2 hydridization with 3 carbon atoms of surrounding by a carbon atom
The cylindrical surface of composition.The special construction of carbon nanotube makes it be likely to become a kind of excellent lithium ion battery energy storage material.It is big
Interlamellar spacing make lithium ion be easier to be embedded in abjection, tubular structure will not collapse after multiple charge and discharge cycles, can mention significantly
The performance of high-lithium ion battery and service life.
Prepare SnSe2/ CNTs composite material, can effectively solve SnSe2As existing for lithium ion battery electrode material embedding
Biggish volume expansion can be still led to the problem of when de- lithium reaction.In the present invention, using a kind of common preparation method hydro-thermal method,
SnSe is realized by controlling its reaction temperature and reaction time2The successful preparation of/CNTs nanocomposite.And by SnSe2/
CNTs nanocomposite carries out electrochemical property test as lithium ion battery negative material, finds synthesized composite material
Specific discharge capacity with higher, good high rate performance and stable circulation performance.
Summary of the invention
Tin-based material is lithium ion battery electrode material a kind of very excellent and with good development prospect, wherein
SnSe2As important a member of tin-based material, equally there is very excellent lithium ion battery chemical property.The present invention is to lithium
The exploration for the negative electrode material that ion battery is had excellent performance, it is intended to it is designed by reasonable material microstructure, it is this using hydro-thermal method
The most common preparation method in easy to operate, inexpensive and laboratory is realized to SnSe2The system of/CNTs nanocomposite powder
It is standby, by SnSe2/ CNTs nanocomposite carries out electrochemical property test as lithium ion battery negative material.The present invention is special
The main purpose of benefit is, using the doping of carbon nanotube, effectively solution SnSe2As existing for lithium ion battery electrode material
Embedding de- lithium leads to the problem of biggish volume expansion when reacting, it is de- that the big interlamellar spacing of carbon nanotube itself makes lithium ion be easier insertion
Out, tubular structure will not collapse after multiple charge and discharge cycles, can greatly improve performance and the service life of lithium ion battery.
SnSe2/ CNTs nanocomposite specific discharge capacity with higher, good high rate performance and stable circulation performance etc. are electrochemical
Learn performance.
The present invention provides preparation SnSe2Method of/CNTs the nanocomposite as lithium ion battery electrode material.This
Invention realizes SnSe by control hydrothermal temperature and reaction time2The successful preparation of/CNTs nanocomposite utilizes
The volume expansion of the high resiliency buffering alloy lithiumation stone of carbon nanotube, improves the electrical contact of alloying pellet, is lithium ion and electronics
Diffusion admittance is provided, so that SnSe2/ CNTs composite material has excellent lithium ion battery chemical property.
SnSe prepared by the present invention2/ CNTs nanocomposite is used as lithium ion battery electrode material, in electric current
Density is in the electro-chemical test of 0.1 C, and the specific discharge capacity of preceding charge and discharge cycles three times is respectively 803.7 mAh g-1,
521.3 mAh g-1, 454.7 mAh g-1, specific discharge capacity is 210.3 mAh g after 100 circulations-1, in addition, 0.5
Charge and discharge discharge capacity remains to be maintained at 176.5 mAh g under the high current density of C-1。
The present invention provides preparation SnSe2The hydrothermal method of/CNTs nano composite lithium ion cell electrode material, including such as
Lower step:
1) a certain amount of SnCl is weighed according to molar ratio2And SeO2；
2) two kinds of reaction raw materials are put into clean water thermal response axe liner；
3) according to certain mass ratio (SnCl2: carbon nanotube) a certain amount of carbon nanotube is weighed, equally put into liner；
4) a certain amount of deionized water is added into liner, subsequent magnetic agitation after a certain period of time puts into liner close in reaction kettle
Envelope；
5) reaction kettle is put into setting certain temperature, time response in drying box；
6) reaction product deionized water and dehydrated alcohol alternating centrifugal are cleaned after the reaction was completed and dries a timing afterwards several times
Between；
Further, SnCl in the step 1)2With SeO2Molar ratio be 1:2.
Further, SnCl in the step 3)2Mass ratio with carbon nanotube is 10:1.
Further, the loading of deionized water is preferably 80% in the liner in the step 4).
Further, the magnetic agitation time in the step 4) is suitable for for 30 min.
Further, drying box temperature is 160~200 DEG C in the step 5), and soaking time is 24 h, and cold with furnace
But to room temperature.
Further, the alternating centrifugal in the step 6) cleans 3 times.
Further, drying temperature is 80 DEG C after being centrifuged in the step 6), and drying time is 12 h.
Further, the SnSe that the present invention synthesizes2/ CNTs nanocomposite applications are in lithium ion battery, carbon nanometer
The doping of pipe can effectively solve SnSe2It is larger as can still be generated existing for lithium ion battery electrode material when embedding de- lithium reacts
Volume expansion problem, the big interlamellar spacing of carbon nanotube itself makes lithium ion be easier to be embedded in abjection, and tubular structure repeatedly filling
It will not be collapsed after discharge cycles, performance and the service life of lithium ion battery can be greatly improved.SnSe2/ CNTs nanocomposite
Preparation can reach and effectively improve SnSe2The electric discharge specific capacitance of electrode material and the effect of cyclical stability.
Beneficial achievement of the invention is:
1) the present invention is directed to be designed by reasonable material microstructure, by easy to operate, inexpensive experimental method hydro-thermal method
Success prepares SnSe2/ CNTs nanocomposite is as lithium ion battery electrode material.The present invention is by controlling its reaction temperature
SnSe is realized with the reaction time2The successful preparation of/CNTs nanocomposite, it is slow using the high resiliency of carbon nanotube graphene
The volume expansion of alloy lithiumation stone is rushed, the doping of carbon nanotube can effectively solve SnSe2It is deposited as lithium ion battery electrode material
In the reaction of embedding de- lithium when can still lead to the problem of biggish volume expansion, and the big interlamellar spacing of carbon nanotube makes lithium ion more
It is easy insertion abjection, tubular structure will not collapse after multiple charge and discharge cycles, so that SnSe2/ CNTs composite material tool
There is excellent lithium ion battery chemical property.
2) SnSe prepared by the present invention2/ CNTs nanocomposite as negative electrode material be applied to lithium ion battery in into
Row electro-chemical test shows very excellent chemical property, current density be 0.1 C electro-chemical test in, it is preceding three times
The specific discharge capacity of charge and discharge cycles is respectively 803.7 mAh g-1, 521.3 mAh g-1, 454.7 mAh g-1, by 100 times
Specific discharge capacity is 210.3 mAh g after circulation-1, in addition, charge and discharge discharge capacity remains to protect under the high current density of 0.5 C
It holds in 176.5 mAh g-1.SnSe prepared by the present invention2/ CNTs nanocomposite specific discharge capacity with higher, it is excellent
Electrochemistry high rate performance and stable circulation performance, can expand significantly electrochemical lithium ion battery electrode material preparation method and
Application field.
3) experimental implementation of the present invention is very simple, does not need any complex device, it can be achieved that SnSe2/ CNTs nanometers multiple
The preparation of condensation material powder, and be applied to progress electro-chemical test in lithium ion battery as negative electrode material and show very
Excellent chemical property.
Detailed description of the invention
Fig. 1 is SnSe made from embodiment 12Low power scanning electron microscope (SEM) figure of/CNTs lithium ion battery electrode material.
Fig. 2 is SnSe made from embodiment 12High power scanning electron microscope (SEM) figure of/CNTs lithium ion battery electrode material.
Fig. 3 is SnSe made from embodiment 12Cycle life curve figure under/CNTs lithium ion battery different multiplying.
Fig. 4 is SnSe made from embodiment 12/ CNTs cycle life of lithium ion battery curve graph.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
According to molar ratio (Sn:Se=1:2), a certain amount of SnCl is weighed2And SeO2, two kinds of reaction raw materials are put into 50 ml hydro-thermals
In reaction kettle liner, liner utilizes deionized water and washes of absolute alcohol clean in advance.According to certain mass ratio (SnCl2:
CNTs=10:1) a certain amount of carbon nanotube is weighed, equally put into liner.A certain amount of deionized water is added into liner, guarantees
Loading is 80%, will be sealed in liner threading reaction kettle after then carrying out 30 min magnetic agitations.Reaction kettle is put into constant temperature to do
Cooled to room temperature after 180 DEG C of 24 h of reaction in dry case.By resulting product deionized water and dehydrated alcohol alternately from
12 h are dried in 80 DEG C of insulating box after heart cleaning three times.
Embodiment 2
According to molar ratio (Sn:Se=1:2), a certain amount of SnCl is weighed2And SeO2, two kinds of reaction raw materials are put into 50 ml hydro-thermals
In reaction kettle liner, liner utilizes deionized water and washes of absolute alcohol clean in advance.According to certain mass ratio (SnCl2:
CNTs=10:1) a certain amount of carbon nanotube is weighed, equally put into liner.A certain amount of deionized water is added into liner, guarantees
Loading is 80%, will be sealed in liner threading reaction kettle after then carrying out 30 min magnetic agitations.Reaction kettle is put into constant temperature to do
Cooled to room temperature after 160 DEG C of 24 h of reaction in dry case.By resulting product deionized water and dehydrated alcohol alternately from
12 h are dried in 80 DEG C of insulating box after heart cleaning three times.
Embodiment 3
According to molar ratio (Sn:Se=1:2), a certain amount of SnCl is weighed2And SeO2, two kinds of reaction raw materials are put into 50 ml hydro-thermals
In reaction kettle liner, liner utilizes deionized water and washes of absolute alcohol clean in advance.According to certain mass ratio (SnCl2:
CNTs=10:1) a certain amount of carbon nanotube is weighed, equally put into liner.A certain amount of deionized water is added into liner, guarantees
Loading is 80%, will be sealed in liner threading reaction kettle after then carrying out 30 min magnetic agitations.Reaction kettle is put into constant temperature to do
Cooled to room temperature after 200 DEG C of 24 h of reaction in dry case.By resulting product deionized water and dehydrated alcohol alternately from
12 h are dried in 80 DEG C of insulating box after heart cleaning three times.
Chemical raw material SnCl used in above embodiments2, SeO2And carbon nanotube is that analysis is pure.
Performance test:
1) SEM is tested: by the final SnSe obtained of the various embodiments described above2/ CNTs nanocomposite is swept in low power and high power SEM
It retouches and is observed under Electronic Speculum.It is as shown in Figure 1, Figure 2 respectively SnSe made from embodiment 12The low power and height of/CNTs nanocomposite
Times scanning electron microscope (SEM) photograph, it is apparent that SnSe from Fig. 1,22In regular hexagon lamellar, thickness is between 10-50nm
Typical two-dimensional nanostructure material.And carbon nano tube structure is apparent that from partial enlargement Fig. 2, it is carbon nano tube-doped
In monolithic stratiform SnSe2Between, well and SnSe2In conjunction with each self-growing SnSe originally2Piece is combined into an entirety, this
Sample can be substantially reduced SnSe during carrying out electrochemistry cycle charge-discharge2Structure, which is seriously damaged even, there is local take off
It falls situation and reduces the cycle performance of battery.
2) the cycle life test under different multiplying: by the last SnSe obtained of the various embodiments described above2/ CNTs is nano combined
Material is made electrode slice and is assembled into lithium ion battery progress constant current charge-discharge test.If Fig. 3 is SnSe made from embodiment 12/
CNTs nanocomposite 0.1 C, 0.2 C, 0.3 C, 0.4 C, 0.5 C, 0.1 C different multiplying under cycle charge-discharge
Curve, it can be seen that SnSe2/CNTs nanometer combined electrode material presents excellent high rate performance.
3) cycle life is tested: by the last SnSe obtained of the various embodiments described above2Electrode is made in/CNTs nanocomposite
Piece is assembled into lithium ion battery and carries out cyclic charging and discharging test.If attached drawing 4 is SnSe made from embodiment 12/ CNTs is nano combined
The cycle charge-discharge curve graph of material, in the electro-chemical test that current density is 0.1 C, the electric discharge of preceding charge and discharge cycles three times
Specific capacity is respectively 803.7 mAh g-1, 521.3 mAh g-1, 454.7 mAh g-1, the specific discharge capacity after 100 circulations
For 210.3 mAh g-1, illustrate SnSe2/ CNTs nanometer combined electrode material presents excellent charge and discharge cycles stability.
Claims (5)
1. a kind of SnSe2The preparation method of/CNTs lithium ion battery electrode material, it is characterised in that include the following steps:
1) a certain amount of SnCl is weighed according to molar ratio2And SeO2,；
2) two kinds of reaction raw materials are put into hydro-thermal reaction axe liner；
3) a certain amount of carbon nanotube is weighed according to certain mass ratio, equally put into liner；
4) deionized water is added into liner, stirs, liner is put into reaction kettle and is sealed；
5) reaction kettle is put into drying box and carries out hydro-thermal reaction；
6) reaction product deionized water and dehydrated alcohol alternating centrifugal are cleaned after the reaction was completed and is dried afterwards several times；
Wherein, SnCl in step 1)2With SeO2Molar ratio be 1:2；
The carbon nanotube amount of weighing meets SnCl in step 3)2Mass ratio with carbon nanotube is 10:1.
2. a kind of SnSe according to claim 12The preparation method of/CNTs lithium ion battery electrode material, feature exist
In: the deionized water that loading is 80% is added in the step 4) into liner.
3. a kind of SnSe according to claim 12The preparation method of/CNTs lithium ion battery electrode material, feature exist
In: the step 4) mixing time is 30 min.
4. a kind of SnSe according to claim 12The preparation method of/CNTs lithium ion battery electrode material, feature exist
In: hydrothermal temperature is 160~200 DEG C, soaking time is 24 h and cools to room with the furnace in the step 5) drying box
Temperature.
5. a kind of SnSe according to claim 12The preparation method of/CNTs lithium ion battery electrode material, feature exist
In: the drying temperature after the step 6) centrifugation is 80 DEG C, drying time is 12 h.
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| CN113540335A (en) * | 2021-07-15 | 2021-10-22 | 陕西科技大学 | S-doped SnSe/CNTs composite flexible film and preparation method thereof |
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| CN110752353A (en) * | 2019-09-19 | 2020-02-04 | 广东工业大学 | Flexible self-supporting tin diselenide/carbon nano tube composite film electrode material and preparation method and application thereof |
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| CN113540335A (en) * | 2021-07-15 | 2021-10-22 | 陕西科技大学 | S-doped SnSe/CNTs composite flexible film and preparation method thereof |
| CN113540335B (en) * | 2021-07-15 | 2022-11-15 | 陕西科技大学 | S-doped SnSe/CNTs composite flexible film and preparation method thereof |
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Application publication date: 20190830 |