CN106784598A - A kind of used as negative electrode of Li-ion battery flake SnSe2Nanocrystalline preparation method - Google Patents
A kind of used as negative electrode of Li-ion battery flake SnSe2Nanocrystalline preparation method Download PDFInfo
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- CN106784598A CN106784598A CN201611180184.XA CN201611180184A CN106784598A CN 106784598 A CN106784598 A CN 106784598A CN 201611180184 A CN201611180184 A CN 201611180184A CN 106784598 A CN106784598 A CN 106784598A
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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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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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Abstract
The present invention relates to a kind of used as negative electrode of Li-ion battery flake SnSe2Nanocrystalline preparation method, this method is by a certain amount of SnCl2·2H2O is added in deionized water, and stirring to form solution A to being completely dissolved；A certain amount of selenium powder is weighed again, is added in hydrazine hydrate, stirring to formation claret solution B；Solution B is added dropwise to again form mixed solution in solution A, then mixed solution is transferred to and is incubated 2~12h in high pressure water heating kettle at 200~240 DEG C, final collection pelleting centrifugation water and ethanol cyclic washing obtain the SnSe of the flaky texture of pure phase2It is nanocrystalline, charge/discharge capacity and preferable cyclical stability higher is shown as lithium ion battery negative material using it.Present invention process is simple, short preparation period, and repeatability is high, meets demand prepared by large-scale production.
Description
【Technical field】
SnSe is prepared the present invention relates to a kind of hydro-thermal method2A kind of nanocrystalline method, and in particular to lithium ion battery negative
Use laminar SnSe2Nanocrystalline preparation method.
【Background technology】
At present, due to the extensive use of lithium ion battery, the exploitation of lithium ion battery negative material also turns into study hotspot.
Especially tin base cathode material, because tin base cathode not only has theoretical capacity higher, and is easy to and the Vth main group
The element of element and the VIth main group forms the alloy cpd of two-phase.In recent years, for SnSb, Sn3P4、SnO2、SnS2Deng tin
The report of alloy cpd is relatively more, but for SnSe2Report it is fewer.SnSe2Be the layer structure of hexagonal phase, layer with
Combination between layer is weaker, is conducive to the insertion and abjection of lithium ion, has larger development space as negative material.But
It is by SnSe2Negative material is applied in practice, and its chemical property need further raising.
The method of most common lifting chemical property is exactly the electrode material for preparing nano-scale, because nano material can
To shorten the diffusion path of lithium ion, increase and the contact area of electrolyte, the high rate performance of lithium ion battery is greatly improved.But
Again with some problems while being nanosizing, nanosizing makes material have specific surface energy high, forms thicker SEI
Film, and be susceptible to reunite, this have impact on the chemical property of electrode material again to a certain extent.According to the literature, make
The electrode material of standby two-dimensional sheet structure is equally beneficial for the lifting of chemical property, because the expansion of lithium ion in a thickness direction
Scattered path is shorter, and is not easy to reunite.But it is fewer for the report of this aspect at present.Xing Zhou etc. with
SnI2As raw material, SnSe is prepared for using electrochemical deposition method2Laminated structure, and have studied its photodetection performance (Xing
Zhou,Lin Gan et.al,Ultrathin SnSe2Flakes Grown by Chemical Vapor Deposition
for High-Performance Photodetectors,Adv.Mater.2015,27,8035–8041)。Gi Dae Park
Deng with SeO2And SnO2It is raw material, SnSe nanometer sheets is prepared for using spray pyrolysis, is showed as anode material of lithium-ion battery
Preferable chemical property (Gi Dae Park, Jong-Heun Lee et.al, Superior Na-Ion Storage are gone out
Properties of High Aspect Ratio SnSe Nanoplates Prepared by Spray Pyrolysis
Process,2016,DOI:10.1039/C6NR02983C).Yang Huanghao etc. dissolves ultrasound using selenium powder as raw material in concentrated base
Precipitation has prepared the selenizing tin material of sheet, but product uneven (Yang Huanghao, Zhang Xiaolong etc., a kind of stannic selenide nanometer material
Material and its preparation method and application, China Patent No.：201510114830.1).Therefore, prepared using a kind of simple method equal
The stannic selenide of even flaky texture has scientific meaning very much.
【The content of the invention】
SnSe is prepared it is an object of the invention to provide a kind of hydro-thermal method2Nanocrystalline method, prepared SnSe2Nanometer
Crystalline substance is a kind of flake structure of pure phase.
To reach above-mentioned purpose, present invention employs following technical scheme：
A kind of used as negative electrode of Li-ion battery flake SnSe2Nanocrystalline preparation method, comprises the following steps：
1) take inorganic tin salts to be added in deionized water, stirring to form solution A to being completely dissolved；Selenium powder is weighed, is added to
In hydrazine hydrate, stirring to form claret solution B to being completely dissolved；Then solution B is added dropwise to be formed in solution A and mixes molten
Liquid C, and stir；Wherein, tin ion and the mol ratio of selenium atom are 1：(1~4)；
2) above-mentioned mixed liquor C is transferred in water heating kettle, water heating kettle is then placed in hydro-thermal reaction instrument in 200~240 DEG C
Reaction, reaction cools to room temperature with the furnace after terminating, and is then washed respectively with deionized water and absolute ethyl alcohol, is centrifuged and obtains black
Powder, SnSe is obtained by isolated powder drying2It is nanocrystalline.
Step 1) in, described inorganic tin salts are SnCl2·2H2O, SnCl2·2H2O concentration in aqueous is
0.0033~0.167molL-1。
Step 1) in, it is magnetic agitation to stir, and mixing speed is 400~600r/min, 10~30min of mixing time.
Step 1) it is specially：By 0.0226~2.256 part of SnCl2·2H2O is added in 30~60mL deionized waters, stirring
To SnCl2·2H2O is completely dissolved to form solution A；0.0158~1.579 part of selenium powder is weighed, is added in 10~20mL hydrazine hydrates,
Stirring extremely forms claret solution B；Then solution B is added dropwise to form mixed solution C in solution A.
Step 2) in, the compactedness of the water heating kettle is controlled 40~80%.
Described SnSe2Nanocrystalline is a kind of flake structure, and the size of thin slice is 6~10 μm, and thickness is 30~50nm.
Relative to prior art, beneficial effects of the present invention are embodied in：
The present invention using water as solvent, with SnCl2·2H2, used as Xi Yuan, used as selenium source, hydrazine hydrate is used as reduction for selenium powder for O
Agent, SnSe is prepared for using one step hydro thermal method2Nano flake, size of the thin slice on thickness is about 30~50nm, and this is significantly
The diffusion path of lithium ion is shortened, the contact surface with electrolyte is increased, is conducive to improving SnSe2It is negative as lithium ion battery
The chemical property of pole material.Preparation method of the present invention is simple, and experimental repeatability is high, cycle is short, is adapted to extensive
The need for prepared by production, there is significant scientific meaning in terms of lithium ion battery applications.Present invention process is simple, manufacturing cycle
Short, repeatability is high, meets demand prepared by large-scale production.
SnSe prepared by the present invention2Nano flake, size of the thin slice on thickness is about 30~50nm, and this is greatly shortened
The diffusion path of lithium ion, increases the contact surface with electrolyte, is conducive to improving SnSe2As lithium ion battery negative material
The chemical property of material.
【Brief description of the drawings】
Fig. 1 is the SnSe prepared by embodiment 42Nanocrystalline X-ray diffraction (XRD) collection of illustrative plates；
Fig. 2 is the SnSe prepared by embodiment 42Nanocrystalline ESEM (SEM) photo；
Fig. 3 is the SnSe prepared by embodiment 42Nanocrystalline high rate performance figure, wherein, Cycle number：Circulation time
Number；Capacity：Capacity.
【Specific embodiment】
The present invention is elaborated with reference to the accompanying drawings and examples.
1) in parts by weight, by 0.0226~2.256 part of SnCl2·2H2O is added in 30~60mL deionized waters, is stirred
Mix to SnCl2·2H2O forms solution A；0.0158~1.579 part of selenium powder is weighed, is added in 10~20mL hydrazine hydrates, stirring is extremely
It is completely dissolved to form claret solution B；Then solution B is added dropwise to form mixed solution C in solution A, is placed in magnetic force
10~30min is stirred with the speed of 400~600r/min on mixer.SnCl2·2H2O concentration in aqueous is 0.0017
~0.33molL-1。SnCl2·2H2O is 1 with the mol ratio of selenium powder：(1~4)；
2) above-mentioned mixed liquor C is transferred in 100mL polytetrafluoroethylene (PTFE) water heating kettles, the compactedness control of the water heating kettle exists
40~80%.Then polytetrafluoroethylene (PTFE) water heating kettle is placed in hydro-thermal reaction instrument and reacts 6~24h in 200~240 DEG C, reaction terminates
After cool to room temperature with the furnace, then, wash 3~6 times respectively with deionized water and absolute ethyl alcohol and be centrifuged and obtain the powder of black, will
Isolated powder drying obtains SnSe2It is nanocrystalline.
Prepared SnSe2Nanocrystalline is a kind of flake structure, and the size of piece is about 6~10 μm, thickness is about 30~
50nm。
Embodiment 1
1) by 0.2256g SnCl2·2H2O is added in 30mL deionized waters, stirring to SnCl2·2H2O is completely dissolved
Form solution A；0.079g selenium powders are weighed, is added in 10mL hydrazine hydrates, stirring to formation claret solution B；Then by solution B
It is added dropwise to form mixed solution C in solution A, is placed on magnetic stirrer stirring 10min with the speed of 500r/min.
2) above-mentioned mixed liquor C is transferred in 100mL polytetrafluoroethylene (PTFE) water heating kettles, then puts polytetrafluoroethylene (PTFE) water heating kettle
12h is reacted in 200 DEG C in hydro-thermal reaction instrument, reaction cools to room temperature with the furnace after terminating, then, with deionized water and absolute ethyl alcohol
Wash respectively 3 times and the powder for obtaining black is centrifuged, isolated powder drying is obtained into SnSe2It is nanocrystalline.
Embodiment 2
1) by 0.4512g SnCl2·2H2O is added in 50mL deionized waters, stirring to SnCl2·2H2O is completely dissolved
Form solution A；0.158g selenium powders are weighed, is added in 20mL hydrazine hydrates, stirring to formation claret solution B；Then by solution B
It is added dropwise to form mixed solution C in solution A, is placed on magnetic stirrer stirring 30min with the speed of 500r/min.
2) above-mentioned mixed liquor C is transferred in 100mL polytetrafluoroethylene (PTFE) water heating kettles, then puts polytetrafluoroethylene (PTFE) water heating kettle
8h is reacted in 220 DEG C in hydro-thermal reaction instrument, reaction cools to room temperature with the furnace after terminating, then, with deionized water and absolute ethyl alcohol
Wash respectively 3 times and the powder for obtaining black is centrifuged, isolated powder drying is obtained into SnSe2It is nanocrystalline.
Embodiment 3
1) by 0.9024g SnCl2·2H2O is added in 60mL deionized waters, stirring to SnCl2·2H2O is completely dissolved
Form solution A；0.316g selenium powders are weighed, is added in 15mL hydrazine hydrates, stirring to formation claret solution B；Then by solution B
It is added dropwise to form mixed solution C in solution A, is placed on magnetic stirrer stirring 25min with the speed of 500r/min.
2) above-mentioned mixed liquor C is transferred in 100mL polytetrafluoroethylene (PTFE) water heating kettles, then puts polytetrafluoroethylene (PTFE) water heating kettle
12h is reacted in 220 DEG C in hydro-thermal reaction instrument, reaction cools to room temperature with the furnace after terminating, then, with deionized water and absolute ethyl alcohol
Wash respectively 3 times and the powder for obtaining black is centrifuged, isolated powder drying is obtained into SnSe2It is nanocrystalline.
Embodiment 4
1) by 0.4512g SnCl2·2H2O is added in 60mL deionized waters, stirring to SnCl2·2H2O is completely dissolved
Form solution A；0.158g selenium powders are weighed, is added in 15mL hydrazine hydrates, stirring to formation claret solution B；Then by solution B
It is added dropwise to form mixed solution C in solution A, is placed on magnetic stirrer stirring 20min with the speed of 500r/min.
2) above-mentioned mixed liquor C is transferred in 100mL polytetrafluoroethylene (PTFE) water heating kettles, then puts polytetrafluoroethylene (PTFE) water heating kettle
8h is reacted in 240 DEG C in hydro-thermal reaction instrument, reaction cools to room temperature with the furnace after terminating, then, with deionized water and absolute ethyl alcohol
Wash respectively 3 times and the powder for obtaining black is centrifuged, isolated powder drying is obtained into SnSe2It is nanocrystalline.
3) sample (SnSe is analyzed with Rigaku D/max2000PCX- x ray diffractometer xs2It is nanocrystalline), find sample with
JCPDS numberings are the SnSe of the hexagonal crystal system of 89-31972Structure is consistent, and crystal grows along (001) high preferred orientation.Will
The sample is observed with field emission scanning electron microscope (FESEM), it can be seen that prepared SnSe2Nanocrystalline is one kind
Flake structure, the big or small slice of piece is about 6~10 μm, and thickness is about 30~50nm.With the SnSe of laminated structure2Nanocrystalline conduct is born
Pole, is assembled into lithium ion battery, and flake SnSe is found using the chemical property of BTS charging/discharging apparatus test battery2Nanometer
Crystalline substance has reversible capacity higher, in 100mA g-1Current density under circulation 30 circle after reversible capacity be about 700mAh g-1
Show preferable chemical property.
Embodiment 5
1) by 0.2256g SnCl2·2H2O is added in 30mL deionized waters, stirring to SnCl2·2H2O is completely dissolved
Form solution A；0.079g selenium powders are weighed, is added in 20mL hydrazine hydrates, stirring to formation claret solution B；Then by solution B
It is added dropwise to form mixed solution C in solution A, is placed on magnetic stirrer stirring 15min with the speed of 500r/min.
2) above-mentioned mixed liquor C is transferred in 100mL polytetrafluoroethylene (PTFE) water heating kettles, then puts polytetrafluoroethylene (PTFE) water heating kettle
12h is reacted in 230 DEG C in hydro-thermal reaction instrument, reaction cools to room temperature with the furnace after terminating, then, with deionized water and absolute ethyl alcohol
Wash respectively 3 times and the powder for obtaining black is centrifuged, isolated powder drying is obtained into SnSe2It is nanocrystalline.
Embodiment 6
1) by 2.256g SnCl2·2H2O is added in 60mL deionized waters, stirring to SnCl2·2H2O forms solution A；
1.579g selenium powders are weighed, is added in 20mL hydrazine hydrates, stirring to form claret solution B to being completely dissolved；Then by solution B by
It is added dropwise in solution A and forms mixed solution C, is placed on magnetic stirrer stirring 30min with the speed of 400r/min.
SnCl2·2H2O concentration in aqueous is 0.167molL-1。
2) above-mentioned mixed liquor C is transferred in 100mL polytetrafluoroethylene (PTFE) water heating kettles, the compactedness control of the water heating kettle exists
80%.Then polytetrafluoroethylene (PTFE) water heating kettle is placed in hydro-thermal reaction instrument and 12h is reacted in 240 DEG C, reaction is cooled to the furnace after terminating
Room temperature, then, washs the powder that 3 centrifugations obtain black, by isolated powder respectively with deionized water and absolute ethyl alcohol
Drying obtains SnSe2It is nanocrystalline.
Prepared SnSe2Nanocrystalline is a kind of flake structure, and the size of piece is about 6~10 μm, thickness is about 30~
50nm。
Embodiment 7
1) by 0.0226g SnCl2·2H2O is added in 30mL deionized waters, stirring to SnCl2·2H2O forms solution
A；0.0158g selenium powders are weighed, is added in 10mL hydrazine hydrates, stirring to form claret solution B to being completely dissolved；Then by solution
B is added dropwise to form mixed solution C in solution A, is placed on magnetic stirrer stirring 10min with the speed of 600r/min.
SnCl2·2H2O concentration in aqueous is 0.0033molL-1。
2) above-mentioned mixed liquor C is transferred in 100mL polytetrafluoroethylene (PTFE) water heating kettles, the compactedness control of the water heating kettle exists
40%.Then polytetrafluoroethylene (PTFE) water heating kettle is placed in hydro-thermal reaction instrument and 6h is reacted in 200 DEG C, reaction cools to room with the furnace after terminating
Temperature, then, the powder that 6 centrifugations obtain black is washed with deionized water and absolute ethyl alcohol respectively, and isolated powder is dried
It is dry to obtain SnSe2It is nanocrystalline.
Prepared SnSe2Nanocrystalline is a kind of flake structure, and the size of piece is about 6~10 μm, thickness is about 30~
50nm。
In a word, the present invention is prepared for laminar SnSe using water as solvent using simple hydro-thermal method2It is nanocrystalline, should
Nanometer sheet thickness about 30~50nm, because the migration path of lithium ion in a thickness direction is shorter, therefore it is used as lithium ion battery
Negative material has capacity higher, 100mA g-1Current density under after the circle of circulation 30 capacity up to about 700mAh g-1Body
Reveal preferable cyclical stability, this performance is adapted to practical application.And preparation method of the invention is simple, and experimental temperature is low,
Repeated high, thermal and hydric environment can realize nanocrystalline controlledly synthesis, with certain scientific meaning.
Claims (6)
1. a kind of used as negative electrode of Li-ion battery flake SnSe2Nanocrystalline preparation method, it is characterised in that：Comprise the following steps：
1) take inorganic tin salts to be added in deionized water, stirring to form solution A to being completely dissolved；Selenium powder is weighed, hydration is added to
In hydrazine, stirring to form claret solution B to being completely dissolved；Then solution B is added dropwise to form mixed solution C in solution A,
And stir；Wherein, tin ion and the mol ratio of selenium atom are 1：(1~4)；
2) above-mentioned mixed liquor C is transferred in water heating kettle, water heating kettle then is placed in into hydro-thermal reaction instrument reacts in 200~240 DEG C,
Reaction cools to room temperature with the furnace after terminating, and is then washed respectively with deionized water and absolute ethyl alcohol, the powder for obtaining black is centrifuged,
Isolated powder drying is obtained into SnSe2It is nanocrystalline.
2. a kind of used as negative electrode of Li-ion battery flake SnSe according to claim 12Nanocrystalline preparation method, its feature
It is：Step 1) in, described inorganic tin salts are SnCl2·2H2O, SnCl2·2H2O concentration in aqueous is 0.0033
~0.167molL-1。
3. a kind of used as negative electrode of Li-ion battery flake SnSe according to claim 12Nanocrystalline preparation method, its feature
It is：Step 1) in, it is magnetic agitation to stir, and mixing speed is 400~600r/min, 10~30min of mixing time.
4. a kind of used as negative electrode of Li-ion battery flake SnSe according to claim 12Nanocrystalline preparation method, its feature
It is：According to parts by weight, step 1) it is specially：By 0.0226~2.256 part of SnCl2·2H2O be added to 30~60mL go from
In sub- water, stirring to SnCl2·2H2O is completely dissolved to form solution A；0.0158~1.579 part of selenium powder is weighed, it is added to 10~
In 20mL hydrazine hydrates, stirring to formation claret solution B；Then solution B is added dropwise to form mixed solution C in solution A.
5. a kind of used as negative electrode of Li-ion battery flake SnSe according to claim 12Nanocrystalline preparation method, its feature
It is：Step 2) in, the compactedness of the water heating kettle is controlled 40~80%.
6. a kind of used as negative electrode of Li-ion battery flake SnSe according to claim 12Nanocrystalline preparation method, its feature
It is：Described SnSe2Nanocrystalline is a kind of flake structure, and the size of thin slice is 6~10 μm, and thickness is 30~50nm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601441A (en) * | 2017-10-10 | 2018-01-19 | 陕西科技大学 | A kind of method of hydro-thermal method synthesis stannic selenide micron crystalline flour body |
| CN107706404A (en) * | 2017-11-23 | 2018-02-16 | 东北师范大学 | A kind of selenium cladding tin ash/graphene nanocomposite material prepares and its application |
| CN107934924A (en) * | 2017-11-17 | 2018-04-20 | 陕西科技大学 | A kind of Hydrothermal preparation method for controlling laminated structure stannic selenide thickness |
| CN108588838A (en) * | 2018-03-23 | 2018-09-28 | 桂林电子科技大学 | A method of preparing the SnSe polycrystalline bulks with high thermoelectricity capability |
| CN108695510A (en) * | 2018-07-07 | 2018-10-23 | 苏州思创源博电子科技有限公司 | A kind of preparation method of stannic selenide composite negative pole material |
| CN108807987A (en) * | 2018-07-07 | 2018-11-13 | 苏州思创源博电子科技有限公司 | A kind of preparation method of carbon coating selenizing tin negative pole material |
| CN113005328A (en) * | 2021-02-23 | 2021-06-22 | 西安航空学院 | Tin-selenium-sulfur ternary alloy cathode material for sodium ion battery and preparation method and application thereof |
| CN113200565A (en) * | 2021-05-08 | 2021-08-03 | 湖南工学院 | Flaky tin disulfide and preparation method and application thereof |
-
2016
- 2016-12-19 CN CN201611180184.XA patent/CN106784598A/en active Pending
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| 彭红瑞等: "SnSe2纳米片的制备及结构表征", 《青岛科技大学学报》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601441A (en) * | 2017-10-10 | 2018-01-19 | 陕西科技大学 | A kind of method of hydro-thermal method synthesis stannic selenide micron crystalline flour body |
| CN107934924A (en) * | 2017-11-17 | 2018-04-20 | 陕西科技大学 | A kind of Hydrothermal preparation method for controlling laminated structure stannic selenide thickness |
| CN107934924B (en) * | 2017-11-17 | 2020-06-05 | 陕西科技大学 | Hydrothermal preparation method for controlling thickness of tin selenide with sheet structure |
| CN107706404A (en) * | 2017-11-23 | 2018-02-16 | 东北师范大学 | A kind of selenium cladding tin ash/graphene nanocomposite material prepares and its application |
| CN107706404B (en) * | 2017-11-23 | 2020-04-21 | 东北师范大学 | Preparation and application of selenium-coated tin dioxide/graphene nanocomposite |
| CN108588838A (en) * | 2018-03-23 | 2018-09-28 | 桂林电子科技大学 | A method of preparing the SnSe polycrystalline bulks with high thermoelectricity capability |
| CN108588838B (en) * | 2018-03-23 | 2019-12-06 | 桂林电子科技大学 | method for preparing SnSe polycrystalline block with high thermoelectric performance |
| CN108695510A (en) * | 2018-07-07 | 2018-10-23 | 苏州思创源博电子科技有限公司 | A kind of preparation method of stannic selenide composite negative pole material |
| CN108807987A (en) * | 2018-07-07 | 2018-11-13 | 苏州思创源博电子科技有限公司 | A kind of preparation method of carbon coating selenizing tin negative pole material |
| CN113005328A (en) * | 2021-02-23 | 2021-06-22 | 西安航空学院 | Tin-selenium-sulfur ternary alloy cathode material for sodium ion battery and preparation method and application thereof |
| CN113005328B (en) * | 2021-02-23 | 2021-12-07 | 西安航空学院 | Tin-selenium-sulfur ternary alloy cathode material for sodium ion battery and preparation method and application thereof |
| CN113200565A (en) * | 2021-05-08 | 2021-08-03 | 湖南工学院 | Flaky tin disulfide and preparation method and application thereof |
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Application publication date: 20170531 |