CN109286011A - A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode - Google Patents
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode Download PDFInfo
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- CN109286011A CN109286011A CN201811140062.7A CN201811140062A CN109286011A CN 109286011 A CN109286011 A CN 109286011A CN 201811140062 A CN201811140062 A CN 201811140062A CN 109286011 A CN109286011 A CN 109286011A
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
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Abstract
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, it belongs to the preparation method of flexible electrode.The present invention is cooled to room temperature on carbon cloth using plasma enhanced chemical vapor deposition method growth of vertical graphene after reaction, for use；Stannic chloride pentahydrate is dissolved in n-butanol under stirring conditions, thioacetamide is then added, carrier solution is obtained after stirring, for use；Hydro-thermal reaction in carrier solution obtained is immersed at vertical graphene-based bottom obtained, cleaning, drying are taken out after reaction, a kind of stannic disulfide/vertical graphene nanometer sheet array electrode is made.The present invention not only has the characteristics of carbon-based material high conductivity by vertical graphene prepared by plasma enhanced chemical vapor deposition method, but also vertical graphene has cellular network.Vertical graphene has good electric conductivity, high porosity, the low and big specific surface area of density, excellent chemical property.
Description
Technical field
The invention belongs to the preparation methods of ion battery electrode, and in particular to a kind of stannic disulfide/vertical graphene nano
The preparation method of chip arrays electrode.
Background technique
With the continuous development demand of electronic equipment, some disadvantages of lithium ion battery gradually expose, for example, shortage of resources and
It is at high cost, it has been transferred to researcher sight gradually in sodium-ion battery.Performance of the electrode material to sodium-ion battery
Play the role of vital, especially negative electrode material, thus study preparation be suitable for sodium-ion battery negative electrode material it is aobvious
It obtains particularly important.
Transient metal sulfide has high theoretical specific capacity, is a kind of candidate of good anode material of lithium-ion battery
Person, but low conductivity makes metal sulfide have poor cycle performance and high rate performance, meanwhile, sodium-ion battery charge and discharge
It is also can not ignore the shortcomings that transient metal sulfide electrode material, which can generate biggish volume expansion, in the process.To understand
The certainly above problem, mostly use metal sulfide and carbon-based material are carried out it is compound, to improve the conductivity of active material, simultaneously
The cushion space of active material can be increased effectively to inhibit active in charge and discharge process by preparing cavernous array structure
The volume expansion of material.For being chosen to for a key point for carbon-based material, currently used carbon-based material mainly has carbon
Nanotube, redox graphene, Nano carbon balls etc., but above-mentioned carbon material is not able to satisfy porous requirement.
Summary of the invention
It is an object of the present invention to provide a kind of stannic disulfide/vertical graphene nanometer sheet array electrode preparation methods.
The invention is realized by the following technical scheme:
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, includes the following steps:
The preparation of step 1, vertical Graphene electrodes is grown on carbon cloth using plasma enhanced chemical vapor deposition method
Vertical graphene is cooled to room temperature after reaction, for use；
Step 2 prepares carrier solution, and stannic chloride pentahydrate is dissolved in n-butanol under stirring conditions, then plus
Enter thioacetamide, carrier solution is obtained after stirring, for use；
Step 3 prepares stannic disulfide/vertical graphene nanometer sheet array electrode, by the electricity of vertical graphene made from step 1
Hydro-thermal reaction in carrier solution is immersed made from step 2 in pole, and cleaning, drying are taken out after reaction, and a kind of stannic disulfide/vertical is made
Graphene nanometer sheet array electrode.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method, carbon in step 1
Cloth is 8~10 μm of the carbon fiber diameter in carbon cloth, the smooth no hole in surface.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method, in step 1
For when cabin pressure reaches 10mTorr, carbon cloth is put into cabin the step of chemical vapor deposition growth vertical graphene on carbon cloth
It is interior, then, when temperature is raised to 400 DEG C, it is passed through hydrogen and methane, hydrogen and methane flow rate ratio are 3:2, plasma generator function
Rate 550W, reaction time 2h.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method, in step 1
Hydrogen flowing quantity is 90sccm, methane flow 60sccm during the vertical graphene of chemical vapor deposition growth on carbon cloth.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method, five in step 2
Water tin tetrachloride, n-butanol, thioacetamide mass ratio be 2~3:140~150:1.5~2.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method, five in step 2
Water tin tetrachloride, n-butanol, thioacetamide mass ratio be 2.16:148.18:1.84.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method is stirred in step 2
Mix 15~30min of time.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method is hung down in step 3
Straight Graphene electrodes immerse in carrier solution.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method, water in step 3
Thermal rection condition reacts for 24 hours under conditions of being 180 DEG C.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method, it is clear in step 3
It washes to be cleaned 3~5 times with deionized water, then with washes of absolute alcohol 3~5 times, cleaning post-baking temperature is 60 DEG C.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method, the two of preparation
Artificial gold nanometer sheet is uniformly covered in vertical graphene-based bottom, and stannic disulphide nano slice pattern stable homogeneous, it is not present
The substance of his structure and morphology, and stannic disulphide nano slice vertical-growth is at the top of vertical graphene；The thickness of stannic disulphide nano slice
Degree is about 128nm, and length is about 1 μm, while visible stannic disulphide nano slice is interconnected with one another to form fenestral fabric；Preparation
Stannic disulfide/vertical graphene nanometer sheet array electrode in ultra-thin stannic disulphide nano slice be interconnected with one another.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method, described one
Stannic disulfide/vertical graphene nanometer sheet of kind stannic disulfide/vertical graphene nanometer sheet array electrode preparation method preparation
Array electrode is assembled into button cell, and assembling process carries out in glove box, assembling sequence are as follows: anode cover, electrode material, electricity
Solve liquid, diaphragm, electrolyte, lithium piece, nickel foam, electrolyte, negative electrode casing.The group of battery can be completed with sealing machine encapsulation later
Dress carries out cycle performance test, current density 100mA g-1, first circle specific discharge capacity can be up to 1160mAh g-1；Work as electric current
Density is 1A g-1When, specific discharge capacity is 897mAh g-1；When current density is up to 5A g-1When, electrode is still able to maintain 727mAh
g-1Capacity.Current density again returns to low current 1A g-1When, specific discharge capacity has been restored to 879mAh g-1, electric discharge
Specific capacity has substantially returned to the capacity before fast charging and discharging.
A kind of stannic disulfide of the present invention/vertical graphene nanometer sheet array electrode preparation method, by it is equal from
The vertical graphene of daughter enhancing CVD method (PECVD) preparation not only has the spy of the high conductivity of carbon-based material
Point, and vertical graphene has cellular network.Vertical graphene has good electric conductivity, high porosity, density
Low and big specific surface area, a kind of stannic disulfide/vertical graphene nanometer sheet array electrode of preparation have excellent
Performance.
Detailed description of the invention
Fig. 1 amplifies 1000 times of SEM figure for the carbon fiber in carbon cloth used in one method of specific embodiment；
Fig. 2 is the SEM figure that the vertical Graphene electrodes of one method of specific embodiment preparation amplify 2000 times；
Fig. 3 is the SEM figure that the vertical Graphene electrodes of one method of specific embodiment preparation amplify 5000 times；
Fig. 4 is stannic disulfide/vertical graphene nanometer sheet array electrode amplification of one method of specific embodiment preparation
3000 times of SEM figure；
Fig. 5 is stannic disulfide/vertical graphene nanometer sheet array electrode amplification of one method of specific embodiment preparation
13000 times of SEM figure；
Fig. 6 is stannic disulfide/vertical graphene nanometer sheet array electrode amplification of one method of specific embodiment preparation
40000 times of SEM figure；
Fig. 7 is two sulphur on stannic disulfide/vertical graphene nanometer sheet array electrode of one method of specific embodiment preparation
Change the TEM figure that tin nanometer sheet amplifies 10000 times；
Fig. 8 is two sulphur on stannic disulfide/vertical graphene nanometer sheet array electrode of one method of specific embodiment preparation
Change the TEM figure that tin nanometer sheet amplifies 20000 times；
Fig. 9 is two sulphur on stannic disulfide/vertical graphene nanometer sheet array electrode of one method of specific embodiment preparation
Change the HRTEM figure that tin nanometer sheet amplifies 400000 times；
Figure 10 is two sulphur on stannic disulfide/vertical graphene nanometer sheet array electrode of one method of specific embodiment preparation
Change tin nanometer sheet electron diffraction diagram；
Figure 11 is that stannic disulfide/vertical graphene nanometer sheet array electrode XRD of one method of specific embodiment preparation is surveyed
Try curve；
Figure 12 is stannic disulfide/vertical graphene nanometer sheet array electrode Raman of one method of specific embodiment preparation
Spectrum；
Figure 13 is stannic disulfide/vertical graphene nanometer sheet array electrode circulation of one method of specific embodiment preparation
Volt-ampere curve；
Figure 14 is stannic disulfide/vertical graphene nanometer sheet array electrode circulation of one method of specific embodiment preparation
Number charge/discharge capacity curve；
Figure 15 is stannic disulfide/vertical graphene nanometer sheet array electrode and pure two of one method of specific embodiment preparation
The AC impedance for vulcanizing tin powder compares map；
Figure 16 is stannic disulfide/vertical graphene nanometer sheet array electrode and pure two of one method of specific embodiment preparation
Vulcanize the AC impedance analog circuit figure of tin powder.
Specific embodiment
Specific embodiment 1:
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, includes the following steps:
The preparation of step 1, vertical Graphene electrodes utilizes chemical vapour deposition technique growth of vertical graphene on carbon cloth,
After reaction, it is cooled to room temperature, for use；
Step 2 prepares carrier solution, and stannic chloride pentahydrate is dissolved in n-butanol under stirring conditions, then plus
Enter thioacetamide, carrier solution is obtained after stirring, for use；
Step 3 prepares stannic disulfide/vertical graphene nanometer sheet array electrode, by the electricity of vertical graphene made from step 1
Hydro-thermal reaction in carrier solution is immersed made from step 2 in pole, and cleaning, drying are taken out after reaction, and a kind of stannic disulfide/vertical is made
Graphene nanometer sheet array electrode.
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, step 1 described in present embodiment
Middle carbon cloth is 8~10 μm of the carbon fiber diameter in carbon cloth, the smooth no hole in surface.
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, step 1 described in present embodiment
In the vertical graphene of chemical vapor deposition growth on carbon cloth the step of for when cabin pressure reaches 10mTorr, carbon cloth is put into
In cabin, then, when temperature is raised to 400 DEG C, it is passed through hydrogen and methane, hydrogen and methane flow rate ratio are 3:2, and plasma occurs
Device power 550W, reaction time 2h.
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, step 1 described in present embodiment
During the vertical graphene of chemical vapor deposition growth on carbon cloth hydrogen flowing quantity be 90sccm, methane flow is
60sccm。
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, step 2 described in present embodiment
Middle stannic chloride pentahydrate, n-butanol, thioacetamide mass ratio be 2.16:148.18:1.84.
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, step 2 described in present embodiment
Middle 15~30min of mixing time.
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, step 3 described in present embodiment
In vertical Graphene electrodes immerse in carrier solution.
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, step 3 described in present embodiment
Middle hydrothermal reaction condition reacts for 24 hours under conditions of being 180 DEG C.
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, step 3 described in present embodiment
Middle cleaning is to be cleaned 3~5 times with deionized water, then with washes of absolute alcohol 3~5 times, cleaning post-baking temperature is 60 DEG C.
It is used in a kind of stannic disulfide described in present embodiment/vertical graphene nanometer sheet array electrode preparation method
Carbon fiber in carbon cloth amplifies 1000 times of SEM figure as shown in Figure 1, from FIG. 1, it can be seen that described in preparation present embodiment
A kind of carbon cloth carbon fiber surface of stannic disulfide/vertical graphene nanometer sheet array electrode is smooth, no hole.
A kind of preparation method preparation of stannic disulfide described in present embodiment/vertical graphene nanometer sheet array electrode
The SEM that vertical Graphene electrodes amplify 2000 times schemes as shown in Figure 2,5000 times SEM and schemes as shown in figure 3, vertical graphene is
Graphene film vertical-growth is interconnected with one another to form porous web grating texture on carbon fiber, and the thickness of graphene film is about
96nm。
A kind of preparation method preparation of stannic disulfide described in present embodiment/vertical graphene nanometer sheet array electrode
The SEM figure that stannic disulfide/vertical graphene nanometer sheet array electrode amplifies 3000 times is as shown in Figure 4, amplifies 13000 times of SEM
Figure is as shown in Figure 5,40000 times of amplification SEM figure is as shown in Figure 6: from Fig. 4 and Fig. 5 it is found that stannic disulphide nano slice uniformly covers
It is placed on vertical graphene-based bottom, and stannic disulphide nano slice pattern stable homogeneous, there is no the substances of other structures pattern, and
Stannic disulphide nano slice vertical-growth is in vertical graphene surface.As can be seen from Figure 6 a kind of stannic disulfide described in present embodiment/
Vertical graphene nanometer sheet array electrode, the thickness of stannic disulphide nano slice is about 128nm, and length is about 1 μm, while visible two
Artificial gold nanometer sheet is interconnected with one another to form fenestral fabric.
A kind of preparation method preparation of stannic disulfide described in present embodiment/vertical graphene nanometer sheet array electrode
The TEM figure that stannic disulfide/vertical graphene nanometer sheet array electrode amplifies 10000 times is as shown in Figure 7, amplifies 20000 times of TEM
Figure is as shown in Figure 8: from Fig. 7 and Fig. 8 it is found that stannic disulfide/vertical graphene nanometer sheet of one method of specific embodiment preparation
Ultra-thin SnS in array electrode2Nanometer sheet is interconnected with one another.
A kind of preparation method preparation of stannic disulfide described in present embodiment/vertical graphene nanometer sheet array electrode
Stannic disulfide/vertical graphene nanometer sheet array electrode amplifies 400000 times of HRTEM figures as shown in figure 9, as can be seen from Figure 9, passing through
The spacing that lattice is analyzed between adjacent side edge lattice plane is respectively 0.18nm and 0.59nm, corresponding to stannic disulphide nano slice
(001) and (200) crystal face.
A kind of preparation method preparation of stannic disulfide described in present embodiment/vertical graphene nanometer sheet array electrode
Stannic disulfide/vertical graphene nanometer sheet array electrode electron diffraction diagram is as shown in Figure 10, can confirm again from Figure 10
There is (200) and (100) crystal face in the stannic disulphide nano slice in stannic disulfide/vertical graphene nanometer sheet array electrode.
A kind of preparation method preparation of stannic disulfide described in present embodiment/vertical graphene nanometer sheet array electrode
Stannic disulfide/vertical graphene nanometer sheet array electrode XRD test curve is as shown in figure 11, as can be seen from Figure 11, described one kind
Stannic disulfide/vertical graphene nanometer sheet array electrode array diffraction maximum respectively appears in 15.0,28.2,32.1,41.9,
50.0,52.5,55.0 and 60.6 °, correspond respectively to (001), (100), (101), (102), (110), (111), (103) and
(201) crystal face, by being hexaplanar stannic disulfide known to reference standard spectrogram (JCPDF42-1467).
A kind of preparation method preparation of stannic disulfide described in present embodiment/vertical graphene nanometer sheet array electrode
Stannic disulfide/vertical graphene nanometer sheet array electrode Raman spectrum is as shown in figure 12, from Figure 12 it can be seen that in 200cm-1
And 2000cm-1Between, 370cm-1The Raman peaks that place occurs correspond to the raman characteristic peak of stannic disulfide, are located at 1323cm-1With
1589cm-1The Raman peaks at place, corresponding to the peak D and the peak G of vertical graphene, Raman spectrum analysis confirms a kind of curing
The presence of stannic disulfide and vertical graphene in tin/vertical graphene nanometer sheet array electrode.
A kind of preparation method preparation of stannic disulfide described in present embodiment/vertical graphene nanometer sheet array electrode
Stannic disulfide/vertical graphene nanometer sheet array electrode, is assembled into button cell, and assembling process carries out in glove box, assembling
Sequentially are as follows: anode cover, electrode material, electrolyte, diaphragm, electrolyte, lithium piece, nickel foam, electrolyte, negative electrode casing.Later with envelope
The assembling of battery can be completed after installation encapsulation, progress cyclic voltammetry test curve is as shown in figure 13, carries out circulation time
Number charge/discharge capacity curve is as shown in figure 14: it can be seen that a kind of stannic disulfide/vertical graphene nano chip arrays from Figure 13
Occurs apparent Reversible redox reaction in electrode charge and discharge process；The test current density of Figure 14 is respectively as follows: 0.1,
0.2,0.3,0.5,1,2,3 and 5A g-1, it can be seen that current density 100mA g from Figure 14-1, first circle specific discharge capacity can
To be up to 1160mAh g-1；When current density is 1A g-1When, specific discharge capacity is 897mAh g-1；When current density is up to
5Ag-1When, electrode is still able to maintain 727mAh g-1Capacity.Current density again returns to low current 1A g-1When, electric discharge ratio
Capacity restoration has arrived 879mAh g-1, specific discharge capacity substantially returned to the capacity before fast charging and discharging.Illustrate this embodiment party
A kind of stannic disulfide of formula method preparation/vertical graphene nanometer sheet array electrode has excellent chemical property.
A kind of preparation method preparation of stannic disulfide described in present embodiment/vertical graphene nanometer sheet array electrode
Stannic disulfide/vertical graphene nanometer sheet array electrode, is assembled into the pure curing glass putty of button cell and same method preparation
The AC impedance comparison diagram at end is as shown in figure 15, AC impedance analog circuit schematic diagram is as shown in figure 16: from figure 15, it can be known that two sulphur
Change stannic disulfide/vertical graphene nano chip arrays electricity of tin/vertical graphene nanometer sheet array electrode preparation method preparation
The impedance of pole is much smaller than the pure stannic disulphide nano slice impedance of method of the same race preparation.Table 1 is the impedance pair of AC impedance analog circuit
Ratio is as shown in table 1:
1 AC impedance analog circuit impedance contrast value of table
Specific resistance value as can be seen from Table 1, by comparing a kind of stannic disulfide/vertical graphene nano
Chip arrays electrode resistance value corresponding with pure stannic disulphide nano slice electrode, a kind of stannic disulfide/vertical graphene are received
The R of rice chip arrays electrodebFor 2.543 Ω, R1For 1.947 Ω, R2For 3.961 Ω, a kind of stannic disulfide/vertical graphite
Alkene nano-chip arrays electrode has smaller resistance value, i.e., more excellent conductivity performance.
Specific embodiment 2:
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, includes the following steps:
The preparation of step 1, vertical Graphene electrodes utilizes chemical vapour deposition technique growth of vertical graphene on carbon cloth,
After reaction, it is cooled to room temperature, for use；
Step 2 prepares carrier solution, and stannic chloride pentahydrate is dissolved in n-butanol under stirring conditions, then plus
Enter thioacetamide, carrier solution is obtained after stirring, for use；
Step 3 prepares stannic disulfide/vertical graphene nanometer sheet array electrode, by the electricity of vertical graphene made from step 1
Hydro-thermal reaction in carrier solution is immersed made from step 2 in pole, and cleaning, drying are taken out after reaction, and a kind of stannic disulfide/vertical is made
Graphene nanometer sheet array electrode.
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, preparation described in present embodiment
Stannic disulphide nano slice be uniformly covered in vertical graphene-based bottom, and stannic disulphide nano slice pattern stable homogeneous, do not deposit
In the substance of other structures pattern, and stannic disulphide nano slice vertical-growth is at the top of vertical graphene；Stannic disulphide nano slice
Thickness be about 128nm, length is about 1 μm, while visible stannic disulphide nano slice is interconnected with one another to form fenestral fabric；
Ultra-thin stannic disulphide nano slice in the stannic disulfide of preparation/vertical graphene nanometer sheet array electrode is interconnected with one another.
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, described described in present embodiment
Stannic disulfide/vertical graphene of stannic disulfide/vertical graphene nanometer sheet array electrode preparation method preparation a kind of receive
Rice chip arrays electrode, is assembled into button cell, assembling process carries out in glove box, assembling sequence are as follows: anode cover, electrode material
Material, electrolyte, diaphragm, electrolyte, lithium piece, nickel foam, electrolyte, negative electrode casing.It can be completed later with sealing machine encapsulation later
The assembling of battery carries out cycle performance test, current density 100mA g-1, first circle specific discharge capacity can be up to 1160mAh g-1；When current density is 1A g-1When, specific discharge capacity is 897mAh g-1；When current density is up to 5A g-1When, electrode remains to protect
Hold 727mAh g-1Capacity.Current density again returns to low current 1A g-1When, specific discharge capacity has been restored to 879mAh
g-1, specific discharge capacity substantially returned to the capacity before fast charging and discharging.
A kind of preparation method of stannic disulfide/vertical graphene nanometer sheet array electrode, passes through described in present embodiment
The vertical graphene of plasma enhanced CVD method (PECVD) preparation not only has the high conductivity of carbon-based material
Feature, and vertical graphene has cellular network.Vertical graphene has good electric conductivity, high porosity, close
Low and big specific surface area is spent, a kind of stannic disulfide/vertical graphene nanometer sheet array electrode of preparation has excellent
Performance.
Specific embodiment 3:
A kind of preparation side of stannic disulfide/vertical graphene nanometer sheet array electrode according to specific embodiment two
Method, carbon cloth is 8~10 μm of the carbon fiber diameter in carbon cloth in step 1, the smooth no hole in surface.
Specific embodiment 4:
A kind of preparation side of stannic disulfide/vertical graphene nanometer sheet array electrode according to specific embodiment two
Method, for when cabin pressure reaches 10mTorr the vertical graphene of chemical vapor deposition growth on carbon cloth the step of in step 1,
Carbon cloth is put into cabin, then, when temperature is raised to 400 DEG C, is passed through hydrogen and methane, and hydrogen and methane flow rate ratio are 3:2, wait from
Daughter generator power 550W, reaction time 2h.
Specific embodiment 5:
A kind of preparation side of stannic disulfide/vertical graphene nanometer sheet array electrode according to specific embodiment two
Method, hydrogen flowing quantity is 90sccm, methane flow during the vertical graphene of chemical vapor deposition growth on carbon cloth in step 1
For 60sccm.
Specific embodiment 6:
A kind of preparation side of stannic disulfide/vertical graphene nanometer sheet array electrode according to specific embodiment two
Method, stannic chloride pentahydrate in step 2, n-butanol, thioacetamide mass ratio be 2~3:140~150:1.5~2.
Specific embodiment 7:
A kind of preparation side of stannic disulfide/vertical graphene nanometer sheet array electrode according to specific embodiment two
Method, stannic chloride pentahydrate in step 2, n-butanol, thioacetamide mass ratio be 2.16:148.18:1.84.
Specific embodiment 8:
A kind of preparation side of stannic disulfide/vertical graphene nanometer sheet array electrode according to specific embodiment two
Method, 15~30min of mixing time in step 2.
Specific embodiment 9:
A kind of preparation side of stannic disulfide/vertical graphene nanometer sheet array electrode according to specific embodiment two
Method, vertical Graphene electrodes immerse in carrier solution in step 3.
Specific embodiment 10:
A kind of preparation side of stannic disulfide/vertical graphene nanometer sheet array electrode according to specific embodiment two
Method, hydrothermal reaction condition reacts for 24 hours under conditions of being 180 DEG C in step 3.
Specific embodiment 11:
A kind of preparation side of stannic disulfide/vertical graphene nanometer sheet array electrode according to specific embodiment two
Method, cleaning is clean 3~5 times with deionized water in step 3, then with washes of absolute alcohol 3~5 times, cleaning post-baking temperature is
60℃。
Claims (9)
1. a kind of stannic disulfide/vertical graphene nanometer sheet array electrode preparation method, it is characterised in that: including walking as follows
It is rapid:
The preparation of step 1, vertical Graphene electrodes utilizes plasma enhanced chemical vapor deposition method growth of vertical on carbon cloth
Graphene is cooled to room temperature after reaction, for use；
Step 2 prepares carrier solution, and stannic chloride pentahydrate is dissolved in n-butanol under stirring conditions, sulphur is then added
For acetamide, carrier solution is obtained after stirring, for use；
Step 3 prepares stannic disulfide/vertical graphene nanometer sheet array electrode, and vertical Graphene electrodes made from step 1 are soaked
Enter hydro-thermal reaction in carrier solution made from step 2, cleaning, drying are taken out after reaction, a kind of stannic disulfide/vertical graphite is made
Alkene nano-chip arrays electrode.
2. a kind of stannic disulfide according to claim 1/vertical graphene nanometer sheet array electrode preparation method, special
Sign is: carbon cloth is in step 1,8~10 μm of the carbon fiber diameter in carbon cloth.
3. a kind of stannic disulfide according to claim 1/vertical graphene nanometer sheet array electrode preparation method, special
Sign is: for when cabin pressure reaches 10mTorr the vertical graphene of chemical vapor deposition growth on carbon cloth the step of in step 1
When, carbon cloth is put into cabin, then, when temperature is raised to 400 DEG C, is passed through hydrogen and methane, and hydrogen and methane flow rate ratio are 3:2,
Plasma generator power 550W, reaction time 2h.
4. a kind of stannic disulfide according to claim 3/vertical graphene nanometer sheet array electrode preparation method, special
Sign is: hydrogen flowing quantity is 90sccm, methane during the vertical graphene of chemical vapor deposition growth on carbon cloth in step 1
Flow is 60sccm.
5. a kind of stannic disulfide according to claim 1/vertical graphene nanometer sheet array electrode preparation method, special
Sign is: stannic chloride pentahydrate in step 2, n-butanol, thioacetamide mass ratio be 2~3:140~150:1.5~2.
6. a kind of stannic disulfide according to claim 5/vertical graphene nanometer sheet array electrode preparation method, special
Sign is: stannic chloride pentahydrate in step 2, n-butanol, thioacetamide mass ratio be 2.16:148.18:1.84.
7. a kind of stannic disulfide according to claim 1/vertical graphene nanometer sheet array electrode preparation method, special
Sign is: 15~30min of mixing time in step 2.
8. a kind of stannic disulfide according to claim 1/vertical graphene nanometer sheet array electrode preparation method, special
Sign is: hydrothermal reaction condition reacts for 24 hours under conditions of being 180 DEG C in step 3.
9. a kind of stannic disulfide according to claim 1/vertical graphene nanometer sheet array electrode preparation method, special
Sign is: cleaning is to be cleaned 3~5 times with deionized water, then with washes of absolute alcohol 3~5 times, temperature is dried after cleaning in step 3
Degree is 60 DEG C.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110190266A (en) * | 2019-06-20 | 2019-08-30 | 北京理工大学 | A kind of preparation method of the stannic disulphide nano slice array of metal heteroatom doping as binder free anode material of lithium-ion battery |
| CN110993908A (en) * | 2019-11-27 | 2020-04-10 | 浙江大学 | Vertical graphene/manganese dioxide composite material and preparation method and application thereof |
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| CN111883761A (en) * | 2020-08-05 | 2020-11-03 | 重庆信合启越科技有限公司 | Silicon graphene composite lithium battery negative electrode material and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014051413A (en) * | 2012-09-07 | 2014-03-20 | National Institute Of Advanced Industrial & Technology | Graphene-cnt structure and production method of the same |
| CN104667950A (en) * | 2015-02-07 | 2015-06-03 | 南昌航空大学 | Method for preparing graphene-SnIn4S8 nano composite photocatalyst at low temperature by adopting coprecipitation method |
| CN105621355A (en) * | 2016-03-08 | 2016-06-01 | 上海大学 | Composite material with hollow graphene spheres loaded with nanometer tin disulfide and method for preparing composite material |
| CN105914374A (en) * | 2016-05-31 | 2016-08-31 | 浙江大学 | Nitrogen-doped carbon-coated molybdenum selenide/graphene core-shell array sandwich structure composite material, preparation method and application thereof |
| CN108172806A (en) * | 2018-01-08 | 2018-06-15 | 北京理工大学 | A kind of composite nanostructure economic benefits and social benefits consolidate the preparation method of sulphur lithium sulfur battery anode material |
-
2018
- 2018-09-28 CN CN201811140062.7A patent/CN109286011B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014051413A (en) * | 2012-09-07 | 2014-03-20 | National Institute Of Advanced Industrial & Technology | Graphene-cnt structure and production method of the same |
| CN104667950A (en) * | 2015-02-07 | 2015-06-03 | 南昌航空大学 | Method for preparing graphene-SnIn4S8 nano composite photocatalyst at low temperature by adopting coprecipitation method |
| CN105621355A (en) * | 2016-03-08 | 2016-06-01 | 上海大学 | Composite material with hollow graphene spheres loaded with nanometer tin disulfide and method for preparing composite material |
| CN105914374A (en) * | 2016-05-31 | 2016-08-31 | 浙江大学 | Nitrogen-doped carbon-coated molybdenum selenide/graphene core-shell array sandwich structure composite material, preparation method and application thereof |
| CN108172806A (en) * | 2018-01-08 | 2018-06-15 | 北京理工大学 | A kind of composite nanostructure economic benefits and social benefits consolidate the preparation method of sulphur lithium sulfur battery anode material |
Non-Patent Citations (4)
| Title |
|---|
| JIAN-GAN WANG等: "Edge-oriented SnS2 nanosheet arrays on carbon paper as advanced binder-free anodes for Li-ion and Na-ion batteries", 《J. MATER. CHEM. A》 * |
| MINGHUA CHEN等: "Construction of reduced graphene oxide supported molybdenum carbides composite electrode as high-performance anode materials for lithium ion batteries", 《MATERIALS RESEARCH BULLETIN》 * |
| WANGWANG XU等: "SnS2@Graphene nanosheet arrays grown on carbon cloth as freestanding binder-free flexible anodes for advanced sodium batteries", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| XINHUI XIA等: "Boosting sodium ion storage by anchoring MoO2 on vertical graphene arrays", 《J. MATER. CHEM. A》 * |
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