CN107394129A - A kind of preparation method of stannic disulfide carbon nano-tube combination electrode material - Google Patents
A kind of preparation method of stannic disulfide carbon nano-tube combination electrode material Download PDFInfo
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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 kind of preparation method of stannic disulfide carbon nano-tube combination electrode material, step is:Step 1, a certain amount of functionalized multi-wall carbonnanotubes are added in a certain amount of absolute ethyl alcohol, 2.5~3.5h of ultrasonic disperse, obtain dispersion liquid A;Step 2, then weigh a certain amount of stannic chloride pentahydrate and be added to step 1 and obtain in dispersion liquid A, stir 10~30min, then under stirring, add a certain amount of thioacetamide, stir 30~40min, obtain solution B;Step 3, solution B step 2 obtained is transferred in the reactor with polytetrafluoroethyllining lining, at a certain temperature hydro-thermal reaction, and reaction naturally cools to room temperature after terminating, and obtains blackish green precipitation;Step 4, the blackish green precipitation that collection step 3 obtains, and then, be placed in vacuum drying chamber and dried, obtain stannic disulfide carbon nano-tube combination electrode material with deionized water, absolute ethyl alcohol centrifuge washing successively.Its preparation process is simple.
Description
Technical field
The invention belongs to electrode material preparation method technical field, is related to a kind of stannic disulfide-carbon nano-tube combination electrode
The preparation method of material.
Background technology
Environmental pollution and energy shortage problem getting worse, the eager needs of people find one kind efficiently, and cleaning is sustainable
New energy.The new energy devices such as lithium ion battery are because its energy density height, good cycling stability, long lifespan, cleaning are without dirt
Dye etc. many excellent specific properties and become the hot topic of research field.As the negative of one of the most important part of lithium ion battery
Pole active material turns into the key point of lithium ion battery development.Stannic disulfide is due to its higher lithium storage content (645mAh g-1) receive the extensive concern of battery material circle.
However, stannic disulfide can produce larger volumetric expansion as lithium ion battery negative material in charge and discharge process
The powder of detached of active material can be caused, and the electric conductivity of stannic disulfide is poor, causes the high rate performance of such material and follows
Ring stability, which is difficult to have, largely to be lifted.A kind of current most common raising lithium ion battery tinbase sulfide negative pole material
The method of material cyclical stability is compound with carbon material, and CNT is due to its one-dimensional tubular structure, electric conductivity height, specific surface area
The advantages that high, is as compound preferable carbon source.
Yurong Ren etc. are emphasized using thiocarbamide as sulphur source, and sodium-ion battery is prepared with flower-shaped using hydro-thermal method using water as solvent
SnS2/ CNTs combination electrodes, obtain stable high rate performance (Three-dimensional SnS2flowers/carbon
nanotubes network:Extraordinary rate capacity for sodium-ion battery,
Materials Letters,2017,186:57-61).Chinese invention patent《A kind of sodium-ion battery prepares SnS with situ2/
The method of CNTs negative materials》(application number:201610595712.1 publication number:CN106058198A) using water as solvent, with two
Water stannous chloride is raw material, prepares sodium-ion battery SnS2/ CNTs negative materials, there are preferable capacity and high rate performance.
Hongyu Sun etc. emphasize to prepare SnS by solvent of water2Nanometer sheet modifying multiwall carbon nano-tube cathode material of lithium ion battery,
It can still reach 510mAh g after 50 circulations-1Reversible capacity (SnS2nanoflakes decorated
multiwalled carbon nanotubes as high performance anode materials for lithium-
ion batteries,Materials Research Bulletin,2014,49:319-324).Chuanxin Zhai etc. are strong
After adjusting the effective kayexalate of multi-wall carbon nano-tube and diallyl dimethyl ammoniumchloride processing, added using water as solvent few
The hydrochloric acid of amount prepares SnS using ultrasonic method2NS@MWCNTs composites, its cycle performance and high rate performance for having had
(Multiwalled Carbon Nanotubes Anchored with SnS2Nanosheets as High-
Performance Anode Materials of Lithium-Ion Batteries,ACS
Appl.Mater.Interfaces,2011,3:4067-4074).Although being greatly promoted with CNT composite electrochemical performance,
But many templates are added in preparation process, dispersant, make preparation process relatively complicated.Therefore, a kind of preparation process is developed
Simply, without adding other reagents, and can be with Effective Regulation stannic disulfide-carbon nano tube compound material structure and the method for performance
Have great importance.
The content of the invention
It is an object of the invention to provide a kind of preparation method of stannic disulfide-carbon nano-tube combination electrode material, and it is prepared
Process is simple.
The technical solution adopted in the present invention is a kind of preparation method of stannic disulfide-carbon nano-tube combination electrode material,
Implement according to following steps:
Step 1, a certain amount of functionalized multi-wall carbonnanotubes are added in a certain amount of absolute ethyl alcohol, ultrasonic disperse
2.5~3.5h, obtain dispersion liquid A;
Step 2, then weigh a certain amount of stannic chloride pentahydrate and be added to step 1 and obtain in dispersion liquid A, stir 10~30min,
Then under stirring, a certain amount of thioacetamide is added, 30~40min is stirred, obtains solution B;
Step 3, solution B step 2 obtained is transferred in the reactor with polytetrafluoroethyllining lining, in certain temperature
Lower hydro-thermal reaction, reaction naturally cool to room temperature after terminating, obtain blackish green precipitation;
Step 4, the blackish green precipitation that collection step 3 obtains, and deionized water, absolute ethyl alcohol centrifuge washing are used successively, so
Afterwards, it is placed in vacuum drying chamber and dries, obtains stannic disulfide-carbon nano-tube combination electrode material.
The features of the present invention also resides in,
Quality-volumetric concentration of dispersion liquid A in step 1 is 0.5~1.5mg/mL.
The mass ratio of stannic chloride pentahydrate in step 2 and the functionalized multi-wall carbonnanotubes in step 1 is 5.5~18:
1;
The mass ratio of thioacetamide in step 2 and the functionalized multi-wall carbonnanotubes in step 1 is 5~15:1.
Hydrothermal temperature in step 3 is 160~200 DEG C, and the reaction time is 12~24h.
Vacuum drying drying temperature in step 4 is 60~80 DEG C, and drying time is 8~12h.
Stannic disulfide-carbon nano-tube combination electrode material of preparation is used as lithium ion battery negative material.
The diameter 30-50nm of stannic disulfide-carbon nano-tube combination electrode material, length are 10-30 μm.
The invention has the advantages that preparation method of the present invention is simple, it is suitable for mass producing, and made
The raw material such as stannic chloride pentahydrate and thioacetamide is easy to get, pollution-free, and without adding other reagents, solvent absolute ethyl alcohol
Not only dispersant can be done but also has certain acidity, there are certain regulation and control to reaction.Easy to operation furthermore this experimental period is short, energy consumption is low, pole
Has industrial prospect.Product size prepared by the present invention is homogeneous, regular appearance, and the introducing of CNT can be effectively
The reunion of stannic disulfide is hindered, improves the electrical conductivity of active material so that lithium ion battery is compound with curing tin-carbon nanometer tube
Negative material has more excellent cycle performance and high rate performance.
Brief description of the drawings
Fig. 1 is prepared by a kind of embodiment 1 of the preparation method of stannic disulfide-carbon nano-tube combination electrode material of the present invention
Stannic disulfide-carbon nano tube compound material X ray diffracting spectrum;
Fig. 2 is prepared by a kind of embodiment 2 of the preparation method of stannic disulfide-carbon nano-tube combination electrode material of the present invention
Stannic disulfide-carbon nano tube compound material transmission electron microscope photo;
Fig. 3 is prepared by a kind of embodiment 3 of the preparation method of stannic disulfide-carbon nano-tube combination electrode material of the present invention
Stannic disulfide-carbon nano tube compound material amplify 40000 times of electron scanning micrographs;
Fig. 4 is prepared by a kind of embodiment 3 of the preparation method of stannic disulfide-carbon nano-tube combination electrode material of the present invention
Stannic disulfide-carbon nano tube compound material amplify 20000 times of electron scanning micrographs;
Fig. 5 is prepared by a kind of embodiment 3 of the preparation method of stannic disulfide-carbon nano-tube combination electrode material of the present invention
Rate charge-discharge performance chart of the stannic disulfide-carbon nano tube compound material as negative material button cell;
Fig. 6 is prepared by a kind of embodiment 4 of the preparation method of stannic disulfide-carbon nano-tube combination electrode material of the present invention
Cyclical stability test chart of the stannic disulfide-carbon nano tube compound material as negative material button cell.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of preparation method of stannic disulfide-carbon nano-tube combination electrode material of the present invention, implements according to following steps:
Step 1, a certain amount of functionalized multi-wall carbonnanotubes are added in a certain amount of absolute ethyl alcohol, ultrasonic disperse
2.5~3.5h, dispersion liquid A is obtained, quality-volumetric concentration that dispersion liquid A is prepared is 0.5~1.5mg/mL;
Step 2, then weigh a certain amount of stannic chloride pentahydrate and be added to step 1 and obtain in dispersion liquid A, wherein, five water tetrachloros
The mass ratio for changing tin and functionalized multi-wall carbonnanotubes is 5.5~18:1,10~30min is stirred, then under stirring, is added
Enter a certain amount of thioacetamide, stir 30~40min, obtain solution B, wherein, thioacetamide and carboxylated multi-wall carbon nano-tube
The mass ratio of pipe is 5~15:1;
Step 3, solution B step 2 obtained is transferred in the reactor with polytetrafluoroethyllining lining, at 160~200 DEG C
12~24h of lower hydro-thermal reaction, reaction naturally cool to room temperature after terminating, obtain blackish green precipitation;
Step 4, the blackish green precipitation that collection step 3 obtains, and deionized water, absolute ethyl alcohol centrifuge washing are used successively, so
Afterwards, it is placed in vacuum drying chamber with 60~80 DEG C of dry 8~12h, obtains stannic disulfide-carbon nano-tube combination electrode material.
Stannic disulfide-carbon nano-tube combination electrode material of preparation is used as lithium ion battery negative material.
The diameter 30-50nm of stannic disulfide-carbon nano-tube combination electrode material, length are 10-30 μm.
Embodiment 1
Step 1,30mg functionalized multi-wall carbonnanotubes are added in 60mL absolute ethyl alcohols, after ultrasonic disperse 3h, obtained
Dispersion liquid A;
Step 2,0.53g stannic chloride pentahydrates are weighed to be added to obtain in dispersion liquid A, stir 20min, then in stirring shape
Under state, 0.45g thioacetamides are added, 30min is stirred, obtains solution B;
Step 3, resulting solution B is transferred in the reactor with polytetrafluoroethyllining lining, protected under the conditions of 160 DEG C
Warm 12h, reaction naturally cool to room temperature after terminating, obtain blackish green precipitation;
Step 4, collect blackish green precipitation and successively with deionized water, absolute ethyl alcohol centrifuge washing, be placed in 60 DEG C of vacuum and do
12h is dried in dry case, obtains lithium ion battery stannic disulfide-carbon nano-tube combination electrode material.
As shown in figure 1, for the XRD spectrum of stannic disulfide-carbon nano tube compound material prepared by embodiment 1, can from 1
To find out, all diffraction maximums in the XRD spectrum of composite are corresponding with the standard diffraction peak of stannic disulfide, in Fig. 1 not
There is the diffraction maximum of CNT, it may be possible to because the relative amount of CNT in composite is less.
Embodiment 2
Step 1,90mg functionalized multi-wall carbonnanotubes are added in 60mL absolute ethyl alcohols, after ultrasonic disperse 2.5h, obtained
To dispersion liquid A;
Step 2,0.53g stannic chloride pentahydrates are weighed to be added to obtain in dispersion liquid A, stir 10min, then in stirring shape
Under state, 0.45g thioacetamides are added, 35min is stirred, obtains solution B;
Step 3, resulting solution is transferred in the reactor with polytetrafluoroethyllining lining, passed under the conditions of 180 DEG C
Unite hydro-thermal 16h, and reaction naturally cools to room temperature after terminating, obtains blackish green precipitation;
Step 4, collect blackish green precipitation and successively with deionized water, absolute ethyl alcohol centrifuge washing, be placed in 80 DEG C of vacuum and do
8h is dried in dry case, obtains lithium ion battery stannic disulfide-carbon nano-tube combination electrode material.
As shown in Fig. 2 shone for the transmission electron microscope of stannic disulfide-carbon nano-tube combination electrode material prepared by embodiment 2
Piece, it is evident that there is the presence of sheet stannic disulfide CNT from figure, and composite diameter is about 30-
50nm。
Embodiment 3
Step 1,60mg functionalized multi-wall carbonnanotubes are added in 60mL absolute ethyl alcohols, after ultrasonic disperse 3.5h, obtained
To dispersion liquid A;
Step 2,0.53g stannic chloride pentahydrates are weighed to be added to obtain in dispersion liquid A, stir 20min, then in stirring shape
Under state, 0.45g thioacetamides are added, 30min is stirred, obtains solution B;
Step 3, resulting solution B is transferred in the reactor with polytetrafluoroethyllining lining, protected under the conditions of 180 DEG C
Warm 12h, reaction naturally cool to room temperature after terminating, obtain blackish green precipitation;
Step 4, collect blackish green precipitation and successively with deionized water, absolute ethyl alcohol centrifuge washing, be placed in 70 DEG C of vacuum and do
10h is dried in dry case, obtains lithium ion battery stannic disulfide-carbon nano-tube combination electrode material.
As shown in Figure 3-4, Fig. 3-4 is the scanning of stannic disulfide-carbon nano-tube combination electrode material prepared by embodiment 3
Electromicroscopic photograph, prepared stannic disulfide-carbon nano-tube combination electrode material size uniformity is can be seen that from Fig. 3 and Fig. 4,
Regular appearance, a diameter of 30-50nm, length are 10-30 μm.
As shown in figure 5, stannic disulfide-carbon nano tube compound materials of the Fig. 5 prepared by embodiment 3 is as negative material button
The rate charge-discharge performance chart of formula battery, from fig. 5, it is seen that be respectively 100,200,300,500 in current density,
1000mA g-1Under conditions of, CNTs@SnS2The specific discharge capacity of composite is respectively 580mAh g-1, 445mAh g-1,
380mAh g-1, 319mAh g-1, 268mAh g-1.And by being 100mA in current density after high current density discharge and recharge
g-1Under conditions of carry out discharge and recharge, CNTs@SnS2The specific discharge capacity of composite still can be maintained at 566mAh g-1。
Embodiment 4
Step 1,40mg functionalized multi-wall carbonnanotubes are added in 60mL absolute ethyl alcohols, after ultrasonic disperse 3h, obtained
Dispersion liquid A;
Step 2,0.35g stannic chloride pentahydrates are weighed to be added to obtain in dispersion liquid, stir 25min, then in stirring shape
Under state, 0.37g thioacetamides are added, 40min is stirred, obtains solution B;
Step 3, resulting solution B is transferred in the reactor with polytetrafluoroethyllining lining, protected under the conditions of 200 DEG C
Warm 24h, reaction naturally cool to room temperature after terminating, obtain blackish green precipitation;
Step 4, collect blackish green precipitation and successively with deionized water, absolute ethyl alcohol centrifuge washing, then, be placed in 75 DEG C very
10h is dried in empty drying box, obtains lithium ion battery stannic disulfide-carbon nano-tube combination electrode material.
As shown in fig. 6, stannic disulfide-carbon nano tube compound materials of the Fig. 6 prepared by embodiment 4 is as negative material button
The cyclical stability test chart of formula battery, it will be appreciated from fig. 6 that composite is 100mAg in current density-1During lower discharge and recharge, circulation
After 60 times, specific discharge capacity still can reach 530mAh g-1。
Embodiment 5
Step 1,50mg functionalized multi-wall carbonnanotubes are added in 60mL absolute ethyl alcohols, after ultrasonic disperse 3.5h, obtained
To dispersion liquid A;
Step 2,0.35g stannic chloride pentahydrates are weighed to be added to obtain in dispersion liquid, stir 30min, then in stirring shape
Under state, 0.45g thioacetamides are added, 30min is stirred, obtains solution B;
Step 3, resulting solution B is transferred in the reactor with polytetrafluoroethyllining lining, protected under the conditions of 160 DEG C
Warm 12h, reaction naturally cool to room temperature after terminating, obtain blackish green precipitation;
Step 4, blackish green precipitation is collected successively with deionized water, absolute ethyl alcohol centrifuge washing, is placed in 80 DEG C of vacuum drying
9h is dried in case, obtains lithium ion battery stannic disulfide-carbon nano-tube combination electrode material.
Embodiment 6
Step 1,80mg functionalized multi-wall carbonnanotubes are added in 60mL absolute ethyl alcohols, after ultrasonic disperse 2.8h, obtained
To dispersion liquid A;
Step 2,0.72g stannic chloride pentahydrates are weighed to be added to obtain in dispersion liquid, stir 20min, then in stirring shape
Under state, 0.6g thioacetamides are added, 40min is stirred, obtains solution B;
Step 3, resulting solution B is transferred in the reactor with polytetrafluoroethyllining lining, passed under the conditions of 200 DEG C
Unite hydro-thermal 12h, and reaction naturally cools to room temperature after terminating, obtains blackish green precipitation;
Step 4, collect blackish green precipitation and successively with deionized water, absolute ethyl alcohol centrifuge washing, be placed in 60 DEG C of vacuum and do
12h is dried in dry case, obtains lithium ion battery stannic disulfide-carbon nano-tube combination electrode material.
Embodiment 7
Step 1,70mg functionalized multi-wall carbonnanotubes are added in 60mL absolute ethyl alcohols, after ultrasonic disperse 3h, obtained
Dispersion liquid A;
Step 2,0.7g stannic chloride pentahydrates are weighed to be added to obtain in dispersion liquid, 25min are stirred, then in stirring
Under, 0.9g thioacetamides are added, 35min is stirred, obtains solution B;
Step 3, resulting solution B is transferred in the reactor with polytetrafluoroethyllining lining, passed under the conditions of 180 DEG C
Unite hydro-thermal 18h, and reaction naturally cools to room temperature after terminating, obtains blackish green precipitation;
Step 4, collect blackish green precipitation and successively with deionized water, absolute ethyl alcohol centrifuge washing, be placed in 65 DEG C of vacuum and do
11h is dried in dry case, obtains lithium ion battery stannic disulfide-carbon nano-tube combination electrode material.
Embodiment 8
Step 1,60mg functionalized multi-wall carbonnanotubes are added in 60mL absolute ethyl alcohols, after ultrasonic disperse 3.2h, obtained
To dispersion liquid;
Step 2,0.35g stannic chloride pentahydrates are weighed to be added to obtain in dispersion liquid A, stir 20min, then in stirring shape
Under state, 0.37g thioacetamides are added, 35min is stirred, obtains solution B;
Step 3, resulting solution B is transferred in the reactor with polytetrafluoroethyllining lining, passed under the conditions of 180 DEG C
Unite hydro-thermal 24h, and reaction naturally cools to room temperature after terminating, obtains blackish green precipitation;
Step 4, collect blackish green precipitation and successively with deionized water, absolute ethyl alcohol centrifuge washing, be placed in 75 DEG C of vacuum and do
11h is dried in dry case, obtains lithium ion battery stannic disulfide-carbon nano-tube combination electrode material.
Embodiment 9
Step 1,60mg functionalized multi-wall carbonnanotubes are added in 60mL absolute ethyl alcohols, after ultrasonic disperse 3.2h, obtained
To dispersion liquid;
Step 2,0.33g stannic chloride pentahydrates are weighed to be added to obtain in dispersion liquid A, stir 20min, then in stirring shape
Under state, 0.37g thioacetamides are added, 35min is stirred, obtains solution B;
Step 3, resulting solution B is transferred in the reactor with polytetrafluoroethyllining lining, passed under the conditions of 180 DEG C
Unite hydro-thermal 24h, and reaction naturally cools to room temperature after terminating, obtains blackish green precipitation;
Step 4, collect blackish green precipitation and successively with deionized water, absolute ethyl alcohol centrifuge washing, be placed in 75 DEG C of vacuum and do
11h is dried in dry case, obtains lithium ion battery stannic disulfide-carbon nano-tube combination electrode material.
Embodiment 10
Step 1,30mg functionalized multi-wall carbonnanotubes are added in 60mL absolute ethyl alcohols, after ultrasonic disperse 3h, obtained
Dispersion liquid A;
Step 2,0.54g stannic chloride pentahydrates are weighed to be added to obtain in dispersion liquid A, stir 20min, then in stirring shape
Under state, 0.45g thioacetamides are added, 30min is stirred, obtains solution B;
Step 3, resulting solution B is transferred in the reactor with polytetrafluoroethyllining lining, protected under the conditions of 160 DEG C
Warm 12h, reaction naturally cool to room temperature after terminating, obtain blackish green precipitation;
Step 4, collect blackish green precipitation and successively with deionized water, absolute ethyl alcohol centrifuge washing, be placed in 60 DEG C of vacuum and do
12h is dried in dry case, obtains lithium ion battery stannic disulfide-carbon nano-tube combination electrode material.
Claims (8)
1. a kind of preparation method of stannic disulfide-carbon nano-tube combination electrode material, it is characterised in that real according to following steps
Apply:
Step 1, a certain amount of functionalized multi-wall carbonnanotubes are added in a certain amount of absolute ethyl alcohol, ultrasonic disperse 2.5~
3.5h, obtain dispersion liquid A;
Step 2, then weigh a certain amount of stannic chloride pentahydrate and be added to step 1 and obtain in dispersion liquid A, stir 10~30min, then
Under stirring, a certain amount of thioacetamide is added, 30~40min is stirred, obtains solution B;
Step 3, solution B step 2 obtained is transferred in the reactor with polytetrafluoroethyllining lining, at a certain temperature water
Thermal response, reaction naturally cool to room temperature after terminating, obtain blackish green precipitation;
Step 4, the blackish green precipitation that collection step 3 obtains, and then, put with deionized water, absolute ethyl alcohol centrifuge washing successively
Dried in vacuum drying chamber, obtain stannic disulfide-carbon nano-tube combination electrode material.
2. a kind of preparation method of stannic disulfide-carbon nano-tube combination electrode material according to claim 1, its feature exist
In quality-volumetric concentration of the dispersion liquid A described in step 1 is 0.5~1.5mg/mL.
3. a kind of preparation method of stannic disulfide-carbon nano-tube combination electrode material according to claim 2, its feature exist
In, stannic chloride pentahydrate described in step 2 and the functionalized multi-wall carbonnanotubes described in step 1 mass ratio for 5.5~
18:1.
4. a kind of preparation method of stannic disulfide-carbon nano-tube combination electrode material according to claim 2, its feature exist
In the mass ratio of the thioacetamide described in step 2 and the functionalized multi-wall carbonnanotubes described in step 1 is 5~15:1.
5. a kind of preparation method of stannic disulfide-carbon nano-tube combination electrode material according to claim 1, its feature exist
In the hydrothermal temperature described in step 3 is 160~200 DEG C, and the reaction time is 12~24h.
6. a kind of preparation method of stannic disulfide-carbon nano-tube combination electrode material according to claim 1, its feature exist
In the vacuum drying drying temperature described in step 4 is 60~80 DEG C, and drying time is 8~12h.
7. a kind of preparation method of stannic disulfide-carbon nano-tube combination electrode material according to claim 1, its feature exist
In stannic disulfide-carbon nano-tube combination electrode material of preparation is used as lithium ion battery negative material.
8. a kind of preparation method of stannic disulfide-carbon nano-tube combination electrode material according to claim 7, its feature exist
In the diameter 30-50nm of the stannic disulfide-carbon nano-tube combination electrode material, length is 10-30 μm.
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CN114695854A (en) * | 2022-03-23 | 2022-07-01 | 西安建筑科技大学 | CNTs-SnS-SnS2@ GO heterostructure composite material and preparation method and application thereof |
CN116099551A (en) * | 2023-02-07 | 2023-05-12 | 昆明理工大学 | Preparation method and application of carbon nano tube composite material |
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