CN105621355B - A kind of hollow plumbago alkene ball load nanometer stannic disulfide composite and preparation method thereof - Google Patents
A kind of hollow plumbago alkene ball load nanometer stannic disulfide composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of hollow plumbago alkene ball to load nanometer stannic disulfide composite, it is using the hollow plumbago alkene ball of submicron-scale as carrier, stannic disulfide nano particle is supported on the inner and outer wall of graphene hollow ball, the stannic disulfide particle size of hollow plumbago alkene ball surface is grown between 10 40 nm, its preparation method comprises the following steps：A. synthesizing cationic type polystyrene spheres：B. hollow plumbago alkene ball is synthesized：C. stannic disulfide is loaded：It can obtain the composite of hollow plumbago alkene ball load nanometer stannic disulfide.The composite is a kind of carbon material of two-dimensional structure, the volumetric expansion of stannic disulfide can be accommodated in charge and discharge process, improve the electric conductivity and structural stability of electrode material, and porous graphene structure can improve the electric conductivity and ion transmission performance of material, be advantageous to lithium ion insertion and abjection in the material.
Description
Technical field
The present invention relates to a kind of hollow plumbago alkene ball as lithium cell cathode material to load nanometer stannic disulfide composite wood
Material and preparation method thereof, belongs to electrochemistry and field of material synthesis technology.
Background technology
Lithium ion battery because with energy density it is high, have extended cycle life, memory-less effect many advantages, such as, it has also become it is current
The secondary cell that the world is most widely used.With further going deep into for Study on Li-ion batteries, high power capacity is developed, high power is forthright
Can, the battery material having extended cycle life turns into the emphasis in the field.At present, the negative material for being actually used in lithium ion battery is general
All it is carbon materials, such as graphite, soft carbon, hard carbon etc..Carbon negative pole material（The mAh/g of theoretical capacity 372）Future can not be met
The needs of high power capacity, various metal composites, metal oxide and metal sulfide are studied to be born instead of carbon by extensive
Pole.Stannic disulfide is due to relatively low embedding lithium voltage and higher theoretical capacity（645 m Ah/g）, it is constantly subjected in recent years
The extensive concern of research worker, but when stannic disulfide is as lithium ion battery negative material, it is the same with other tin-based materials,
The problem of lithium ion battery negative material is during embedding, de- lithium, volumetric expansion, causes electrode powder, causes to store
Capacity and cycle life decline rapidly.
Graphene is a kind of carbon material with special two-dimensional structure, has excellent electric conductivity and chemical property,
There is great application prospect in lithium ion battery electrode material.By graphene and stannic disulfide it is compound can improve material entirety
Electrical conductivity, buffer stannic disulfide charge and discharge process in Volume Changes, suppress stannic disulfide reunite effect, and then meet not
Carry out the needs of lithium ion cell high-capacity.
The content of the invention
The defects of existing for prior art, it is an object of the present invention to provide a kind of hollow plumbago alkene ball to load nanometer
Stannic disulfide composite and preparation method thereof, hollow plumbago alkene ball load nanometer stannic disulfide composite are a kind of two dimension knots
The carbon material of structure, the composite can accommodate the volumetric expansion of stannic disulfide in charge and discharge process, improve electrode material
Electric conductivity and structural stability, and porous graphene structure can improve the electric conductivity and ion transmission performance of material, have
Beneficial to lithium ion insertion and abjection in the material.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that.
A kind of hollow plumbago alkene ball loads nanometer stannic disulfide composite, it is characterised in that with the sky of submicron-scale
Heart graphene ball is carrier, and stannic disulfide nano particle is supported on the inner and outer wall of graphene hollow ball, is grown in hollow stone
The stannic disulfide particle size of black alkene ball surface is between 10-40 nm.
A kind of preparation method of hollow plumbago alkene ball load nanometer stannic disulfide composite, comprises the following steps：
A. synthesizing cationic type polystyrene spheres：Initiator potassium persulfate 0.1-1 g are taken to add in flask with three necks,round bottom,
50 mL deionized waters are added, obtain potassium persulfate solution, potassium persulfate solution is stirred in nitrogen atmosphere, is heated to 50-80
DEG C, styrene monomer 2-10 mL are added, condensing reflux reacts 24 h, and condensing reflux reaction adds 100- after carrying out 2-10 h
500 μ L MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, it is vacuum dried with deionized water centrifuge washing after reaction terminates
6-12 h, the solid obtained after drying, produce cationic polystyrene ball；
B. hollow plumbago alkene ball is synthesized：Above-mentioned steps a is obtained into cationic polystyrene ball to be dispersed in water, ultrasound 1
H, 1 h of a certain amount of graphene oxide solution ultrasound is taken, after ultrasonic, graphene oxide water solution and cationic poly after disperseing
Styrene ball in mass ratio 1:4 mixing, then 30 min of ultrasound, obtain mixed liquor, above-mentioned mixed liquor then are poured into round-bottomed flask,
Add with graphene oxide mass ratio and be（0.1-2）:1 hydrazine hydrate, in 95 DEG C of back flow reaction 1-6 h, after synthetic reaction terminates
Vacuum filtration, is washed with deionized, is dried in vacuo 6-12 h, then dried solid is immersed in toluene poly- to remove
Styrene ball template, then washed with absolute ethyl alcohol, obtain hollow plumbago alkene ball；
C. stannic disulfide is loaded：Take 1-10 mmol butter of tin to be dissolved in ethanol in proper amount, above-mentioned steps b is obtained
Hollow plumbago alkene ball be immersed in butter of tin solution, soak 12 h, take 1-10 mmol sulphur sources to be dissolved in 30 mL ethanol,
It is then added to above-mentioned mixed solution and is transferred in reactor, at 160-180 DEG C, the h of hydro-thermal reaction 4-12, after reaction terminates,
Reactor naturally cools to room temperature, and product is centrifuged, and is washed 1-3 times with absolute ethyl alcohol, and vacuum is drained, that is, obtains hollow stone
The composite of black alkene ball load nanometer stannic disulfide.
The addition quality of graphene oxide described in above-mentioned steps b is the cationic polystyrene described in step a
The 20-100% of the quality of ball.
Sulphur source described in above-mentioned steps c is thiocarbamide, one kind in thioacetamide, Cys, carbon disulfide.
It is of the invention to possess spy following prominent compared with other stannic disulfide/graphene composite materials and preparation method thereof
Point：
(1) preparation technology is simple, and cost of material is low.
(2) the hollow plumbago alkene ball prepared is a kind of macroporous structure of three-dimensional communication, not only remains graphene and compares surface
The advantages of product is big, the reunion of graphene film interlayer can be suppressed, improve the contact area of electrode and electrolyte, it is anti-to add electrochemistry
Answer efficiency.The hollow plumbago alkene spherical structure for being additionally, since preparation is a kind of pore passage structure of three-dimensional communication, increases material and ion
The contact area of phase, the avtive spot of increase ion transmission, the diffusion length of ion is reduced, improves the fortune of ion in the electrolytic solution
Movement Capabilities.
Brief description of the drawings
Fig. 1 is the XRD spectrum of hollow plumbago alkene ball load nanometer stannic disulfide composite prepared by embodiment 1.
Fig. 2 is the SEM pictures of hollow plumbago alkene ball load nanometer stannic disulfide composite prepared by embodiment 1.
Fig. 3 is the TEM pictures of hollow plumbago alkene ball load nanometer stannic disulfide composite prepared by embodiment 1.
Fig. 4 is the charge-discharge performance figure of hollow plumbago alkene ball load nanometer stannic disulfide composite prepared by embodiment 1.
Embodiment
Method provided by the present invention is further illustrated below by embodiment.
Embodiment 1
A kind of Preparation Method of hollow plumbago alkene ball load nanometer stannic disulfide composite, it is as follows the step of this method：
Take the g of initiator potassium persulfate 0.3 to add in flask with three necks,round bottom, add 50 mL deionized waters, add rotor
Potassium persulfate solution is stirred, nitrogen protection is passed through, is heated to 60 DEG C, adds the mL of styrene monomer 2, condensing reflux reaction 24
H, condensing reflux reaction add 500 μ L MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides after carrying out 7 h, after reaction terminates, spent
Ionized water centrifuge washing, vacuum dried 12 h, the solid obtained after drying, produce cationic polystyrene ball；
Cation polystyrene ball will be obtained to be dispersed in water, 1 h of ultrasound, take a certain amount of graphene oxide solution ultrasound 1
H, after ultrasonic, graphene oxide water solution and cation polystyrene ball in mass ratio 1 after disperseing:4 mixing, then ultrasound 30
Min, mixed liquor is obtained, above-mentioned mixed liquor is then poured into round-bottomed flask, it is 0.5 to add with graphene mass ratio:1 hydration
Hydrazine, in 95 DEG C of h of back flow reaction 2, synthetic reaction is filtered by vacuum after terminating, and is washed with deionized, is dried in vacuo 12h, then will
Dried solid is immersed in toluene to remove A Polystyrene Spheres Template, then washed with absolute ethyl alcohol, obtains hollow plumbago alkene
Ball；
5 mmol butter of tin is taken to be dissolved in 40 mL ethanol, the hollow plumbago alkene ball that above-mentioned steps b is obtained soaks
12 h in butter of tin solution, take 5 mmol thiocarbamides to be dissolved in 30 mL ethanol, be then added to above-mentioned solution and be transferred to anti-
Answer in kettle, at 180 DEG C, the h of hydro-thermal reaction 4, after reaction terminates, reactor naturally cools to room temperature, and product is centrifuged,
Washed 2 times with absolute ethyl alcohol, vacuum is drained, that is, obtains the composite of hollow plumbago alkene ball load nanometer stannic disulfide.
The electric performance test of the composite of hollow plumbago alkene ball load nanometer stannic disulfide is made：
Using the product of preparation as working electrode；Using metal lithium sheet as negative pole；Using microporous polypropylene membrane as barrier film；Electrolyte
It is by l.0 mol/L LiPF6Solution（It is dissolved in the solution that the mass ratioes such as EC/DMC are made into）；The group in the glove box full of argon gas
CR2032 type button cells are filled, constant current charge-discharge test are carried out, by the specific capacitance of single electrode that can be calculated material.Product
XRD as shown in Figure 1, as seen from the figure, the stannic disulfide containing pure phase in the composite of preparation, without obvious impurity peaks in the product.
Fig. 2 and Fig. 3 is the ESEM of the composite prepared（SEM）And transmission electron microscope（TEM）Photo, can from Fig. 2 and Fig. 3
Going out hollow plumbago alkene ball is formed by the graphene curling of thin layer, and the size of its hollow ball is about 1 μm；It is spherical in porous hollow
The substantial amounts of nanometer stannic disulfide particle of uniform load on the inside and outside wall of graphene, the size of stannic disulfide is 10-40 nm.Fig. 4 is
The hollow plumbago alkene ball load nanometer stannic disulfide composite of preparation is bent in the discharge and recharge of 0.005-3.00 V voltage ranges
Line.As shown in Figure 4, under 100 mA/g current densities, the first discharge specific capacity of the composite is up to 1133 mAh/g, and
For 2 specific discharge capacities up to 660 mAh/g, the 3rd specific discharge capacity, without obvious decay, shows answering for the present invention compared with the 2nd time
Condensation material has preferable cycle performance.
Embodiment 2
A kind of Preparation Method of hollow plumbago alkene ball load nanometer stannic disulfide composite, it is as follows the step of this method
Take the g of initiator potassium persulfate 0.25 to add in flask with three necks,round bottom, add 50 mL deionized waters, add rotor
Potassium persulfate solution is stirred, nitrogen protection is passed through, is heated to 75 DEG C, adds the mL of styrene monomer 5, condensing reflux reaction 24
H, condensing reflux reaction add 500 μ L MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides after carrying out 5h, after reaction terminates, spent
Ionized water centrifuge washing, vacuum dried 6 h, the solid obtained after drying, produce cationic polystyrene ball；
Cation polystyrene ball will be obtained to be dispersed in water, 1 h of ultrasound, take a certain amount of graphene oxide solution ultrasound 1
H, after ultrasonic, graphene oxide water solution and cation polystyrene ball in mass ratio 1 after disperseing:3 mixing, then ultrasound 30
Min, mixed liquor is obtained, above-mentioned mixed liquor is then poured into round-bottomed flask, it is 0.7 to add with graphene mass ratio:1 hydration
Hydrazine, in 95 DEG C of h of back flow reaction 4, synthetic reaction is filtered by vacuum after terminating, and is washed with deionized, is dried in vacuo 6 h, then will
Dried solid is immersed in toluene to remove A Polystyrene Spheres Template, then washed with absolute ethyl alcohol, obtains hollow plumbago alkene
Ball；
3 mmol butter of tin is taken to be dissolved in 40 mL ethanol, the hollow plumbago alkene ball that above-mentioned steps b is obtained soaks
12 h in butter of tin solution, take 3 mmol thioacetamides to be dissolved in 30 mL ethanol, be then added to above-mentioned solution simultaneously
It is transferred in reactor, at 160 DEG C, the h of hydro-thermal reaction 12, after reaction terminates, reactor naturally cools to room temperature, and product is centrifuged
Separation, is washed 2 times with absolute ethyl alcohol, and vacuum is drained, that is, obtains the composite of hollow plumbago alkene ball load nanometer stannic disulfide.
Embodiment 3
A kind of Preparation Method of hollow plumbago alkene ball load nanometer stannic disulfide composite, it is as follows the step of this method
Take the g of initiator potassium persulfate 0.5 to add in flask with three necks,round bottom, add 50 mL deionized waters, add rotor
Potassium persulfate solution is stirred, nitrogen protection is passed through, is heated to 85 DEG C, adds the mL of styrene monomer 8, condensing reflux reaction 24
H, condensing reflux reaction add 400 μ L MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides after carrying out 10h, after reaction terminates, spent
Ionized water centrifuge washing, vacuum dried 12 h, the solid obtained after drying, produce cationic polystyrene ball；
Cation polystyrene ball will be obtained to be dispersed in water, 1 h of ultrasound, take a certain amount of graphene oxide solution ultrasound 1
H, after ultrasonic, graphene oxide water solution and cation polystyrene ball in mass ratio 1 after disperseing:1 mixing, then ultrasound 30
Min, mixed liquor is obtained, above-mentioned mixed liquor is then poured into round-bottomed flask, it is 0.3 to add with graphene mass ratio:1 hydration
Hydrazine, in 95 DEG C of h of back flow reaction 5, synthetic reaction is filtered by vacuum after terminating, and is washed with deionized, is dried in vacuo 8 h, then
Dried solid is immersed in toluene to remove A Polystyrene Spheres Template, then washed with absolute ethyl alcohol, obtain hollow plumbago
Alkene ball；
10 mmol butter of tin is taken to be dissolved in 40 mL ethanol, the hollow plumbago alkene ball that above-mentioned steps b is obtained soaks
Bubble 12 h in butter of tin solution, take 8 mmol Cys to be dissolved in 30 mL ethanol, are then added to above-mentioned molten
Liquid is simultaneously transferred in reactor, and 8 h are reacted at 180 DEG C, and after reaction terminates, reactor naturally cools to room temperature, by product centrifugation point
From, washed 2 times with absolute ethyl alcohol, vacuum is drained, that is, obtain hollow plumbago alkene ball load nanometer stannic disulfide composite.
Embodiment 4
A kind of Preparation Method of hollow plumbago alkene ball load nanometer stannic disulfide composite, it is as follows the step of this method
Take the g of initiator potassium persulfate 1.0 to add in flask with three necks,round bottom, add 50 mL deionized waters, add rotor
Potassium persulfate solution is stirred, nitrogen protection is passed through, is heated to 90 DEG C, adds the mL of styrene monomer 10, condensing reflux reaction 24
H, condensing reflux reaction add 100 μ L MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides after carrying out 5h, after reaction terminates, spent
Ionized water centrifuge washing, vacuum dried 12 h, the solid that will be obtained after drying, produce cationic polystyrene ball；
Cation polystyrene ball will be obtained to be dispersed in water, 1 h of ultrasound, take a certain amount of graphene oxide solution ultrasound 1
H, graphene oxide water solution and cation polystyrene ball in mass ratio 1 after disperseing:5 mixing, then 30 min of ultrasound, are obtained
To mixed liquor, above-mentioned mixed liquor is then poured into round-bottomed flask, it is 1 to add with graphene mass ratio:1 hydrazine hydrate, at 95 DEG C
The h of back flow reaction 1, synthetic reaction are filtered by vacuum after terminating, and with ion water washing, vacuum drying 9 h, then will be dried
Solid is immersed in toluene to remove A Polystyrene Spheres Template, then washed with absolute ethyl alcohol, obtains hollow plumbago alkene ball；
3 mmol butter of tin is taken to be dissolved in 40 mL ethanol, the hollow plumbago alkene ball that above-mentioned steps b is obtained soaks
12 h in butter of tin solution, take 3 mmol carbon disulfide to be dissolved in 30 mL ethanol, be then added to above-mentioned solution and turn
Enter in reactor, in 180 DEG C of h of hydro-thermal reaction 12, after reaction terminates, reactor naturally cools to room temperature, by product centrifugation point
From, washed 3 times with absolute ethyl alcohol, vacuum is drained, that is, obtain hollow plumbago alkene ball load nanometer stannic disulfide composite.
Claims (3)
1. a kind of preparation method of hollow plumbago alkene ball load nanometer stannic disulfide composite, the composite is with sub-micro meter ruler
Very little hollow plumbago alkene ball is carrier, and stannic disulfide nano particle is supported on the inner and outer wall of graphene hollow ball, is grown in
The stannic disulfide particle size of hollow plumbago alkene ball surface is between 10-40 nm；Characterized in that, the preparation method is included such as
Lower step：
A. synthesizing cationic type polystyrene spheres：Take initiator potassium persulfate 0.1-1 g to add in flask with three necks,round bottom, then add
Enter 50 mL deionized waters, obtain potassium persulfate solution, stir potassium persulfate solution in nitrogen atmosphere, be heated to 50-80 DEG C, then
Styrene monomer 2-10 mL are added, condensing reflux reacts 24 h, and condensing reflux reaction adds 100-500 μ L after carrying out 2-10 h
MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, after reaction terminates, with deionized water centrifuge washing, vacuum dried 6-12 h,
The solid obtained after drying, produce cationic polystyrene ball；
B. hollow plumbago alkene ball is synthesized：Above-mentioned steps a is obtained into cationic polystyrene ball to be dispersed in water, 1 h of ultrasound,
1 h of a certain amount of graphene oxide solution ultrasound is taken, after ultrasonic, graphene oxide water solution and cationic polyphenyl after disperseing
Ethene ball in mass ratio 1:4 mixing, then 30 min of ultrasound, obtain mixed liquor, above-mentioned mixed liquor then are poured into round-bottomed flask, added
Enter and be with graphene oxide mass ratio（0.1-2）:1 hydrazine hydrate, in 95 DEG C of back flow reaction 1-6 h, synthetic reaction is true after terminating
Sky filters, and is washed with deionized, is dried in vacuo 6-12 h, then dried solid is immersed in toluene to remove polyphenyl
Ethene ball template, then washed with absolute ethyl alcohol, obtain hollow plumbago alkene ball；
C. stannic disulfide is loaded：1-10 mmol butter of tin is taken to be dissolved in ethanol in proper amount, the sky that above-mentioned steps b is obtained
Heart graphene ball is immersed in butter of tin solution, is soaked 12 h, is taken 1-10 mmol sulphur sources to be dissolved in 30 mL ethanol, then
It is added to above-mentioned mixed solution and is transferred in reactor, at 160-180 DEG C, the h of hydro-thermal reaction 4-12, after reaction terminates, instead
Answer kettle to naturally cool to room temperature, product is centrifuged, washed 1-3 times with absolute ethyl alcohol, vacuum is drained, that is, obtains hollow plumbago
Alkene ball loads the composite of nanometer stannic disulfide.
2. a kind of preparation method of hollow plumbago alkene ball load nanometer stannic disulfide composite according to claim 1, its
It is characterised by, the addition quality of the graphene oxide described in above-mentioned steps b is the cationic polystyrene described in step a
The 20-100% of the quality of ball.
3. a kind of preparation method of hollow plumbago alkene ball load nanometer stannic disulfide composite according to claim 1, its
It is characterised by, the sulphur source described in above-mentioned steps c is one kind in thiocarbamide, thioacetamide, Cys, carbon disulfide.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102522543A (en) * | 2011-12-15 | 2012-06-27 | 清华大学 | Method for preparing nanometer compound of tin disulfide-graphene |
| CN103346299A (en) * | 2013-06-08 | 2013-10-09 | 上海大学 | In-situ etching method for preparing hollow tin-based oxide/carbon composite nano-material |
| CN105098151A (en) * | 2015-06-19 | 2015-11-25 | 上海交通大学 | Molybdenum disulfide-carbon hollow ball hybrid material and preparation method thereof |
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2016
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102522543A (en) * | 2011-12-15 | 2012-06-27 | 清华大学 | Method for preparing nanometer compound of tin disulfide-graphene |
| CN103346299A (en) * | 2013-06-08 | 2013-10-09 | 上海大学 | In-situ etching method for preparing hollow tin-based oxide/carbon composite nano-material |
| CN105098151A (en) * | 2015-06-19 | 2015-11-25 | 上海交通大学 | Molybdenum disulfide-carbon hollow ball hybrid material and preparation method thereof |
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