CN109326787A - A kind of preparation method of tungsten disulfide/GO combination electrode material - Google Patents
A kind of preparation method of tungsten disulfide/GO combination electrode material Download PDFInfo
- Publication number
- CN109326787A CN109326787A CN201811279164.7A CN201811279164A CN109326787A CN 109326787 A CN109326787 A CN 109326787A CN 201811279164 A CN201811279164 A CN 201811279164A CN 109326787 A CN109326787 A CN 109326787A
- Authority
- CN
- China
- Prior art keywords
- electrode material
- combination electrode
- preparation
- tungsten disulfide
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—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
- H01M4/5815—Sulfides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
A kind of preparation method of tungsten disulfide/GO combination electrode material, GO is add to deionized water to form solution A, then Disodium tungstate (Na2WO4) dihydrate is added, it stirs evenly, add cetyl trimethylammonium bromide, adjusting pH value is 1.3~1.7, is 0~10MPa, carries out microwave hydrothermal reaction at 120~180 DEG C in pressure, obtains WO3/ GO powder；By WO3/ GO powder is mixed with thioacetamide, is then calcined, and tungsten disulfide/GO combination electrode material is obtained.For the present invention using Disodium tungstate (Na2WO4) dihydrate as tungsten source, sulphur source is thioacetamide；Using microwave-hydrothermal method by control Concentration of precursor solution, and under template effect, WS is obtained2/ GO combination product, preparation process is simple, and technological parameter is easy to control, and repeatability is high, and the composite material that the present invention synthesizes is conducive to electron-transport as anode material of lithium-ion battery, to promote the chemical property of battery.
Description
Technical field
The present invention relates to WS2A kind of technical field of nano material preparation, and in particular to tungsten disulfide/GO combination electrode material
The preparation method of material.
Background technique
WS2As a kind of transition metal chalcogenide MX2(M=Mo, W；X=S, Se), with MoS2There is similar structure special
Sign, is the class graphene layer structure of hexagonal phase, and interlamellar spacing is bigThis layer structure can promote to live
Property substance and electrolyte react, increase active site, make that sodium ion is embedded in and abjection process is more smooth, finally make electrochemistry
Performance gets a promotion.But it has biggish volume expansion in charge and discharge process, leads to the stable circulation of material
Property is poor.And material itself arrives poorly conductive, is unfavorable for the transmission of electronics.Solve the problems, such as that volume expansion commonly solves at present
Method is the composite material synthesized using carbon as matrix, alleviates its generated stress during volume expansion, while strengthening material
The electric conductivity of material.
According to the literature, using carbon material as matrix, be conducive to the transmission of electronics, can effectively improve composite material conduct
The chemical property of lithium ion battery negative material.Such as Guowei Huang et al. is by tungsten disulfide and three-dimensional graphene oxide
Compound (Huang G, Liu H, Wang S, et al.Hierarchical architecture of WS2nanosheets on
graphene frameworks with enhanced electrochemical properties for lithium
storage and hydrogen evolution[J].Journal of Materials Chemistry A,2015,3
(47): 24128-24138.) as lithium ion battery negative material, it is compound after tungsten disulfide its chemical property it is big
Width is promoted, and 100 circles are recycled under the current density of 100mA/g, and capacity is maintained at 766mAh/g.Jing Ren et al. is by two sulphur
Change tungsten and three-dimensional single-walled carbon nanotube composite material as lithium ion battery negative material (Ren J, Wang Z, Yang F, et
al.Freestanding 3D single-wall carbon nanotubes/WS2,nanosheets foams as
ultra-long-life anodes for rechargeable lithium ion batteries[J]
.ElectrochimicaActa, the cyclical stability for 2018.), greatly improving material follows under the current density of 1A/g
Ring 1000 encloses, and capacity is stablized in 688.9mAh/g.But the chemical property of sodium-ion battery is up for being promoted.
Summary of the invention
The purpose of the present invention is to provide a kind of tungsten disulfide/GO combination electrode material preparation methods, utilize hydro-thermal method
By controlling Concentration of precursor solution, and under the booster action of template, WS is obtained2/ GO combination product, the present invention prepared by
WS2/ GO combination product, good dispersion is of uniform size, and pattern is uniform, has biggish dive using upper in sodium-ion battery cathode
Energy.
To achieve the above object, the present invention adopts the following technical scheme that:
A kind of preparation method of tungsten disulfide/GO combination electrode material, comprising the following steps:
Step 1: being add to deionized water ultrasound to uniform solution A is formed for GO, Disodium tungstate (Na2WO4) dihydrate be then added,
Stir evenly, add cetyl trimethylammonium bromide, adjusting pH value is 1.3~1.7, pressure be 0~10MPa, 120~
Microwave hydrothermal is carried out at 180 DEG C and reacts 0.5~4h, is washed, it is dry, obtain WO3/ GO powder；
Step 2: being in molar ratio 1:(10~20), by WO3/ GO powder is mixed with thioacetamide, is then calcined, is obtained
To tungsten disulfide/GO combination electrode material.
A further improvement of the present invention lies in that the concentration of GO is 0.5~3mol/L in solution A；Disodium tungstate (Na2WO4) dihydrate and GO
Mass ratio be 0.618~1.65g:25~75mg；The mass ratio of Disodium tungstate (Na2WO4) dihydrate and cetyl trimethylammonium bromide is
10:(1~3).
A further improvement of the present invention lies in that the speed of stirring is 400~600r/min, 0.5~1h of time of stirring.
A further improvement of the present invention lies in that ultrasonic power is 300~1000W, the time is 2~5h.
A further improvement of the present invention lies in that using the nitre acid for adjusting pH value of 1~3mol/L for 1.3~1.7.
A further improvement of the present invention lies in that microwave hydrothermal reaction carries out in high-throughput super-pressure microwave dissolver.
A further improvement of the present invention lies in that the temperature of calcining is 600~900 DEG C, the time is 1~3h.
Compared with prior art, the invention has the benefit that the present invention is using Disodium tungstate (Na2WO4) dihydrate as tungsten source, sulphur source is
Thioacetamide；Using microwave-hydrothermal method by control Concentration of precursor solution, and in template cetyl trimethylammonium bromide
Under booster action, WS is obtained2/ GO combination product, preparation process is simple, and technological parameter is easy to control, and repeatability is high, uses this method
WS obtained2/ GO composite material has wide researching value and application value in electrochemical field.The present invention is synthesized with carbon
The composite material of matrix is conducive to electron-transport as anode material of lithium-ion battery, to promote the chemical property of battery.
Detailed description of the invention
Fig. 1 is WS prepared by embodiment 32X-ray diffraction (XRD) map of/GO composite material；
Fig. 2 is WS prepared by embodiment 32Scanning electron microscope (SEM) photo of/GO composite material；
Fig. 3 is WS prepared by embodiment 32Transmission electron microscope (TEM) photo of/GO composite material；
Fig. 4 is WS prepared by embodiment 32The cycle performance figure of/GO composite material.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing.
Embodiment 1
Step 1: under room temperature, 25mg GO being added in 45mL deionized water, ultrasonic 2h to formation uniform solution A.
Ultrasonic power is 300W；
Step 2: 0.618g Disodium tungstate (Na2WO4) dihydrate being added in solution A and is stirred to being completely dissolved, mixing speed 500r/
Min, mixing time 0.5h；
Step 3: taking 0.0618g cetyl trimethylammonium bromide (CTAB) to be added in above-mentioned solution, controls mass ratio
mSodium tungstate: mCTAB=10:1；
Step 4: concentrated nitric acid is diluted to the clear solution B of 3mol/L, solution B is added drop-wise in above-mentioned solution, keeps its molten
Liquid pH value is 1.3, and acquired solution is solution C；
Step 5: above-mentioned solution C being transferred in microwave hydrothermal kettle, water heating kettle is then sealed, and is put it into high-throughput super
High-pressure microwave is cleared up in instrument, and control microwave hydrothermal temperature is 120 DEG C, pressure 1MPa, reaction time 2h, after reaction certainly
So it is cooled to room temperature.
Step 6: opening microwave reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifuged point
From it is -40 DEG C that repeated washing 4 times, which are placed on temperature, and vacuum degree is dry 12h in 40Pa freeze drier, obtains black
WO3/ GO composite material.
Step 7: resulting WO is taken3/ GO powder is as tungsten source, and thioacetamide is as sulphur source, mole in tungsten source and sulphur source
Than for 1:10, tungsten source taken amount is 0.3g, and 900 DEG C of calcination temperature, soaking time 2h obtains WS2/ GO composite material.
Embodiment 2
Step 1: under room temperature, ultrasound 4h to formation uniform solution A in 50mL deionized water is added in 50mg GO.It is super
Acoustical power is 800W
Step 2: 0.711g Disodium tungstate (Na2WO4) dihydrate being added in solution A and is stirred to being completely dissolved, mixing speed 500r/
Min, mixing time 0.5h；
Step 3: taking 0.0711g cetyl trimethylammonium bromide (CTAB) to be added in above-mentioned solution, controls mass ratio
mSodium tungstate: mCTAB=10:1；
Step 4: concentrated nitric acid is diluted to the clear solution B of 3mol/L, solution B is added drop-wise in solution A, makes its solution
PH value is 1.4, and acquired solution is solution C；
Step 5: above-mentioned solution C being transferred in microwave hydrothermal kettle, water heating kettle is then sealed, and is put it into high-throughput super
High-pressure microwave is cleared up in instrument, and control microwave hydrothermal temperature is 180 DEG C, pressure 8MPa, reaction time 0.5h, after reaction
Cooled to room temperature.
Step 6: opening microwave reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifuged point
From it is -60 DEG C that repeated washing 6 times, which are placed on temperature, and vacuum degree is dry 10h in 20Pa freeze drier, obtains black
WO3/ GO composite material.
Step 7: resulting WO is taken3/ GO powder is as tungsten source, and thioacetamide is as sulphur source, mole in tungsten source and sulphur source
Than for 1:15, tungsten source taken amount is 0.2g, and 900 DEG C of calcination temperature, soaking time 2h obtains WS2/ GO composite material.
Embodiment 3
Step 1: under room temperature, ultrasound 5h to formation uniform solution A in 60mL deionized water is added in 75mg GO.It is super
Acoustical power is 500W
Step 2: 0.825g Disodium tungstate (Na2WO4) dihydrate being added in solution A and is stirred to being completely dissolved, mixing speed 600r/
Min, mixing time 1h；
Step 3: taking 0.0825g cetyl trimethylammonium bromide (CTAB) to be added in above-mentioned solution, controls mass ratio
mSodium tungstate: mCTAB=10:1；
Step 4: concentrated nitric acid is diluted to the clear solution B of 2mol/L, solution B is added drop-wise in solution A, makes its solution
PH value is 1.5, and acquired solution is solution C；
Step 5: above-mentioned solution C being transferred in microwave hydrothermal kettle, water heating kettle is then sealed, and is put it into high-throughput super
High-pressure microwave is cleared up in instrument, and control microwave hydrothermal temperature is 160 DEG C, pressure 5MPa, reaction time 4h, after reaction certainly
So it is cooled to room temperature.
Step 6: opening microwave reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifuged point
From it is -70 DEG C that repeated washing 4 times, which are placed on temperature, and vacuum degree is dry 12h in 30Pa freeze drier, obtains black
WO3/ GO composite material.
Step 7: resulting WO is taken3/ GO powder is as tungsten source, and thioacetamide is as sulphur source, mole in tungsten source and sulphur source
Than for 1:20, tungsten source taken amount is 0.2g, and 900 DEG C of calcination temperature, soaking time 2h obtains WS2/ GO composite material.
Referring to figure 1, figure 2 and figure 3, sample (WS is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2/ GO is compound
Material), the WS for the hexagonal crystal system that discovery sample is 08-0237 with JCPDS number2Structure is consistent, illustrates that this method can be made pure
The WS of phase2.The sample is observed with field emission scanning electron microscope (FESEM), it can be seen that prepared WS2/ GO is multiple
Condensation material product dispersibility is preferably.
Referring to fig. 4, as sodium-ion battery, in 100mA g-1With 1A g-1Current density under carry out electrochemistry
It can test, it can be seen that WS prepared by the present invention2/ GO composite material is under high current during charge and discharge after 150 circle of circulation
Substantially do not decline, capacity can also be maintained at 300mAh g-1, show excellent chemical property.
Embodiment 4
Step 1: under room temperature, ultrasound 2h to formation uniform solution A in 45mL deionized water is added in 40mg GO.It is super
Acoustical power is 1000W
Step 2: 1.28g Disodium tungstate (Na2WO4) dihydrate being added in solution A and is stirred to being completely dissolved, mixing speed 400r/
Min, mixing time 1h；
Step 3: taking 0.128g cetyl trimethylammonium bromide (CTAB) to be added in above-mentioned solution, controls mass ratio
mSodium tungstate: mCTAB=10:1；
Step 4: concentrated nitric acid is diluted to the clear solution B of 1mol/L, solution B is added drop-wise in solution A, makes its solution
PH value is 1.7, and acquired solution is solution C；
Step 5: above-mentioned solution C being transferred in microwave hydrothermal kettle, water heating kettle is then sealed, and is put it into high-throughput super
High-pressure microwave is cleared up in instrument, and control microwave hydrothermal temperature is 150 DEG C, pressure 4MPa, reaction time 2.5h, after reaction
Cooled to room temperature.
Step 6: opening microwave reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifuged point
From it is -60 DEG C that repeated washing 5 times, which are placed on temperature, and vacuum degree is dry 12h in 10Pa freeze drier, obtains black
WO3/ GO composite material.
Step 7: resulting WO is taken3/ GO powder is as tungsten source, and thioacetamide is as sulphur source, mole in tungsten source and sulphur source
Than for 1:16, tungsten source taken amount is 0.5g, and 800 DEG C of calcination temperature, soaking time 2h obtains WS2/ GO composite material.
Embodiment 5
Step 1: under room temperature, ultrasound 3h to formation uniform solution A in 55mL deionized water is added in 30mg GO.It is super
Acoustical power is 600W
Step 2: 1.65g Disodium tungstate (Na2WO4) dihydrate being added in solution A and is stirred to being completely dissolved, mixing speed 500r/
Min, mixing time 0.5h；
Step 3: taking 0.165g cetyl trimethylammonium bromide (CTAB) to be added in above-mentioned solution, controls mass ratio
mSodium tungstate: mCTAB=10:1；
Step 4: concentrated nitric acid is diluted to the clear solution B of 1mol/L, solution B is added drop-wise in solution A, makes its solution
PH value is 1.6, and acquired solution is solution C；
Step 5: above-mentioned solution C being transferred in microwave hydrothermal kettle, water heating kettle is then sealed, and is put it into high-throughput super
High-pressure microwave is cleared up in instrument, and control microwave hydrothermal temperature is 180 DEG C, pressure 3MPa, reaction time 1.5h, after reaction
Cooled to room temperature.
Step 6: opening microwave reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifuged point
From it is -70 DEG C that repeated washing 6 times, which are placed on temperature, and vacuum degree is dry 12h in 15Pa freeze drier, obtains black
WO3/ GO composite material.
Step 7: resulting WO is taken3/ GO powder is as tungsten source, and thioacetamide is as sulphur source, mole in tungsten source and sulphur source
Than for 1:12, tungsten source taken amount is 0.3g, and 700 DEG C of calcination temperature, soaking time 2h obtains WS2/ GO composite material.
Embodiment 6
Step 1: under room temperature, ultrasound 3h to formation uniform solution A in 55mL deionized water is added in 30mg GO.It is super
Acoustical power is 600W
Step 2: 1.65g Disodium tungstate (Na2WO4) dihydrate being added in solution A and is stirred to being completely dissolved, mixing speed 500r/
Min, mixing time 0.5h；
Step 3: taking 0.495g cetyl trimethylammonium bromide (CTAB) to be added in above-mentioned solution, controls mass ratio
mSodium tungstate: mCTAB=10:3；
Step 4: concentrated nitric acid is diluted to the clear solution B of 1mol/L, solution B is added drop-wise in solution A, makes its solution
PH value is 1.5, and acquired solution is solution C；
Step 5: above-mentioned solution C being transferred in microwave hydrothermal kettle, water heating kettle is then sealed, and is put it into high-throughput super
High-pressure microwave is cleared up in instrument, and control microwave hydrothermal temperature is 170 DEG C, pressure 0MPa, reaction time 2h, after reaction certainly
So it is cooled to room temperature.
Step 6: opening microwave reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifuged point
From it is -70 DEG C that repeated washing 6 times, which are placed on temperature, and vacuum degree is dry 12h in 15Pa freeze drier, obtains black
WO3/ GO composite material.
Step 7: resulting WO is taken3/ GO powder is as tungsten source, and thioacetamide is as sulphur source, mole in tungsten source and sulphur source
Than for 1:12, tungsten source taken amount is 0.3g, and 600 DEG C of calcination temperature, soaking time 3h obtains WS2/ GO composite material.
Embodiment 7
Step 1: under room temperature, ultrasound 3h to formation uniform solution A in 55mL deionized water is added in 30mg GO.It is super
Acoustical power is 600W
Step 2: 0.618g Disodium tungstate (Na2WO4) dihydrate being added in solution A and is stirred to being completely dissolved, mixing speed 500r/
Min, mixing time 0.5h；
Step 3: taking 0.1236g cetyl trimethylammonium bromide (CTAB) to be added in above-mentioned solution, controls mass ratio
mSodium tungstate: mCTAB=10:2；
Step 4: concentrated nitric acid is diluted to the clear solution B of 1mol/L, solution B is added drop-wise in solution A, makes its solution
PH value is 1.45, and acquired solution is solution C；
Step 5: above-mentioned solution C being transferred in microwave hydrothermal kettle, water heating kettle is then sealed, and is put it into high-throughput super
High-pressure microwave is cleared up in instrument, and control microwave hydrothermal temperature is 180 DEG C, pressure 0.5MPa, reaction time 3h, after reaction
Cooled to room temperature.
Step 6: opening microwave reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifuged point
From it is -70 DEG C that repeated washing 6 times, which are placed on temperature, and vacuum degree is dry 12h in 15Pa freeze drier, obtains black
WO3/ GO composite material.
Step 7: resulting WO is taken3/ GO powder is as tungsten source, and thioacetamide is as sulphur source, mole in tungsten source and sulphur source
Than for 1:12, tungsten source taken amount is 0.3g, and 800 DEG C of calcination temperature, soaking time 1h obtains WS2/ GO composite material.
For the present invention using Disodium tungstate (Na2WO4) dihydrate as tungsten source, sulphur source is thioacetamide；WS is prepared for using two-step method2/ GO is multiple
Condensation material, preparation process is simple, and technological parameter is easy to control, and repeatability is high, uses WS made from this method2/ GO composite material exists
There are wide researching value and application value in electrochemical field.
Claims (7)
1. a kind of tungsten disulfide/GO combination electrode material preparation method, which comprises the following steps:
Step 1: GO is add to deionized water ultrasound to uniform solution A is formed, Disodium tungstate (Na2WO4) dihydrate is then added, stirs
Uniformly, cetyl trimethylammonium bromide is added, adjusting pH value is 1.3~1.7, is 0~10MPa, 120~180 in pressure
Microwave hydrothermal is carried out at DEG C and reacts 0.5~4h, is washed, it is dry, obtain WO3/ GO powder；
Step 2: being in molar ratio 1:(10~20), by WO3/ GO powder is mixed with thioacetamide, is then calcined, and two sulphur are obtained
Change tungsten/GO combination electrode material.
2. a kind of preparation method of tungsten disulfide/GO combination electrode material according to claim 1, which is characterized in that molten
The concentration of GO is 0.5~3mol/L in liquid A；The mass ratio of Disodium tungstate (Na2WO4) dihydrate and GO are 0.618~1.65g:25~75mg；Two
The mass ratio of tungstic acid hydrate sodium and cetyl trimethylammonium bromide is 10:(1~3).
3. a kind of preparation method of tungsten disulfide/GO combination electrode material according to claim 1, which is characterized in that stir
The speed mixed is 400~600r/min, 0.5~1h of time of stirring.
4. a kind of preparation method of tungsten disulfide/GO combination electrode material according to claim 1, which is characterized in that super
The power of sound is 300~1000W, and the time is 2~5h.
5. a kind of preparation method of tungsten disulfide/GO combination electrode material according to claim 1, which is characterized in that adopt
It is 1.3~1.7 with the nitre acid for adjusting pH value of 1~3mol/L.
6. a kind of preparation method of tungsten disulfide/GO combination electrode material according to claim 1, which is characterized in that micro-
Wave hydro-thermal reaction carries out in high-throughput super-pressure microwave dissolver.
7. a kind of preparation method of tungsten disulfide/GO combination electrode material according to claim 1, which is characterized in that forge
The temperature of burning is 600~900 DEG C, and the time is 1~3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811279164.7A CN109326787B (en) | 2018-10-30 | 2018-10-30 | Preparation method of tungsten disulfide/GO composite electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811279164.7A CN109326787B (en) | 2018-10-30 | 2018-10-30 | Preparation method of tungsten disulfide/GO composite electrode material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109326787A true CN109326787A (en) | 2019-02-12 |
| CN109326787B CN109326787B (en) | 2021-08-10 |
Family
ID=65259945
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811279164.7A Active CN109326787B (en) | 2018-10-30 | 2018-10-30 | Preparation method of tungsten disulfide/GO composite electrode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109326787B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110526296A (en) * | 2019-09-26 | 2019-12-03 | 东华大学 | A kind of preparation method of the tungsten disulfide composite film electrode of doped carbon nanometer pipe |
| CN110880597A (en) * | 2019-11-28 | 2020-03-13 | 陕西科技大学 | Tungsten sulfide/CNTs @ C composite electrode material and preparation method thereof |
| CN111411010A (en) * | 2020-04-08 | 2020-07-14 | 扬州大学 | WS (WS)2Nanoproheet-based lubricating grease and preparation method thereof |
| CN111477855A (en) * | 2020-04-24 | 2020-07-31 | 喻明兵 | Mesoporous carbon coated MoS2The negative electrode material of the sodium ion battery and the preparation method thereof |
| CN111874950A (en) * | 2020-07-31 | 2020-11-03 | 陕西科技大学 | Vanadium-doped tungsten disulfide/graphene oxide composite electrode material and preparation method and application thereof |
| CN111874962A (en) * | 2020-07-31 | 2020-11-03 | 陕西科技大学 | Nickel-doped tungsten disulfide/graphene oxide composite electrode material and preparation method and application thereof |
| CN112018352A (en) * | 2020-08-13 | 2020-12-01 | 五邑大学 | WSe2Mxene composite material and preparation method thereof |
| CN112397699A (en) * | 2020-11-16 | 2021-02-23 | 西北大学 | Transition metal chalcogenide/carbon composite material rich in anion vacancies and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641173A (en) * | 2013-11-04 | 2014-03-19 | 江苏大学 | Preparation method of graphite alkene like tungsten disulfide nanometer sheet |
| CN105870417A (en) * | 2016-04-27 | 2016-08-17 | 中南大学 | Preparation method for tungsten disulfide/carbon nanotube negative electrode composite material of sodium ion battery |
| CN106941168A (en) * | 2017-04-19 | 2017-07-11 | 扬州大学 | A kind of column GO@WO3The preparation method of@S composites |
| US20170342578A1 (en) * | 2014-11-11 | 2017-11-30 | William Marsh Rice University | A new class of electrocatalysts |
| CN108428565A (en) * | 2017-02-13 | 2018-08-21 | 中国科学院宁波材料技术与工程研究所 | Tungsten disulfide/graphene oxide composite material, preparation method and application |
| CN108565434A (en) * | 2018-05-02 | 2018-09-21 | 南昌大学 | A kind of preparation method of tungsten disulfide/nitrogen sulphur codope graphene complex |
-
2018
- 2018-10-30 CN CN201811279164.7A patent/CN109326787B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641173A (en) * | 2013-11-04 | 2014-03-19 | 江苏大学 | Preparation method of graphite alkene like tungsten disulfide nanometer sheet |
| US20170342578A1 (en) * | 2014-11-11 | 2017-11-30 | William Marsh Rice University | A new class of electrocatalysts |
| CN105870417A (en) * | 2016-04-27 | 2016-08-17 | 中南大学 | Preparation method for tungsten disulfide/carbon nanotube negative electrode composite material of sodium ion battery |
| CN108428565A (en) * | 2017-02-13 | 2018-08-21 | 中国科学院宁波材料技术与工程研究所 | Tungsten disulfide/graphene oxide composite material, preparation method and application |
| CN106941168A (en) * | 2017-04-19 | 2017-07-11 | 扬州大学 | A kind of column GO@WO3The preparation method of@S composites |
| CN108565434A (en) * | 2018-05-02 | 2018-09-21 | 南昌大学 | A kind of preparation method of tungsten disulfide/nitrogen sulphur codope graphene complex |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110526296A (en) * | 2019-09-26 | 2019-12-03 | 东华大学 | A kind of preparation method of the tungsten disulfide composite film electrode of doped carbon nanometer pipe |
| CN110880597A (en) * | 2019-11-28 | 2020-03-13 | 陕西科技大学 | Tungsten sulfide/CNTs @ C composite electrode material and preparation method thereof |
| CN111411010A (en) * | 2020-04-08 | 2020-07-14 | 扬州大学 | WS (WS)2Nanoproheet-based lubricating grease and preparation method thereof |
| CN111411010B (en) * | 2020-04-08 | 2022-03-15 | 扬州大学 | WS (WS)2Nanoproheet-based lubricating grease and preparation method thereof |
| CN111477855A (en) * | 2020-04-24 | 2020-07-31 | 喻明兵 | Mesoporous carbon coated MoS2The negative electrode material of the sodium ion battery and the preparation method thereof |
| CN111874950A (en) * | 2020-07-31 | 2020-11-03 | 陕西科技大学 | Vanadium-doped tungsten disulfide/graphene oxide composite electrode material and preparation method and application thereof |
| CN111874962A (en) * | 2020-07-31 | 2020-11-03 | 陕西科技大学 | Nickel-doped tungsten disulfide/graphene oxide composite electrode material and preparation method and application thereof |
| CN111874950B (en) * | 2020-07-31 | 2022-07-29 | 陕西科技大学 | Vanadium-doped tungsten disulfide/graphene oxide composite electrode material and preparation method and application thereof |
| CN112018352A (en) * | 2020-08-13 | 2020-12-01 | 五邑大学 | WSe2Mxene composite material and preparation method thereof |
| CN112397699A (en) * | 2020-11-16 | 2021-02-23 | 西北大学 | Transition metal chalcogenide/carbon composite material rich in anion vacancies and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109326787B (en) | 2021-08-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109326787A (en) | A kind of preparation method of tungsten disulfide/GO combination electrode material | |
| Nulu et al. | Silicon and porous MWCNT composite as high capacity anode for lithium-ion batteries | |
| CN108269982B (en) | Composite material, preparation method thereof and application thereof in lithium ion battery | |
| CN109449411B (en) | Method for synthesizing tungsten disulfide @ C composite electrode material in limited domain | |
| CN105118965B (en) | Sodium-ion battery negative pole SnO2The preparation method of/pyrolysis carbon electrode material | |
| Liu et al. | Synthesis of coral-like Fe 2 N@ C nanoparticles and application in sodium ion batteries as a novel anode electrode material | |
| CN110729463A (en) | Lithium-sulfur battery positive electrode material containing three-dimensional interpenetrating composite carbon material, preparation method of lithium-sulfur battery positive electrode material, positive electrode plate containing lithium-sulfur battery positive electrode material and lithium-sulfur battery | |
| CN109742353A (en) | A kind of SnSe quantum dot/r-GO compound and its preparation method and application | |
| Yang et al. | Self-assembled FeF3 nanocrystals clusters confined in carbon nanocages for high-performance Li-ion battery cathode | |
| CN109956500A (en) | A kind of preparation method of the molybdenum disulfide material of the nano flower-like for lithium sode cell cathode | |
| CN111276679A (en) | Double-carbon composite molybdenum sulfide composite material for sodium ion battery cathode material and preparation method thereof | |
| CN106058249A (en) | Method for preparing carbon coated nano rodlike sodium ferrous phosphate material by solvent thermal | |
| Zhao et al. | Hierarchical flower-like spinel manganese-based oxide nanosheets for high-performance lithium ion battery | |
| CN104577126A (en) | Method for preparing MWCNT@a-C@Co9S8 composite electrode material with uniform morphology and application of material in lithium electrode | |
| Feng et al. | Core–shell structured MnSiO 3 supported with CNTs as a high capacity anode for lithium-ion batteries | |
| CN113517427B (en) | Preparation method and application of carbon-coated antimony/antimony trisulfide composite material | |
| CN105845920B (en) | A kind of high circulation stability nanometer rods self assembly molybdenum trioxide material and preparation method thereof | |
| Hu et al. | A new method of synthesis of Sb 2 Se 3/rGO as a high-rate and low-temperature anode for sodium–ion batteries | |
| Fan et al. | In situ growth of NiS2 nanosheet array on Ni foil as cathode to improve the performance of lithium/sodium-sulfur batteries | |
| Ji et al. | Electrochemical characterization of CuF2/CNTs cathode materials prepared by a coprecipitation method | |
| CN106981626B (en) | A kind of preparation method of tungsten disulfide/Super P sodium-ion battery self-supporting cathode | |
| CN111799458B (en) | Tin elemental composite tungsten disulfide/reduced graphene oxide composite electrode material and preparation method and application thereof | |
| CN107140609B (en) | A kind of method that microwave hydrothermal prepares sodium-ion battery cathode pencil antimony selenide electrode material | |
| CN106848280B (en) | A kind of preparation method of the hollow octahedra anode material for lithium-ion batteries of graphene-supported di iron | |
| Bai et al. | Hierarchical Ti3C2/TiO2/MoS2 Composite as an Anode Material for Sodium-ion Batteries |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |