CN106450296A - Preparation method of SnS2 nanosheet negative electrode material preferably growing along (101) crystal face - Google Patents
Preparation method of SnS2 nanosheet negative electrode material preferably growing along (101) crystal face Download PDFInfo
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- H—ELECTRICITY
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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 invention discloses a preparation method of an SnS2 nanosheet negative electrode material preferably growing along a (101) crystal face. The SnS2 nanosheet preferably growing along the (101) crystal face is prepared through a simple solvent thermal one-step method by using inorganic tin salt as a tin source, organic sulfide as a sulfur source and polyethylene glycol as an additive. According to the nanosheet using (101) the crystal face as exposed surfaces, sufficient electrochemical active sites can be provided in the charging and discharging process, the diffusion paths of lithium ions are shortened, and the electrochemical reaction kinetics is quickened, so that the rate capability of the electrode is excellent. The SnS2 nanosheet preferably growing along the (101) crystal face has the advantages that the preparation technology is simple and practical and the SnS2 nanosheet can be applied to preferable growth of other layers substances. The SnS2 nanosheet preferably growing along the (101) crystal face prepared by using the method has excellent rate capability, is a potential high-performance lithium ion cell negative electrode material, and is expected to be widely applied to various fields such as portable electronic equipment, electric automobiles and aerospace.
Description
Technical field
The invention belongs to new energy materialses and electrochemical field and in particular to a kind of new 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 bases of social development.Continuous with the human society productivity
Development, people drastically increase to the demand of the energy in daily production and life.For tackling increasingly serious energy shortage problem,
Traditional one-shot battery is gradually substituted by reusable secondary cell.However, traditional secondary cell because capacity is low,
Poor safety performance, cycle life are shorter, environmental pollution is more serious and volume heaviness is unfavorable for carrying and gradually new
Lithium ion battery replaced.Lithium ion battery have high voltage, high-energy-density, low self-discharge rate, wide using temperature range,
The advantages of long circulation life, environmental protection, memory-less effect and heavy-current discharge.From 1991 by Sony company introduce to the market first with
Come, lithium ion battery has been widely used in mobile phone, digital product, notebook computer and portable electronic equipment, and
And progressively expand to fields such as electric bicycle, electric automobile, new forms of energy energy storage.
At present, commercial lithium ion battery negative material is graphite, its theoretical specific capacity only 372mAhg-1, cannot expire
Sufficient electric automobile and the demand of electrokinetic cell of hybrid powered vehicle, therefore, new have height ratio capacity in the urgent need to developing
Negative material.Wherein, SnS2Theoretical capacity is up to 1232mAh g-1, aboundresources, low toxicity, the features such as with low cost, in recent years
Receive the extensive concern of researchers.However, SnS2Electric conductivity poor, thus causing its ladder high rate performance not to the utmost as people
Meaning.This problem seriously hinders SnS2Practical application as lithium ion battery negative material.For solving the above problems, document
In to SnS2Improved method include：By reducing particle size, shorten the evolving path of lithium ion, thus accelerating electrode electrochemical
Learn kinetics；By being combined with carbon matrix, thus improving the electronic conductance of composite.Representative SnS2
The research work of base electrode material includes：
(1) Zhejiang University DuNing professor research group adopts hydro-thermal method, with Tin tetrachloride pentahydrate as nickel source, thio second
Amide is sulphur source, is prepared for SnS2Nanometer sheet.Test its chemical property, result shows：In 100mAg-1Electric current density under,
After circulating 50 times, its reversible specific capacity is 513mAhg-1, compared to the reversible capacity of first time circulation, capability retention is 96%
(Chem.Commun.,2011,47,1270-1272).The SnS that this preparation technology obtains2Nanometer sheet stacks along [001] direction
Growth, but the specific capacity showing is relatively low, and its chemical property remains to be further improved.
(2) Tsing-Hua University Cao Huaqiang professor research group using solvent thermal and combines liquid phase method, with sodium borohydride
For reducing agent, synthesize the stannic disulfide/redox graphene composite with double sandwich structures.Compound by obtain
Material carries out performance test as the negative material of lithium ion battery, it is found that：It is 120mAg in electric current density-1When, first
Specific discharge capacity is 1032mAh g-1；After circulation 30 times, its specific discharge capacity is 619mAh g-1(J.Mater.Chem.,
2012,22,23963-23970).But the composite high rate performance of this preparation is poor, and preparation process energy consumption is big, and cost is relatively
High.
At present for lithium ion battery negative material SnS2Study on the modification, and carbon matrix be combined adopt electrostatic attraction,
Surface coating method, but the combination affinity between the component of complex of such method preparation is poor, and compound carbon matrix is adopted mostly
With Graphene, CNT etc. so that preparation cost is higher.
Content of the invention
It is an object of the invention to provide one kind with lithium (101) crystal face preferential growth, that there is excellent high rate performance from
Sub- cell negative electrode material SnS2Nanometer sheet and preparation method thereof.
The invention provides a kind of SnS of (101) crystal face preferential growth2The preparation method of nanometer sheet, is characterized in that adopting
One step solvent-thermal method simultaneously adds surfactant polyethylene, prepares the SnS with (101) crystal face as exposed surface2Nanometer sheet；
Concrete technology step is：
(1) pink salt of certain mol proportion is dissolved in a certain amount of solvent, stir formation settled solution, pink salt dense
Degree controls 1 × 10-4～3 × 10-2mol L-1；Added in settled solution from organic sulphur source, be stirred continuously and make organic sulphur source complete
CL；Add surfactant polyethylene to stir, organic sulphur source concentration controls 4 × 10-4～4 × 10-1mol
L-1, surfactant polyethylene concentration controls 2 × 10-3～5 × 10-1mol L-1.
(2) solution obtaining in step (1) is poured into in teflon-lined water heating kettle, one in calorstat
Determine to react certain time at temperature；
Pink salt wherein described in step (1) be nitric acid stannum, stannic chloride, STANNOUS SULPHATE CRYSTALLINE or its crystallize hydrate；Described is molten
Agent is one or more of deionized water, dehydrated alcohol, propanol, methanol；Described organic sulphur source is ethyl mercaptan, propylene sulfur
Alcohol, thiourea, L-Cysteine；Polyethylene Glycol described in step (1) is polyethylene glycol 200, Macrogol 2000, Polyethylene Glycol
6000th, one or more of Polyethylene Glycol 12000.
In step (2), the temperature of calorstat is 120～240 DEG C；The time of reaction is 10～40h.
This research adopts 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 with inorganic tin salts as Xi Yuan, with organic sulfur compound as sulfur
Source, with Polyethylene Glycol as additive, is prepared by simple solvent-thermal method one step with the SnS of (101) crystal face preferential growth2Receive
Rice piece.These nanometer sheet with (101) crystal face as exposed surface, can provide the electro-chemical activity of abundance in charge and discharge process
Site, and shorten the evolving path of lithium ion, accelerate electrochemical reaction kinetics, so that the high rate performance of electrode is excellent
Different：Even if higher reversible specific capacity also can be shown in high current bottom electrode；When test electric current returns to initial current, electrode
Specific capacity also return to initial value.
It is an advantage of the current invention 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 automobile and Aero-Space.
Brief description
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
With reference to embodiment, the present invention will be further described, but is not limited to protection scope of the present invention：
Embodiment 1：
Weigh 0.3g Tin tetrachloride pentahydrate, be dissolved in 70mL deionized water, stir formation settled solution；
Weigh 0.1g L-Cysteine to add in solution, stir.Then weigh 0.5g polyethylene glycol 200 and add above-mentioned solution
In, finally the settled solution obtaining is poured into 100mL and carry in teflon-lined water heating kettle, react at 120 DEG C
12h.By the product obtaining centrifugation and deionized water and washing with alcohol, then dry at 70 DEG C in thermostatic drying chamber
8h, finally gives SnS2Nanometer sheet.The 70wt.%SnS that will be obtained2The carboxymethyl of material, the acetylene black of 15wt.% and 15wt.%
Sodium cellulosate mix homogeneously, makes slurry, is coated uniformly on Copper Foil, is stamped into circular electrode pole piece, with gold after vacuum drying
Belonging to lithium is to electrode, 1mol L-1LiPF6(volume ratio is 1 to/EC+DEC+DMC:1:1) be electrolyte, Celgard2400 be every
Film, is assembled into button cell.Battery is carried out with ladder high rate performance test, charging/discharging voltage scope is 0.01～3.0V, result
Show：In 0.1A g-1Electric current density under, reversible specific capacity be 1100mAh g-1；In 2A g-1High current density under, reversible
Specific capacity is 850mAh g-1.
Embodiment 2：
Weigh 0.5g Tin tetrachloride pentahydrate, be dissolved in 80mL deionized water, stir formation settled solution；
Weigh 0.3g ethyl mercaptan to add in solution, stir.Then weigh 0.5g polyethylene glycol 6000 and add in above-mentioned solution,
Afterwards the settled solution obtaining is poured into 100mL and carry in teflon-lined water heating kettle, react 24h at 170 DEG C.Will
The product centrifugation arrived deionized water and washing with alcohol, then dry 8h at 70 DEG C in thermostatic drying chamber, final
To SnS2Nanometer sheet.The 70wt.%SnS that will be obtained2The sodium carboxymethyl cellulose of material, the acetylene black of 15wt.% and 15wt.%
Mix homogeneously, makes slurry, is coated uniformly on Copper Foil, is stamped into circular electrode pole piece after vacuum drying, is right with lithium metal
Electrode, 1mol L-1LiPF6(volume ratio is 1 to/EC+DEC+DMC:1:1) it is electrolyte, Celgard 2400 is barrier film, is assembled into
Button cell.Battery is carried out with ladder high rate performance test, charging/discharging voltage scope is 0.01～3.0V, result shows：?
0.1A g-1Electric current density under, reversible specific capacity be 850mAh g-1；In 2A g-1High current density under, reversible specific capacity is
505mAh g-1.
Embodiment 3：
Weigh 0.5g Tin tetrachloride pentahydrate, be dissolved in 80mL deionized water, stir formation settled solution；
Weigh 0.3g ethyl mercaptan to add in solution, stir.Then weigh 0.25g polyethylene glycol 6000 and add in above-mentioned solution,
Finally the settled solution obtaining is poured into 100mL and carry in teflon-lined water heating kettle, react 24h at 170 DEG C.Will
The product centrifugation obtaining deionized water and washing with alcohol, then dry 8h at 70 DEG C in thermostatic drying chamber, finally
Obtain SnS2Nanometer sheet.The 70wt.%SnS that will be obtained2The carboxymethyl cellulose of material, the acetylene black of 15wt.% and 15wt.%
Sodium mix homogeneously, makes slurry, is coated uniformly on Copper Foil, is stamped into circular electrode pole piece, with lithium metal is after vacuum drying
To electrode, 1mol L-1LiPF6(volume ratio is 1 to/EC+DEC+DMC:1:1) it is electrolyte, Celgard 2400 is barrier film, assembling
Become button cell.Battery is carried out with ladder high rate performance test, charging/discharging voltage scope is 0.01～3.0V, result shows：?
0.1A g-1Electric current density under, reversible specific capacity be 600mAh g-1；In 2A g-1High current density under, reversible specific capacity is
409mAh g-1.
Embodiment 4：
Weigh 0.2g Tin tetrachloride pentahydrate, be dissolved in 50mL deionized water, stir formation settled solution；
Weigh 0.4g thiourea to add in solution, stir.Then weigh 0.6g Macrogol 2000 and add in above-mentioned solution, finally
The settled solution obtaining is poured into 100mL and carries in teflon-lined water heating kettle, react 40h at 190 DEG C.To obtain
Product centrifugation and deionized water and washing with alcohol, then dry 8h at 70 DEG C in thermostatic drying chamber, finally give
SnS2Nanometer sheet.The 70wt.%SnS that will be obtained2The sodium carboxymethyl cellulose of material, the acetylene black of 15wt.% and 15wt.% mixes
Close uniformly, make slurry, be coated uniformly on Copper Foil, after vacuum drying, be stamped into circular electrode pole piece, be to electricity with lithium metal
Pole, 1mol L-1LiPF6(volume ratio is 1 to/EC+DEC+DMC:1:1) it is electrolyte, Celgard 2400 is barrier film, is assembled into knob
Button battery.Battery is carried out with ladder high rate performance test, charging/discharging voltage scope is 0.01～3.0V, result shows：In 0.1A
g-1Electric current density under, reversible specific capacity be 1000mAh g-1；In 2A g-1High current density under, reversible specific capacity is
750mAh g-1.
Embodiment 5：
Weigh 0.5g Tin tetrachloride pentahydrate, be dissolved in 80mL deionized water, stir formation settled solution；
Weigh 0.3g ethyl mercaptan to add in solution, stir.Then weigh 1g polyethylene glycol 6000 and add in above-mentioned solution, finally
The settled solution obtaining is poured into 100mL and carries in teflon-lined water heating kettle, react 24h at 170 DEG C.To obtain
Product centrifugation and deionized water and washing with alcohol, then dry 8h at 70 DEG C in thermostatic drying chamber, finally give
SnS2Nanometer sheet.The 70wt.%SnS that will be obtained2The sodium carboxymethyl cellulose of material, the acetylene black of 15wt.% and 15wt.% mixes
Close uniformly, make slurry, be coated uniformly on Copper Foil, after vacuum drying, be stamped into circular electrode pole piece, be to electricity with lithium metal
Pole, 1mol L-1LiPF6(volume ratio is 1 to/EC+DEC+DMC:1:1) it is electrolyte, Celgard 2400 is barrier film, is assembled into knob
Button battery.Battery is carried out with ladder high rate performance test, charging/discharging voltage scope is 0.01～3.0V, result shows：In 0.1A
g-1Electric current density under, reversible specific capacity be 950mAh g-1；In 2A g-1High current density under, reversible specific capacity is
705mAh g-1.
Claims (7)
1. a kind of SnS of (101) crystal face preferential growth2The preparation method of nanometer sheet negative material, is characterized in that using a step solvent
Full-boiled process simultaneously adds surfactant polyethylene, prepares the SnS with (101) crystal face as exposed surface2Nanometer sheet；Concrete technology
Step is：
(1) pink salt of certain mol proportion is dissolved in a certain amount of solvent, stir formation settled solution, the concentration control of pink salt
Make 1 × 10-4～3 × 10-2mol L-1；Added in settled solution from organic sulphur source, be stirred continuously and make organic sulphur source completely molten
Solution；Add surfactant polyethylene to stir, organic sulphur source concentration controls 4 × 10-4～4 × 10-1mol L-1,
Surfactant polyethylene concentration controls 2 × 10-3～5 × 10-1mol L-1；
(2) solution obtaining in step (1) is poured into in teflon-lined water heating kettle, a constant temperature in calorstat
Degree is lower to react certain time.
2. the SnS of (101) according to claim 1 crystal face preferential growth2The preparation method of nanometer sheet negative material, it is special
Levy and be：Pink salt described in step (1) be nitric acid stannum, stannic chloride, STANNOUS SULPHATE CRYSTALLINE or its crystallize hydrate.
3. the SnS of (101) according to claim 1 crystal face preferential growth2The preparation method of nanometer sheet negative material, it is special
Levy and be：Solvent described in step (1) is one or more of deionized water, dehydrated alcohol, propanol, methanol.
4. the SnS of (101) according to claim 1 crystal face preferential growth2The preparation method of nanometer sheet negative material, it is special
Levy and be：Organic sulphur source described in step (1) is ethyl mercaptan, propylene mercaptan, thiourea, L-Cysteine.
5. the SnS of (101) according to claim 1 crystal face preferential growth2The preparation method of nanometer sheet negative material, it is special
Levy and be：Polyethylene Glycol described in step (1) is polyethylene glycol 200, Macrogol 2000, polyethylene glycol 6000, poly- second two
One or more of alcohol 12000.
6. the SnS of (101) according to claim 1 crystal face preferential growth2The preparation method of nanometer sheet negative material, it is special
Levy and be：In step (2), the temperature of calorstat is 120～240 DEG C.
7. the SnS of (101) according to claim 1 crystal face preferential growth2The preparation method of nanometer sheet negative material, it is special
Levy and be：In step (2), the time of reaction is 10～40h.
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Cited By (6)
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| CN107275617A (en) * | 2017-07-05 | 2017-10-20 | 东莞中汽宏远汽车有限公司 | Compound lithium cell cathode material and preparation method thereof and cathode of lithium battery, lithium battery |
| CN109449397A (en) * | 2018-10-22 | 2019-03-08 | 北京科技大学 | A kind of composite negative pole material and preparation method thereof with excellent high rate performance |
| CN110034278A (en) * | 2018-01-12 | 2019-07-19 | 中南大学 | A kind of SnS2Film lithium cell cathode and its preparation and application |
| CN111268720A (en) * | 2020-01-13 | 2020-06-12 | 信阳师范学院 | Preparation method of large interlayer spacing tin disulfide nanoflower sodium ion battery negative electrode material |
| CN111871431A (en) * | 2020-08-27 | 2020-11-03 | 东北师范大学 | Tin disulfide/gold composite catalyst and preparation method and application thereof |
| CN113772718A (en) * | 2021-09-09 | 2021-12-10 | 西安建筑科技大学 | SnS-SnS2@ GO heterostructure composite material and preparation method and application thereof |
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| CN105800674A (en) * | 2016-03-23 | 2016-07-27 | 昆明理工大学 | Preparation method and application of tin sulfide material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107275617A (en) * | 2017-07-05 | 2017-10-20 | 东莞中汽宏远汽车有限公司 | Compound lithium cell cathode material and preparation method thereof and cathode of lithium battery, lithium battery |
| CN110034278A (en) * | 2018-01-12 | 2019-07-19 | 中南大学 | A kind of SnS2Film lithium cell cathode and its preparation and application |
| CN109449397A (en) * | 2018-10-22 | 2019-03-08 | 北京科技大学 | A kind of composite negative pole material and preparation method thereof with excellent high rate performance |
| CN111268720A (en) * | 2020-01-13 | 2020-06-12 | 信阳师范学院 | Preparation method of large interlayer spacing tin disulfide nanoflower sodium ion battery negative electrode material |
| CN111268720B (en) * | 2020-01-13 | 2022-07-01 | 信阳师范学院 | Preparation method of large interlayer spacing tin disulfide nanoflower sodium ion battery negative electrode material |
| CN111871431A (en) * | 2020-08-27 | 2020-11-03 | 东北师范大学 | Tin disulfide/gold composite catalyst and preparation method and application thereof |
| CN111871431B (en) * | 2020-08-27 | 2022-09-20 | 东北师范大学 | Tin disulfide/gold composite catalyst, and preparation method and application thereof |
| CN113772718A (en) * | 2021-09-09 | 2021-12-10 | 西安建筑科技大学 | SnS-SnS2@ GO heterostructure composite material and preparation method and application thereof |
| CN113772718B (en) * | 2021-09-09 | 2022-11-22 | 西安建筑科技大学 | SnS-SnS 2 @ GO heterostructure composite material and preparation method and application thereof |
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