CN106450296B - A kind of SnS of (101) crystal face preferential growth2The preparation method of nanometer sheet negative electrode material - Google Patents
A kind of SnS of (101) crystal face preferential growth2The preparation method of nanometer sheet negative electrode material Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 13
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000005864 Sulphur Substances 0.000 claims abstract description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 7
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 6
- -1 polyethylene Polymers 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 229960003511 macrogol Drugs 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical group CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 235000013878 L-cysteine Nutrition 0.000 claims description 3
- 239000004201 L-cysteine Substances 0.000 claims description 3
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 2
- KKKAMDZVMJEEHQ-UHFFFAOYSA-N [Sn].[N+](=O)(O)[O-] Chemical compound [Sn].[N+](=O)(O)[O-] KKKAMDZVMJEEHQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 2
- YGKHJWTVMIMEPQ-UHFFFAOYSA-N 1,2-propanedithiol Chemical compound CC(S)CS YGKHJWTVMIMEPQ-UHFFFAOYSA-N 0.000 claims 1
- XEUCQOBUZPQUMQ-UHFFFAOYSA-N Glycolone Chemical compound COC1=C(CC=C(C)C)C(=O)NC2=C1C=CC=C2OC XEUCQOBUZPQUMQ-UHFFFAOYSA-N 0.000 claims 1
- UWIULCYKVGIOPW-UHFFFAOYSA-N Glycolone Natural products CCOC1=C(CC=CC)C(=O)N(C)c2c(O)cccc12 UWIULCYKVGIOPW-UHFFFAOYSA-N 0.000 claims 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 11
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 11
- 229910052744 lithium Inorganic materials 0.000 abstract description 8
- 238000011160 research Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 239000010406 cathode material Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000003487 electrochemical reaction Methods 0.000 abstract description 2
- 150000002898 organic sulfur compounds Chemical class 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 13
- 239000000463 material Substances 0.000 description 13
- 230000002441 reversible effect Effects 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 238000012360 testing method Methods 0.000 description 7
- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910001290 LiPF6 Inorganic materials 0.000 description 5
- 239000006230 acetylene black Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 239000011889 copper foil Substances 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 229960004756 ethanol Drugs 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000001768 carboxy methyl cellulose Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 2
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 1
- SZPSEPZTPITHRZ-UHFFFAOYSA-N [S].CC=C Chemical compound [S].CC=C SZPSEPZTPITHRZ-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229940093429 polyethylene glycol 6000 Drugs 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
Classifications
-
- 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
- H01M4/5815—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of SnS of (101) crystal face preferential growth2The preparation method of nanometer sheet negative electrode material.This research is using inorganic tin salts as tin source, using organic sulfur compound as sulphur source, using polyethylene glycol as additive, is prepared by simple one step of solvent-thermal method with the SnS of (101) crystal face preferential growth2Nanometer sheet.These can provide sufficient electro-chemical activity site using (101) crystal face as the nanometer sheet of exposed surface in charge and discharge process, shorten the diffusion path of lithium ion, accelerate electrochemical reaction dynamics, so that the high rate performance of electrode is excellent.The advantage of the invention is that the SnS of (101) crystal face preferential growth2Preparation is simple for nanometer sheet, and can be applied to the preferential growth of other bedded substances.The SnS of (101) crystal face preferential growth of the method preparation2Nanometer sheet has excellent high rate performance, is a kind of potential high performance lithium ionic cell cathode material, is expected to be widely applied to the fields such as various portable electronic devices, electric car and aerospace.
Description
Technical field
The invention belongs to new energy materials and electrochemical field, and in particular to a kind of novel with (101) crystal face preferential growth
Lithium ion battery negative material SnS2Nanometer sheet and preparation method thereof.
Technical background
The energy is the material base of human survival and the economic base of social development.It is continuous with human society productivity
Development, demand of the people in daily production and life to the energy sharply increase.To cope with the energy shortage problem got worse,
Traditional one-shot battery is gradually substituted by reusable secondary cell.However, traditional secondary cell due to capacity is low,
Poor safety performance, cycle life are shorter, environmental pollution is more serious and volume it is heavy be unfavorable for carry and it is gradually novel
Lithium ion battery replaced.Lithium ion battery have high voltage, high-energy density, low self-discharge rate, wide use temperature range,
The advantages that long circulation life, environmental protection, memory-less effect and heavy-current discharge.Since 1991 by Sony company introduce to the market first with
Coming, lithium ion battery has been widely used in mobile phone, digital product, laptop and portable electronic equipment, and
And it is gradually expanded to fields such as electric bicycle, electric car, new energy energy storage.
Currently, commercial lithium ion battery negative material is graphite, theoretical specific capacity only 372mAhg-1, can not expire
The demand of sufficient electric car and electrokinetic cell of hybrid powered vehicle, therefore, there is an urgent need to develop novel with height ratio capacity
Negative electrode material.Wherein, SnS2Theoretical capacity is up to 1232mAh g-1, it is resourceful, low toxicity, it is low in cost the features such as, in recent years
Receive the extensive concern of researchers.However, SnS2Electric conductivity it is poor, to cause its ladder high rate performance not to the utmost such as people
Meaning.This problem seriously hinders SnS2Practical application as lithium ion battery negative material.To solve the above problems, document
In to SnS2Improved method include: by reduce particle size, shorten the diffusion path of lithium ion, to accelerate electrode electrochemical
Learn kinetics；It is compound by being carried out with carbon matrix, to improve the electronic conductance of composite material.Representative
SnS2The research work of base electrode material includes:
(1) Zhejiang University DuNing teaches research group and uses hydro-thermal method, using Tin tetrachloride pentahydrate as nickel source, thio second
Amide is sulphur source, is prepared for SnS2Nanometer sheet.Test its chemical property, the results showed that in 100mAg-1Current density under,
Its reversible specific capacity is 513mAhg after circulation 50 times-1, compared to the reversible capacity of first time circulation, capacity retention ratio 96%
(Chem.Commun.,2011,47, 1270-1272).The SnS that the preparation process obtains2Nanometer sheet is stacked along [001] direction
Growth, but the specific capacity shown is lower, and chemical property remains to be further improved.
(2) Tsinghua University Cao Huaqiang teaches research group using solvent heat and combines liquid phase method, with sodium borohydride
For reducing agent, synthesize stannic disulfide/redox graphene composite material with double sandwich structures.It is compound by what is obtained
Material is tested for the property as the negative electrode material of lithium ion battery, as a result, it has been found that: it is 120mAg in current density-1When, for the first time
Specific discharge capacity is 1032mAh g-1；After circulation 30 times, specific discharge capacity is 619mAh g-1(J.Mater.Chem.,
2012,22,23963-23970).But the composite material high rate performance of the preparation is poor, and energy consumption is high for preparation process, cost compared with
It is high.
At present for lithium ion battery negative material SnS2Study on the modification and carbon matrix it is compound mostly use electrostatic attraction,
Surface cladding process, but the combination affinity between the component of the compound of such method preparation is poor, and compound carbon matrix is adopted mostly
With graphene, carbon nanotube etc., so that preparation cost is higher.
Summary of the invention
The purpose of the present invention is to provide one kind with (101) crystal face preferential growth, lithium with excellent high rate performance from
Sub- cell negative electrode material SnS2Nanometer sheet and preparation method thereof.
The present invention provides a kind of SnS of (101) crystal face preferential growth2The preparation method of nanometer sheet, it is characterized in that using
One step solvent-thermal method simultaneously adds surfactant polyethylene, prepares using (101) crystal face as the SnS of exposed surface2Nanometer sheet；
Specific process step are as follows:
(1) pink salt of certain mol proportion is dissolved in a certain amount of solvent, stirs evenly to form clear solution, pink salt it is dense
Degree control is 1 × 10-4~3 × 10-2mol L-1；Organic sulphur source is selected to be added in clear solution, being stirred continuously keeps organic sulphur source complete
Fully dissolved；It adds surfactant polyethylene to stir evenly, organic sulphur source concentration control is 4 × 10-4~4 × 10-1mol
L-1, the control of surfactant polyethylene concentration is 2 × 10-3~5 × 10-1 mol L-1。
(2) solution obtained in step (1) is poured into the water heating kettle with polytetrafluoroethyllining lining, in insulating box one
Determine to react certain time at temperature；
Wherein pink salt described in step (1) is nitric acid tin, stannic chloride, STANNOUS SULPHATE CRYSTALLINE or its crystallization hydrate；Described is molten
Agent is one or more of deionized water, dehydrated alcohol, propyl alcohol, methanol；Organic sulphur source is ethyl mercaptan, propylene sulphur
Alcohol, thiocarbamide, L-cysteine；Polyethylene glycol described in step (1) is polyethylene glycol 200, polyethylene glycol 2000, polyethylene glycol
6000, one or more of polyethylene glycol 12000.
The temperature of insulating box is 120~240 DEG C in step (2)；The time of reaction is 10~40h.
This research uses nano modification measure, and considers SnS2Material has the layer structure of class graphene, brilliant
The direction of growth of body is larger to Electrochemical Performances.Therefore, the present invention is using inorganic tin salts as tin source, using organic sulfur compound as sulphur
It is prepared using polyethylene glycol as additive by simple one step of solvent-thermal method with the SnS of (101) crystal face preferential growth in source2
Nanometer sheet.It is living can to provide sufficient electrochemistry using (101) crystal face as the nanometer sheet of exposed surface in charge and discharge process for these
Property site, and shorten the diffusion path of lithium ion, accelerate electrochemical reaction dynamics, so that the high rate performance of electrode is excellent
It is different: higher reversible specific capacity can be shown the electrode under high current；When test electric current is restored to initial current, electrode
Specific capacity also return to initial value.
The advantage of the invention is that the SnS of (101) crystal face preferential growth2Preparation is simple for nanometer sheet, and can
To be applied to the preferential growth of other bedded substances.The SnS of (101) crystal face preferential growth of the method preparation2Nanometer sheet has
Excellent high rate performance is a kind of potential high performance lithium ionic cell cathode material, is expected to be widely applied to various portable
The fields such as electronic equipment, electric car and aerospace.
Detailed description of the invention
Fig. 1 is the SnS of embodiment 1 (101) crystal face preferential growth2The scanning electron microscope (SEM) photograph of nanometer sheet.
Fig. 2 is the SnS of embodiment 1 (101) crystal face preferential growth2The transmission High-Resolution Map of nanometer sheet.
Fig. 3 is the SnS of embodiment 1 (101) crystal face preferential growth2The high rate performance figure of nanometer sheet.
Fig. 4 is the SnS of embodiment 2 (101) crystal face preferential growth2The scanning electron microscope (SEM) photograph of nanometer sheet.
Fig. 5 is the SnS of embodiment 3 (101) crystal face preferential growth2The scanning electron microscope (SEM) photograph of nanometer sheet.
Specific embodiment
Below with reference to embodiment, the present invention will be further described, but is not limited to protection scope of the present invention:
Embodiment 1:
0.3g Tin tetrachloride pentahydrate is weighed, is dissolved in 70mL deionized water, stirs evenly to form clear solution；
It weighs 0.1g L-cysteine to be added in solution, stir evenly.Then it weighs 0.5g polyethylene glycol 200 and above-mentioned solution is added
In, obtained clear solution is finally poured into 100mL in the water heating kettle of polytetrafluoroethyllining lining, is reacted at 120 DEG C
12h.Obtained product is centrifugated and is used deionized water and ethanol washing, is then dried at 70 DEG C in thermostatic drying chamber
8h finally obtains SnS2Nanometer sheet.By 70wt.%SnS obtained2The carboxymethyl of material, the acetylene black of 15wt.% and 15wt.%
Sodium cellulosate is uniformly mixed, and slurry is made, is coated uniformly on copper foil, circular electrode pole piece is stamped into after vacuum drying, with gold
Belonging to lithium is to electrode, 1mol L-1LiPF6/ EC+DEC+DMC (volume ratio 1:1:1) be electrolyte, Celgard 2400 be every
Film is assembled into button cell.The test of ladder high rate performance is carried out to battery, charging/discharging voltage range is 0.01~3.0V, as a result
Show: in 0.1A g-1Current density under, reversible specific capacity be 1100mAh g-1；In 2A g-1High current density under, it is reversible
Specific capacity is 850mAh g-1。
Embodiment 2:
0.5g Tin tetrachloride pentahydrate is weighed, is dissolved in 80mL deionized water, stirs evenly to form clear solution；
It weighs 0.3g ethyl mercaptan to be added in solution, stir evenly.Then it weighs 0.5g Macrogol 6000 and is added in above-mentioned solution,
Obtained clear solution is finally poured into 100mL in the water heating kettle of polytetrafluoroethyllining lining, is reacted for 24 hours at 170 DEG C.It will
Obtained product is centrifugated and uses deionized water and ethanol washing, then dries 8h at 70 DEG C in thermostatic drying chamber, finally
Obtain SnS2Nanometer sheet.By 70wt.%SnS obtained2The carboxymethyl cellulose of material, the acetylene black of 15wt.% and 15wt.%
Sodium is uniformly mixed, and slurry is made, is coated uniformly on copper foil, circular electrode pole piece is stamped into after vacuum drying, is with lithium metal
To electrode, 1mol L-1LiPF6/ EC+DEC+DMC (volume ratio 1:1:1) is electrolyte, and Celgard 2400 is diaphragm, group
Dress up button cell.The test of ladder high rate performance is carried out to battery, charging/discharging voltage range is 0.01~3.0V, the results showed that
In 0.1A g-1Current density under, reversible specific capacity be 850mAh g-1；In 2A g-1High current density under, reversible specific capacity
For 505mAh g-1。
Embodiment 3:
0.5g Tin tetrachloride pentahydrate is weighed, is dissolved in 80mL deionized water, stirs evenly to form clear solution；
It weighs 0.3g ethyl mercaptan to be added in solution, stir evenly.Then it weighs 0.25g Macrogol 6000 and is added in above-mentioned solution,
Obtained clear solution is finally poured into 100mL in the water heating kettle of polytetrafluoroethyllining lining, is reacted for 24 hours at 170 DEG C.It will
Obtained product is centrifugated and uses deionized water and ethanol washing, then dries 8h at 70 DEG C in thermostatic drying chamber, finally
Obtain SnS2Nanometer sheet.By 70wt.%SnS obtained2The carboxymethyl cellulose of material, the acetylene black of 15wt.% and 15wt.%
Sodium is uniformly mixed, and slurry is made, is coated uniformly on copper foil, circular electrode pole piece is stamped into after vacuum drying, is with lithium metal
To electrode, 1mol L-1LiPF6/ EC+DEC+DMC (volume ratio 1:1:1) is electrolyte, and Celgard 2400 is diaphragm, group
Dress up button cell.The test of ladder high rate performance is carried out to battery, charging/discharging voltage range is 0.01~3.0V, the results showed that
In 0.1A g-1Current density under, reversible specific capacity be 600mAh g-1；In 2A g-1High current density under, reversible specific capacity
For 409mAh g-1。
Embodiment 4:
0.2g Tin tetrachloride pentahydrate is weighed, is dissolved in 50mL deionized water, stirs evenly to form clear solution；
It weighs 0.4g thiocarbamide to be added in solution, stir evenly.Then it weighs 0.6g polyethylene glycol 2000 and is added in above-mentioned solution, most
Obtained clear solution is poured into 100mL in the water heating kettle of polytetrafluoroethyllining lining afterwards, reacts 40h at 190 DEG C.Will
The product arrived is centrifugated and uses deionized water and ethanol washing, then dries 8h at 70 DEG C in thermostatic drying chamber, final to obtain
To SnS2Nanometer sheet.By 70wt.%SnS obtained2The sodium carboxymethylcellulose of material, the acetylene black of 15wt.% and 15wt.%
It is uniformly mixed, slurry is made, is coated uniformly on copper foil, circular electrode pole piece is stamped into after vacuum drying, be pair with lithium metal
Electrode, 1mol L-1LiPF6/ EC+DEC+DMC (volume ratio 1:1:1) is electrolyte, and Celgard 2400 is diaphragm, assembling
At button cell.The test of ladder high rate performance is carried out to battery, charging/discharging voltage range is 0.01~3.0V, the results showed that
0.1A g-1Current density under, reversible specific capacity be 1000mAh g-1；In 2A g-1High current density under, reversible specific capacity
For 750mAh g-1。
Embodiment 5:
0.5g Tin tetrachloride pentahydrate is weighed, is dissolved in 80mL deionized water, stirs evenly to form clear solution；
It weighs 0.3g ethyl mercaptan to be added in solution, stir evenly.Then it weighs 1g Macrogol 6000 and is added in above-mentioned solution, most
Obtained clear solution is poured into 100mL in the water heating kettle of polytetrafluoroethyllining lining afterwards, is reacted for 24 hours at 170 DEG C.Will
The product arrived is centrifugated and uses deionized water and ethanol washing, then dries 8h at 70 DEG C in thermostatic drying chamber, final to obtain
To SnS2Nanometer sheet.By 70wt.%SnS obtained2The sodium carboxymethylcellulose of material, the acetylene black of 15wt.% and 15wt.%
It is uniformly mixed, slurry is made, is coated uniformly on copper foil, circular electrode pole piece is stamped into after vacuum drying, be pair with lithium metal
Electrode, 1mol L-1LiPF6/ EC+DEC+DMC (volume ratio 1:1:1) is electrolyte, and Celgard 2400 is diaphragm, assembling
At button cell.The test of ladder high rate performance is carried out to battery, charging/discharging voltage range is 0.01~3.0V, the results showed that
0.1A g-1Current density under, reversible specific capacity be 950mAh g-1；In 2A g-1High current density under, reversible specific capacity is
705mAh g-1。
Claims (5)
1. a kind of SnS of (101) crystal face preferential growth2The preparation method of nanometer sheet negative electrode material, it is characterized in that using a step solvent
Thermal method simultaneously adds surfactant polyethylene, prepares using (101) crystal face as the SnS of exposed surface2Nanometer sheet；Concrete technology
Step are as follows:
(1) pink salt of certain molar weight is dissolved in a certain amount of solvent, stirs evenly to form clear solution, the concentration of pink salt
Control is 1 × 10-4~3 × 10-2mol· L-1；Organic sulphur source is selected to be added in clear solution, being stirred continuously keeps organic sulphur source complete
Fully dissolved；It adds surfactant polyethylene to stir evenly, organic sulphur source concentration control is 4 × 10-4~4 × 10- 1mol· L-1, the control of surfactant polyethylene concentration is 2 × 10-3~5 × 10-1mol· L-1；
(2) solution obtained in step (1) is poured into the water heating kettle with polytetrafluoroethyllining lining, in temperature certain in insulating box
Degree is lower to react certain time；
Organic sulphur source described in step (1) is ethyl mercaptan, propylene mercaptan, thiocarbamide, L-cysteine；
Polyethylene glycol described in step (1) is polyethylene glycol 200, polyethylene glycol 2000, Macrogol 6000, polyethylene glycol
One or more of 12000.
2. the SnS of (101) crystal face preferential growth according to claim 12The preparation method of nanometer sheet negative electrode material, it is special
Sign is: pink salt described in step (1) is nitric acid tin, stannic chloride, STANNOUS SULPHATE CRYSTALLINE or its crystallization hydrate.
3. the SnS of (101) crystal face preferential growth according to claim 12The preparation method of nanometer sheet negative electrode material, it is special
Sign is: solvent described in step (1) is one or more of deionized water, dehydrated alcohol, propyl alcohol, methanol.
4. the SnS of (101) crystal face preferential growth according to claim 12The preparation method of nanometer sheet negative electrode material, it is special
Sign is: the temperature of insulating box is 120~240 DEG C in step (2).
5. the SnS of (101) crystal face preferential growth according to claim 12The preparation method of nanometer sheet negative electrode material, it is special
Sign is: the time reacted in step (2) is 10~40h.
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| "Solvothermally synthesized SnS nanorods with high carrier mobility leading to thermoelectric enhancement";Qing Tan,et al.;《The Royal Society of Chemistry》;20160428;第6卷;第43985–43988页 |
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