CN106784814A - A kind of hexagonal sheet SnS2The preparation method of anode material of lithium-ion battery - Google Patents
A kind of hexagonal sheet SnS2The preparation method of anode material of lithium-ion battery Download PDFInfo
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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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Abstract
The present invention discloses a kind of hexagonal sheet SnS2The preparation method of anode material of lithium-ion battery, including：1) thioacetamide is dissolved in deionized water, obtains solution A；2) solution A is added to obtain transparent settled solution C ten hexamethyl trimethylammonium bromides；3) according to elemental mole ratios nSn:nS=1.0：Be dissolved in stannic chloride pentahydrate in transparent settled solution C by (1.2~2.4), mixes and is uniformly configured to mixed solution D；4) pH=1~9 of regulation mixed solution D form solution E；5) gained E solution is carried out into microwave hydrothermal reaction；6) product washing, freeze-drying are to obtain hexagonal sheet SnS2Anode material of lithium-ion battery.The inventive method, with preparation cost is low, simple to operate, short preparation period the characteristics of, prepared product, lamellar spacing size reaches that a few to tens of nanometers, purity are high, crystallinity is strong, pattern is uniform, and being applied to sodium-ion battery negative pole has excellent charge-discharge magnification performance.
Description
Technical field
The invention belongs to anode material of lithium-ion battery technical field, more particularly to a kind of anode material of lithium-ion battery
Preparation method.
Background technology
Sodium-ion battery is a kind of model electrochemical power supply, with raw material resources is abundant, relatively low cost, specific capacity and effect
The advantages of rate is higher, more meets the requirement of scale stored energy application, is lifting extensive regenerative resource grid integration ability, is carrying
Electric energy service efficiency high and quality of power supply aspect have application potential, simultaneously because its specific capacity is high, light weight, long lifespan and nothing
The significant advantages such as Memorability, also have extensive in fields such as Aero-Space, hybrid-electric car and portable electric appts
Using.In this context, sodium-ion battery causes the extensive concern in worldwide, critical material and related skill in recent years
Art progress is rapid.But for lithium ion, sodium ion has larger ionic radius (0.102nm vs.0.076nm
Of Li), this causes that finding suitable embedding sodium material tool acquires a certain degree of difficulty.
Stannic disulfide (SnS2) belong to IV:VI race's binary compound, a=b=0.365nm, c=0.589nm, with CdI2
The layer structure of type.This construction unit is the sandwich structure that tin ion is added by the sulphion centre of two-layer hexagonal closs packing
(S-Sn-S) constitute, there are six sulphions to take AB AB hexagonal closs packings to form regular octahedron around each tin ion and be coordinated,
Sn4+It is placed in two-layer S2-Between, it is Covalent bonding together in layer, there is weak Van der Waals force between layers.SnS2This stratiform
There are many lattice vacancies in structure, can be used as the host lattice of " intercalation ".Superior pliability in this structure is enabled it to
As substrate, by the insertion of conjugated compound, the intercalation compound with unique photoelectric property is formed.Therefore SnS2It is considered as
It is the promising candidate of negative material of sodium-ion battery.With going deep into for research, it has been found that SnS2Can also with sodium from
There is the alloy reaction similar with tin oxide in son, and compare SnO2With more preferable cyclical stability, therefore SnS in recent years2As sodium
Ion battery cathode material is received significant attention.
Because granule-morphology is likely to affect to the chemical property of sample, particle is smaller, specific surface
Product is bigger, then contact of the material with electrolyte is better, Na+Migration distance can also shorten, be so more beneficial for sodium-ion battery
The lifting of negative material high rate performance, in addition, Doped ions can not only change in nano material the optics of material, electricity and
The properties such as magnetics, under certain condition, can be with the pattern of controlled material.Nano material some special structures are in electrochemistry
The characteristics of aspects such as energy can produce some novel.
The preparation nanometer SnS for being reported at present2The method of material be mainly chemical precipitation method [Yong C Z, Zhen N D,
Li K W,et al.Size-Controlled Hydrothermal Synthesis Of SnS2Nanoparticles With
High Performance In Visible Light-Driven Photocatalytic Degradation Of
Aqueous Methyl Orange[J].Separation&Purification Technology,2011,81(1):101–
107.], solid reaction process [Qamar M, Gondal M A, Zh.Y.Laser-induced efficient reduction of
Cr(VI)catalyzed by ZnO nanoparticles.[J].Journal of Hazardous Materials,2011,
187(4):258-263.], solvent thermal reaction method [Qihua Wang, Dewei Wang, et.al.Porous
SnO2nanoflakes with loose-packed structure Morphology conserved
transformation from SnS2precursor and application in lithium ion batteries
and gas sensors[J].Journal of Physics&Chemistry of Solids,2011,72(6):630-
636.].Wherein chemical precipitation method can chemically react at room temperature, but the product crystallinity for generally yielding it is very poor (or
It is amorphous), granule-morphology and size be irregular and broad particle distribution.Although solid reaction process have do not need solvent,
Equipment is simple and the advantages of easy control of reaction conditions, but carried out in solid phase due to reacting, and generally reaction is not thorough, yield
It is relatively low.Solvent thermal reaction method needs the condition of strict control solvent heat.Hydro-thermal method has incomparable excellent of many other methods
More property, prepares for nano-powder in recent years and nano materials research causes the attention of people, but conventional hydrothermal reaction side
Method prepares SnS2Powder has that the reaction time is more long, granule-morphology is whard to control, it is middle easily to occur.
The content of the invention
It is an object of the invention to provide a kind of hexagonal sheet SnS2The preparation method of anode material of lithium-ion battery, with
Solve above-mentioned technical problem.
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of hexagonal sheet SnS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
1) thioacetamide is dissolved in deionized water, is configured to the solution A that concentration is 0.2~1.2mol/L；
2) to being formed uniformly suspension B in ten hexamethyl trimethylammonium bromides being added into solution A under magnetic agitation effect,
Ultrasonic disperse to being completely dissolved, transparent settled solution C；
3) according to elemental mole ratios nSn:nS=1.0：Stannic chloride pentahydrate is dissolved in transparent settled solution C by (1.2~2.4)
In, stirred under the conditions of magnetic agitation and be configured to mixed solution D；
4) pH=1~9 of regulation mixed solution D form solution E；
5) gained E solution is put into microwave hydrothermal reaction kettle sealing, packing ratio is controlled 40%~60%, is put into Microwave Water
Thermal response instrument, at 120~210 DEG C, the reaction time is controlled in 0.5~3h for reaction temperature control；
6) after question response terminates, presoma is taken out, washing obtains yellowish-brown presoma, and freeze-drying is to obtain hexagonal lamella
Shape SnS2Anode material of lithium-ion battery.
Further, step 2) in 15~20min of ultrasonic disperse be completely dissolved.
Further, step 4) in the pH of mixed solution D is adjusted by organic base.
Further, step 4) described in organic base be diethylenetriamine.
Further, the washing is to distinguish centrifuge washing 2~3 times through deionized water and absolute ethyl alcohol.
Further, the time of freeze-drying is 10~12h.
Further, in mixed solution D the molar concentration of Sn ions and ten hexamethyl trimethylammonium bromides molar concentration
Ratio be 1~10.
Further,
1) thioacetamide is dissolved in deionized water, is configured to the solution A that concentration is 0.5mol/L；
2) to being formed uniformly suspension B in ten hexamethyl trimethylammonium bromides being added into solution A under magnetic agitation effect,
15~20min of ultrasonic disperse is completely dissolved, transparent settled solution C；
3) according to elemental mole ratios nSn:nS=1.0:1.2 are dissolved in transparent settled solution C stannic chloride pentahydrate, in magnetic
10~15min is stirred under power stirring condition and is configured to solution D；The molar concentration of Sn ions and ten hexamethyls three in mixed solution D
The ratio of the molar concentration of methyl bromide ammonium is 1~10；
4) organic alkali source diethylenetriamine is added dropwise under magnetic agitation effect to mixed solution D, pH value of solution is adjusted
=7 form solution E；
5) gained E solution is put into microwave hydrothermal reaction kettle sealing, packing ratio is controlled 40%, is put into microwave hydrothermal reaction
Instrument, at 180 DEG C, the reaction time is controlled in 2h for reaction temperature control；
6) after question response terminates, presoma is taken out, centrifuge washing is distinguished 2~3 times through deionized water and absolute ethyl alcohol, obtained
Yellowish-brown presoma, 10~12h of freeze-drying obtains hexagonal sheet SnS2Anode material of lithium-ion battery.
Further, the hexagonal sheet SnS2Anode material of lithium-ion battery under 200mA/g current densities first
Discharge capacity is 1120mAh/g, and coulombic efficiency is 99% after 3 circulations.
Relative to prior art, the invention has the advantages that：
The present invention prepares hexagonal sheet SnS2The method of anode material of lithium-ion battery, with preparation cost it is low, operation
Simply, the characteristics of short preparation period, prepared hexagonal sheet SnS2Anode material of lithium-ion battery, lamellar spacing size reaches
To a few to tens of nanometers, purity is high, crystallinity is strong, pattern is uniform, and being applied to sodium-ion battery negative pole has excellent filling
Discharge-rate performance.
Further, the SnS that prepared by the present invention2Anode material of lithium-ion battery is that hexagonal is laminar structured, stratiform thickness
Size reaches a few to tens of nanometers, and its preparation cost is low, charge-discharge performance is excellent, and under the current density of 200mA/g, it is first
Discharge capacity can reach 625mAh/g, and after circulating 50 times, capacity is maintained at 300mAh/g, have under high current density higher
Capability retention.
Brief description of the drawings
Fig. 1 is nanometer hexagonal sheet SnS prepared by the embodiment of the present invention 12The SEM figures of anode material of lithium-ion battery.
Fig. 2 is nanometer hexagonal sheet SnS prepared by the embodiment of the present invention 12The cyclicity of anode material of lithium-ion battery
Can figure.
Specific embodiment
Embodiment 1
A kind of hexagonal sheet SnS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
(1) by thioacetamide (CH3CSNH2) be dissolved in deionized water, by CH under the conditions of magnetic agitation3CSNH2Stirring
To being completely dissolved, the solution A that concentration is 0.5mol/L is configured to；
(2) to being formed uniformly in ten hexamethyl trimethylammonium bromides (CTAB) being added into solution A under magnetic agitation effect
Suspension B, 15~20min of ultrasonic disperse is completely dissolved, transparent settled solution C；
(3) according to elemental mole ratios nSn:nS=1.0:1.2 by stannic chloride pentahydrate (SnCl4·5H2O) it is dissolved in transparent clarification
In solution C, 10~15min of stirring is configured to solution D under the conditions of magnetic agitation；The molar concentration of Sn ions in mixed solution D
It is 1 with the ratio of the molar concentration of ten hexamethyl trimethylammonium bromides；
(4) organic alkali source diethylenetriamine (C is added dropwise under magnetic agitation effect to mixed solution D4H13N3), adjust
Section pH value of solution=7 form solution E；
(5) gained E solution is put into microwave hydrothermal reaction kettle sealing, packing ratio is controlled 40%, is put into microwave hydrothermal anti-
Ying Yi, at 180 DEG C, the reaction time is controlled in 2h for reaction temperature control；
(6) after question response terminates, presoma is taken out, centrifuge washing is distinguished 2~3 times through deionized water and absolute ethyl alcohol, obtained
To yellowish-brown presoma, 10~12h of freeze-drying is to obtain hexagonal sheet SnS2Anode material of lithium-ion battery.
Fig. 1 is nanometer hexagonal sheet SnS prepared by the embodiment of the present invention 12The SEM figures of anode material of lithium-ion battery.
As can be seen from the figure prepared sample has stronger crystallinity.
Fig. 2 is nanometer hexagonal sheet SnS prepared by the embodiment of the present invention 12The cyclicity of anode material of lithium-ion battery
Can figure.As can be seen from the figure prepared nanometer hexagonal sheet SnS2Anode material of lithium-ion battery is close in 200mA/g electric currents
Discharge capacity is 1120mAh/g first under degree, and coulombic efficiency is close to 99% after 3 circulations.
Embodiment 2
A kind of hexagonal sheet SnS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
(1) by thioacetamide (CH3CSNH2) be dissolved in deionized water, by CH under the conditions of magnetic agitation3CSNH2Stirring
To being completely dissolved, the solution A that concentration is 0.9mol/L is configured to；
(2) to being formed uniformly in ten hexamethyl trimethylammonium bromides (CTAB) being added into solution A under magnetic agitation effect
Suspension B, 15~20min of ultrasonic disperse is completely dissolved, transparent settled solution C；
(3) according to elemental mole ratios nSn:nS=1.0:2.0 by stannic chloride pentahydrate (Sn Cl4·5H2O) it is dissolved in transparent clear
In clear solution C, 10~15min of stirring is configured to solution D under the conditions of magnetic agitation；Sn ions is mole dense in mixed solution D
Degree is 1 with the ratio of the molar concentration of ten hexamethyl trimethylammonium bromides；
(4) organic alkali source diethylenetriamine (C is added dropwise under magnetic agitation effect to mixed solution D4H13N3), adjust
Section pH value of solution=9 form solution E；
(5) gained E solution is put into microwave hydrothermal reaction kettle sealing, packing ratio is controlled 50%, is put into microwave hydrothermal anti-
Ying Yi, at 120 DEG C, the reaction time is controlled in 0.5h for reaction temperature control；
(6) after question response terminates, presoma is taken out, centrifuge washing is distinguished 2~3 times through deionized water and absolute ethyl alcohol, obtained
To yellowish-brown presoma, 10~12h of freeze-drying is to obtain hexagonal sheet SnS2Anode material of lithium-ion battery.
Embodiment 3
A kind of hexagonal sheet SnS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
(1) by thioacetamide (CH3CSNH2) be dissolved in deionized water, by CH under the conditions of magnetic agitation3CSNH2Stirring
To being completely dissolved, the solution A that concentration is 1.2mol/L is configured to；
(2) to being formed uniformly in ten hexamethyl trimethylammonium bromides (CTAB) being added into solution A under magnetic agitation effect
Suspension B, 15~20min of ultrasonic disperse is completely dissolved, transparent settled solution C；
(3) according to elemental mole ratios nSn:nS=1.0:2.4 by stannic chloride pentahydrate (Sn Cl4·5H2O) it is dissolved in transparent clear
In clear solution C, 10~15min of stirring is configured to solution D under the conditions of magnetic agitation；Sn ions is mole dense in mixed solution D
Degree is 10 with the ratio of the molar concentration of ten hexamethyl trimethylammonium bromides；
(4) organic alkali source diethylenetriamine (C is added dropwise under magnetic agitation effect to mixed solution D4H13N3), adjust
Section pH value of solution=1 forms solution E；
(5) gained E solution is put into microwave hydrothermal reaction kettle sealing, packing ratio is controlled 60%, is put into microwave hydrothermal anti-
Ying Yi, at 210 DEG C, the reaction time is controlled in 3h for reaction temperature control；
(6) after question response terminates, presoma is taken out, centrifuge washing is distinguished 2~3 times through deionized water and absolute ethyl alcohol, obtained
To yellowish-brown presoma, 10~12h of freeze-drying is to obtain hexagonal sheet SnS2Anode material of lithium-ion battery.
Embodiment 4
A kind of hexagonal sheet SnS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
(1) by thioacetamide (CH3CSNH2) be dissolved in deionized water, by CH under the conditions of magnetic agitation3CSNH2Stirring
To being completely dissolved, the solution A that concentration is 0.2mol/L is configured to；
(2) to being formed uniformly in ten hexamethyl trimethylammonium bromides (CTAB) being added into solution A under magnetic agitation effect
Suspension B, 15~20min of ultrasonic disperse is completely dissolved, transparent settled solution C；
(3) according to elemental mole ratios nSn:nS=1.0:1.8 by stannic chloride pentahydrate (Sn Cl4·5H2O) it is dissolved in transparent clear
In clear solution C, 10~15min of stirring is configured to solution D under the conditions of magnetic agitation；Sn ions is mole dense in mixed solution D
Degree is 5 with the ratio of the molar concentration of ten hexamethyl trimethylammonium bromides；
(4) organic alkali source diethylenetriamine (C is added dropwise under magnetic agitation effect to mixed solution D4H13N3), adjust
Section pH value of solution=5 form solution E；
(5) gained E solution is put into microwave hydrothermal reaction kettle sealing, packing ratio is controlled 40%, is put into microwave hydrothermal anti-
Ying Yi, at 180 DEG C, the reaction time is controlled in 1.5h for reaction temperature control；
(6) after question response terminates, presoma is taken out, centrifuge washing is distinguished 2~3 times through deionized water and absolute ethyl alcohol, obtained
To yellowish-brown presoma, 10~12h of freeze-drying is to obtain hexagonal sheet SnS2Anode material of lithium-ion battery.
Claims (9)
1. a kind of hexagonal sheet SnS2The preparation method of anode material of lithium-ion battery, it is characterised in that comprise the following steps：
1) thioacetamide is dissolved in deionized water, is configured to the solution A that concentration is 0.2~1.2mol/L；
2) it is ultrasonic to suspension B is formed uniformly in ten hexamethyl trimethylammonium bromides being added into solution A under magnetic agitation effect
It is dispersed to and is completely dissolved, transparent settled solution C；
3) according to elemental mole ratios nSn:nS=1.0：Be dissolved in stannic chloride pentahydrate in transparent settled solution C by (1.2~2.4),
Stirred under the conditions of magnetic agitation and be configured to mixed solution D；
4) pH=1~9 of regulation mixed solution D form solution E；
5) gained E solution is put into microwave hydrothermal reaction kettle sealing, packing ratio is controlled 40%~60%, is put into microwave hydrothermal anti-
Ying Yi, at 120~210 DEG C, the reaction time is controlled in 0.5~3h for reaction temperature control；
6) after question response terminates, presoma is taken out, washing obtains yellowish-brown presoma, and freeze-drying is to obtain hexagonal sheet
SnS2Anode material of lithium-ion battery.
2. a kind of hexagonal sheet SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
Be, step 2) in 15~20min of ultrasonic disperse be completely dissolved.
3. a kind of hexagonal sheet SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
Be, step 4) in the pH of mixed solution D is adjusted by organic base.
4. a kind of hexagonal sheet SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
It is that the washing is to distinguish centrifuge washing 2~3 times through deionized water and absolute ethyl alcohol.
5. a kind of hexagonal sheet SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
It is that the time of freeze-drying is 10~12h.
6. a kind of hexagonal sheet SnS according to claim 32The preparation method of anode material of lithium-ion battery, its feature
It is that the organic base is diethylenetriamine.
7. a kind of hexagonal sheet SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
Be, in mixed solution D the ratio of the molar concentration of the molar concentration of Sn ions and ten hexamethyl trimethylammonium bromides for 1~
10。
8. a kind of hexagonal sheet SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
It is,
1) thioacetamide is dissolved in deionized water, is configured to the solution A that concentration is 0.5mol/L；
2) it is ultrasonic to suspension B is formed uniformly in ten hexamethyl trimethylammonium bromides being added into solution A under magnetic agitation effect
15~20min of dispersion is completely dissolved, transparent settled solution C；
3) according to elemental mole ratios nSn:nS=1.0:1.2 are dissolved in transparent settled solution C stannic chloride pentahydrate, are stirred in magnetic force
10~15min is stirred under the conditions of mixing and is configured to solution D；The molar concentration of Sn ions and ten hexamethyl trimethyls in mixed solution D
The ratio of the molar concentration of ammonium bromide is 1~10；
4) organic alkali source diethylenetriamine is added dropwise under magnetic agitation effect to mixed solution D, pH value of solution=7 shape is adjusted
Into solution E；
5) gained E solution is put into microwave hydrothermal reaction kettle sealing, packing ratio is controlled 40%, is put into microwave hydrothermal reaction,
At 180 DEG C, the reaction time is controlled in 2h for reaction temperature control；
6) after question response terminates, presoma is taken out, centrifuge washing is distinguished 2~3 times through deionized water and absolute ethyl alcohol, obtain yellowish-brown
Color presoma, 10~12h of freeze-drying obtains hexagonal sheet SnS2Anode material of lithium-ion battery.
9. a kind of hexagonal sheet SnS according to claim 82The preparation method of anode material of lithium-ion battery, its feature
It is, the hexagonal sheet SnS2Discharge capacity is anode material of lithium-ion battery first under 200mA/g current densities
1120mAh/g, coulombic efficiency is 99% after 3 circulations.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112164787A (en) * | 2020-09-25 | 2021-01-01 | 贵港益乐科技发展有限公司 | Three-dimensional SnS2Lithium ion battery cathode material for modifying N-doped mesoporous carbon |
| CN113968590A (en) * | 2021-10-15 | 2022-01-25 | 陕西科技大学 | Alkali metal ion intercalation SnS2Preparation method thereof, application of preparation method in battery negative electrode material and preparation method |
| WO2022021642A1 (en) * | 2020-07-31 | 2022-02-03 | 广东凯金新能源科技股份有限公司 | Sodium ion battery negative electrode material and preparation method therefor |
-
2016
- 2016-12-07 CN CN201611116943.6A patent/CN106784814A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| CHUNRUI WANG等: "Hydrothermal Synthesis and Characterization of SnS2 Nanocrystals", 《CHEMISTRY LETTERS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022021642A1 (en) * | 2020-07-31 | 2022-02-03 | 广东凯金新能源科技股份有限公司 | Sodium ion battery negative electrode material and preparation method therefor |
| CN112164787A (en) * | 2020-09-25 | 2021-01-01 | 贵港益乐科技发展有限公司 | Three-dimensional SnS2Lithium ion battery cathode material for modifying N-doped mesoporous carbon |
| CN113968590A (en) * | 2021-10-15 | 2022-01-25 | 陕西科技大学 | Alkali metal ion intercalation SnS2Preparation method thereof, application of preparation method in battery negative electrode material and preparation method |
| CN113968590B (en) * | 2021-10-15 | 2023-08-22 | 陕西科技大学 | Alkali metal ion intercalation SnS 2 And preparation method thereof, and application of battery anode material and preparation method thereof |
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Application publication date: 20170531 |