CN109326787B - Preparation method of tungsten disulfide/GO composite electrode material - Google Patents

Preparation method of tungsten disulfide/GO composite electrode material Download PDF

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CN109326787B
CN109326787B CN201811279164.7A CN201811279164A CN109326787B CN 109326787 B CN109326787 B CN 109326787B CN 201811279164 A CN201811279164 A CN 201811279164A CN 109326787 B CN109326787 B CN 109326787B
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tungsten disulfide
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CN109326787A (en
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黄剑锋
罗晓敏
曹丽云
李嘉胤
席乔
郭玲
王蓉
王芳敏
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Shaanxi University of Science and Technology
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    • 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

Abstract

Adding GO into deionized water to form a solution A, then adding sodium tungstate dihydrate, uniformly stirring, then adding hexadecyl trimethyl ammonium bromide, adjusting the pH value to be 1.3-1.7, and carrying out microwave hydrothermal reaction at the pressure of 0-10 MPa and the temperature of 120-180 ℃ to obtain WO3GO powder; mixing WO3And mixing the/GO powder with thioacetamide, and then calcining to obtain the tungsten disulfide/GO composite electrode material. The invention takes sodium tungstate dihydrate as a tungsten source, and a sulfur source as thioacetamide; the WS is obtained by controlling the concentration of the precursor solution by a microwave hydrothermal method and under the action of a template agent2The composite material synthesized by the method is used as a cathode material of the sodium ion battery, and is beneficial to electron transmission, so that the electrochemical performance of the battery is improved.

Description

Preparation method of tungsten disulfide/GO composite electrode material
Technical Field
The present invention relates to WS2The technical field of nano material preparation, in particular to a preparation method of a tungsten disulfide/GO composite electrode material.
Background
WS2As a transition metal chalcogenide MX2(M ═ Mo, W; (X ═ S, Se), and MoS2Has similar structural characteristics and is hexagonalPhase graphene-like layered structure with large interlayer spacing
Figure BDA0001847687590000011
The layered structure can promote the reaction of active substances and electrolyte, increase active sites, enable the process of sodium ion insertion and extraction to be smoother, and finally improve the electrochemical performance. But the material has a larger volume expansion problem in the charging and discharging process, so that the cycling stability of the material is poor. And the material itself has poor conductivity, which is not conducive to electron transport. At present, the common solution to the problem of volume expansion is to synthesize a composite material using carbon as a matrix, relieve the stress generated in the volume expansion process, and enhance the conductivity of the material.
According to the report of the literature, the carbon material is used as the matrix, which is beneficial to the transmission of electrons and can effectively improve the electrochemical performance of the composite material as the negative electrode material of the lithium ion battery. For example, Guowei Huang et al compounds tungsten disulfide with graphene oxide in three dimensions (Huang G, Liu H, Wang S, et al, hierarchical architecture of WS2nanosheets on graphene frames with enhanced electrochemical properties for lithium storage and hydrogen evolution [ J]Journal of Materials Chemistry A,2015,3(47): 24128-24138) as the negative electrode material of the lithium ion battery, the electrochemical performance of the tungsten disulfide after being compounded is greatly improved, the tungsten disulfide is cycled for 100 circles under the current density of 100mA/g, and the capacity of the tungsten disulfide is kept at 766 mAh/g. The compound material of tungsten disulfide and three-dimensional single-walled carbon nanotube is used as the cathode material of lithium ion battery (Ren J, Wang Z, Yang F, et al free and 3D single-walled carbon nanotubes/WS)2,nanosheets foams as ultra-long-life anodes for rechargeable lithium ion batteries[J]Electrochimica acta,2018.), greatly improves the cycling stability of the material, the material circulates for 1000 circles under the current density of 1A/g, and the capacity is stabilized at 688.9 mAh/g. However, the electrochemical performance of the sodium ion battery is to be improved.
Disclosure of Invention
The invention aims to provide a preparation method of a tungsten disulfide/GO composite electrode material, which utilizes a hydrothermal method to control precursor liquidConcentration and with the aid of a templating agent, WS2Composite product of/GO, WS prepared according to the invention2the/GO composite product has good dispersibility, uniform size and uniform appearance, and has great potential in the application of sodium ion battery cathodes.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a tungsten disulfide/GO composite electrode material comprises the following steps:
the method comprises the following steps: adding GO into deionized water, performing ultrasonic treatment to form a uniform solution A, adding sodium tungstate dihydrate, stirring uniformly, adding hexadecyl trimethyl ammonium bromide, adjusting the pH value to be 1.3-1.7, performing microwave hydrothermal reaction for 0.5-4 h at the pressure of 0-10 MPa and the temperature of 120-180 ℃, washing, and drying to obtain WO3GO powder;
step two: according to the molar ratio of 1 (10-20), adding WO3And mixing the/GO powder with thioacetamide, and then calcining to obtain the tungsten disulfide/GO composite electrode material.
The invention has the further improvement that the concentration of GO in the solution A is 0.5-3 mol/L; the mass ratio of sodium tungstate dihydrate to GO is 0.618-1.65 g: 25-75 mg; the mass ratio of the sodium tungstate dihydrate to the hexadecyl trimethyl ammonium bromide is 10 (1-3).
The invention has the further improvement that the stirring speed is 400-600 r/min, and the stirring time is 0.5-1 h.
The invention has the further improvement that the power of the ultrasonic wave is 300-1000W, and the time is 2-5 h.
The further improvement of the invention is that 1-3 mol/L nitric acid is adopted to adjust the pH value to 1.3-1.7.
The invention is further improved in that the microwave hydrothermal reaction is carried out in a high-flux ultrahigh-pressure microwave digestion instrument.
The further improvement of the invention is that the calcining temperature is 600-900 ℃ and the time is 1-3 h.
Compared with the prior art, the invention has the following beneficial effects: the invention takes sodium tungstate dihydrate as a tungsten source, and a sulfur source as thioacetamide; by usingThe microwave hydrothermal method obtains WS by controlling the concentration of the precursor solution and under the auxiliary action of a template agent of hexadecyl trimethyl ammonium bromide2the/GO composite product has simple preparation process, easily controlled process parameters and high repeatability, and the WS prepared by the method2the/GO composite material has wide research value and application value in the electrochemical field. The composite material taking carbon as a matrix is synthesized to be used as the cathode material of the sodium-ion battery, so that the electron transmission is facilitated, and the electrochemical performance of the battery is improved.
Drawings
FIG. 1 shows WS prepared in example 32An X-ray diffraction (XRD) pattern of the/GO composite material;
FIG. 2 shows WS prepared in example 32Scanning Electron Microscope (SEM) pictures of/GO composites;
FIG. 3 shows WS prepared in example 32Transmission Electron Microscope (TEM) pictures of/GO composites;
FIG. 4 shows WS prepared in example 32Cycle performance profile of/GO composite.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Example 1
The method comprises the following steps: at room temperature, 25mg of GO is added into 45mL of deionized water and is subjected to ultrasonic treatment for 2 hours until a uniform solution A is formed. The ultrasonic power is 300W;
step two: adding 0.618g of sodium tungstate dihydrate into the solution A, and stirring for 0.5h at the stirring speed of 500r/min until the sodium tungstate dihydrate is completely dissolved;
step three: adding 0.0618g Cetyl Trimethyl Ammonium Bromide (CTAB) into the solution, controlling mass ratio mSodium tungstate：mCTAB＝10:1；
Step four: diluting concentrated nitric acid into a transparent solution B of 3mol/L, and dropwise adding the solution B into the solution to enable the pH value of the solution to be 1.3, wherein the obtained solution is a solution C;
step five: and transferring the solution C into a microwave hydrothermal kettle, sealing the hydrothermal kettle, putting the hydrothermal kettle into a high-flux ultrahigh-pressure microwave digestion instrument, controlling the microwave hydrothermal temperature at 120 ℃, the pressure at 1MPa and the reaction time at 2h, and naturally cooling to room temperature after the reaction is finished.
Step six: opening the microwave reaction kettle, taking out the product, sequentially washing with anhydrous ethanol and deionized water, centrifuging, washing for 4 times, drying in a freeze dryer at-40 deg.C and vacuum degree of 40Pa for 12 hr to obtain black WO3a/GO composite material.
Step seven: taking the obtained WO3The tungsten source is 0.3g of tungsten source, the calcination temperature is 900 ℃, the heat preservation time is 2h, and the WS is obtained2a/GO composite material.
Example 2
The method comprises the following steps: at room temperature, 50mg of GO was added to 50mL of deionized water and sonicated for 4h to form a homogeneous solution A. The ultrasonic power is 800W
Step two: adding 0.711g of sodium tungstate dihydrate into the solution A, and stirring for 0.5h at the stirring speed of 500r/min until the sodium tungstate dihydrate is completely dissolved;
step three: 0.0711g of cetyltrimethylammonium bromide (CTAB) are added into the solution, and the mass ratio m is controlledSodium tungstate：mCTAB＝10:1；
Step four: diluting concentrated nitric acid into a transparent solution B of 3mol/L, dropwise adding the solution B into the solution A to enable the pH value of the solution to be 1.4, and obtaining a solution C;
step five: and transferring the solution C into a microwave hydrothermal kettle, sealing the hydrothermal kettle, putting the hydrothermal kettle into a high-flux ultrahigh-pressure microwave digestion instrument, controlling the microwave hydrothermal temperature at 180 ℃, the pressure at 8MPa and the reaction time at 0.5h, and naturally cooling to room temperature after the reaction is finished.
Step six: opening the microwave reaction kettle, taking out the product, sequentially washing with anhydrous ethanol and deionized water, centrifuging, repeatedly washing for 6 times, drying in a freeze dryer at-60 deg.C and vacuum degree of 20Pa for 10 hr to obtain black WO3a/GO composite material.
Step seven: taking the obtained WO3the/GO powder is used as a tungsten source, and thioacetamide is used asSulfur source, the molar ratio of tungsten source to sulfur source is 1:15, the amount of tungsten source is 0.2g, the calcining temperature is 900 ℃, the holding time is 2h, and WS is obtained2a/GO composite material.
Example 3
The method comprises the following steps: at room temperature, 75mg of GO was added to 60mL of deionized water and sonicated for 5h to form a homogeneous solution A. The ultrasonic power is 500W
Step two: adding 0.825g of sodium tungstate dihydrate into the solution A, and stirring for 1h at the stirring speed of 600r/min until the sodium tungstate dihydrate is completely dissolved;
step three: 0.0825g hexadecyl trimethyl ammonium bromide (CTAB) is added into the solution, and the mass ratio m is controlledSodium tungstate：mCTAB＝10:1；
Step four: diluting concentrated nitric acid into a transparent solution B with the concentration of 2mol/L, dropwise adding the solution B into the solution A to enable the pH value of the solution A to be 1.5, and obtaining a solution C;
step five: and transferring the solution C into a microwave hydrothermal kettle, sealing the hydrothermal kettle, putting the hydrothermal kettle into a high-flux ultrahigh-pressure microwave digestion instrument, controlling the microwave hydrothermal temperature at 160 ℃, the pressure at 5MPa and the reaction time at 4h, and naturally cooling to room temperature after the reaction is finished.
Step six: opening the microwave reaction kettle, taking out the product, sequentially washing with anhydrous ethanol and deionized water, centrifuging, washing for 4 times, drying in a freeze dryer at-70 deg.C and vacuum degree of 30Pa for 12 hr to obtain black WO3a/GO composite material.
Step seven: taking the obtained WO3The tungsten source is 0.2g, the calcination temperature is 900 ℃, the heat preservation time is 2h, and the WS is obtained2a/GO composite material.
Referring to FIGS. 1, 2 and 3, the samples were analyzed by a Japanese science D/max2000 PCX-ray diffractometer (WS)2/GO composite) found with WS of hexagonal system with JCPDS numbers 08-02372The structures are consistent, which shows that the method can prepare pure-phase WS2. The sample was observed with a Field Emission Scanning Electron Microscope (FESEM)To see the WS prepared2The product of the/GO composite material has better dispersibility.
Referring to FIG. 4, it is used as a sodium ion battery at 100mA g-1And 1A g-1The current density of the prepared WS is tested, and the WS can be seen2the/GO composite material is not reduced basically after circulating for 150 circles in the process of charging and discharging under high current, and the capacity can be kept at 300mAh g-1And shows excellent electrochemical performance.
Example 4
The method comprises the following steps: at room temperature, 40mg of GO is added into 45mL of deionized water and is subjected to ultrasonic treatment for 2h until a uniform solution A is formed. The ultrasonic power is 1000W
Step two: adding 1.28g of sodium tungstate dihydrate into the solution A, and stirring for 1h at the stirring speed of 400r/min until the sodium tungstate dihydrate is completely dissolved;
step three: adding 0.128g Cetyl Trimethyl Ammonium Bromide (CTAB) into the above solution, and controlling mass ratio mSodium tungstate：mCTAB＝10:1；
Step four: diluting concentrated nitric acid into a transparent solution B with the concentration of 1mol/L, dropwise adding the solution B into the solution A to enable the pH value of the solution to be 1.7, and obtaining a solution C;
step five: and transferring the solution C into a microwave hydrothermal kettle, sealing the hydrothermal kettle, putting the hydrothermal kettle into a high-flux ultrahigh-pressure microwave digestion instrument, controlling the microwave hydrothermal temperature at 150 ℃, the pressure at 4MPa and the reaction time at 2.5h, and naturally cooling to room temperature after the reaction is finished.
Step six: opening the microwave reaction kettle, taking out the product, sequentially washing with anhydrous ethanol and deionized water, centrifuging, washing for 5 times, drying in a freeze dryer at-60 deg.C and vacuum degree of 10Pa for 12 hr to obtain black WO3a/GO composite material.
Step seven: taking the obtained WO3The tungsten source is 0.5g, the calcination temperature is 800 ℃, the heat preservation time is 2h, and the WS is obtained2a/GO composite material.
Example 5
The method comprises the following steps: at room temperature, 30mg of GO was added to 55mL of deionized water and sonicated for 3h to form a homogeneous solution A. The ultrasonic power is 600W
Step two: adding 1.65g of sodium tungstate dihydrate into the solution A, and stirring for 0.5h at the stirring speed of 500r/min until the sodium tungstate dihydrate is completely dissolved;
step three: 0.165g of cetyltrimethylammonium bromide (CTAB) is added into the above solution, and the mass ratio m is controlledSodium tungstate：mCTAB＝10:1；
Step four: diluting concentrated nitric acid into a transparent solution B with the concentration of 1mol/L, dropwise adding the solution B into the solution A to enable the pH value of the solution to be 1.6, and obtaining a solution C;
step five: and transferring the solution C into a microwave hydrothermal kettle, sealing the hydrothermal kettle, putting the hydrothermal kettle into a high-flux ultrahigh-pressure microwave digestion instrument, controlling the microwave hydrothermal temperature at 180 ℃, the pressure at 3MPa and the reaction time at 1.5h, and naturally cooling to room temperature after the reaction is finished.
Step six: opening the microwave reaction kettle, taking out the product, sequentially washing with anhydrous ethanol and deionized water, centrifuging, repeatedly washing for 6 times, drying in a freeze dryer at-70 deg.C and vacuum degree of 15Pa for 12 hr to obtain black WO3a/GO composite material.
Step seven: taking the obtained WO3The tungsten source is 0.3g, the calcination temperature is 700 ℃, and the heat preservation time is 2h to obtain WS2a/GO composite material.
Example 6
The method comprises the following steps: at room temperature, 30mg of GO was added to 55mL of deionized water and sonicated for 3h to form a homogeneous solution A. The ultrasonic power is 600W
Step two: adding 1.65g of sodium tungstate dihydrate into the solution A, and stirring for 0.5h at the stirring speed of 500r/min until the sodium tungstate dihydrate is completely dissolved;
step three: 0.495g of hexadecyl trimethyl ammonium bromide (CTAB) is added into the solution, and the mass ratio m is controlledSodium tungstate：mCTAB＝10:3；
Step four: diluting concentrated nitric acid into a transparent solution B with the concentration of 1mol/L, dropwise adding the solution B into the solution A to enable the pH value of the solution to be 1.5, and obtaining a solution C;
step five: and transferring the solution C into a microwave hydrothermal kettle, sealing the hydrothermal kettle, putting the hydrothermal kettle into a high-flux ultrahigh-pressure microwave digestion instrument, controlling the microwave hydrothermal temperature at 170 ℃, the pressure at 0MPa and the reaction time at 2h, and naturally cooling to room temperature after the reaction is finished.
Step six: opening the microwave reaction kettle, taking out the product, sequentially washing with anhydrous ethanol and deionized water, centrifuging, repeatedly washing for 6 times, drying in a freeze dryer at-70 deg.C and vacuum degree of 15Pa for 12 hr to obtain black WO3a/GO composite material.
Step seven: taking the obtained WO3The tungsten source is 0.3g, the calcination temperature is 600 ℃, the heat preservation time is 3h, and the WS is obtained2a/GO composite material.
Example 7
The method comprises the following steps: at room temperature, 30mg of GO was added to 55mL of deionized water and sonicated for 3h to form a homogeneous solution A. The ultrasonic power is 600W
Step two: adding 0.618g of sodium tungstate dihydrate into the solution A, and stirring for 0.5h at the stirring speed of 500r/min until the sodium tungstate dihydrate is completely dissolved;
step three: 0.1236g of cetyltrimethylammonium bromide (CTAB) are added into the solution, and the mass ratio m is controlledSodium tungstate：mCTAB＝10:2；
Step four: diluting concentrated nitric acid into a transparent solution B with the concentration of 1mol/L, dropwise adding the solution B into the solution A to enable the pH value of the solution to be 1.45, and obtaining a solution C;
step five: and transferring the solution C into a microwave hydrothermal kettle, sealing the hydrothermal kettle, putting the hydrothermal kettle into a high-flux ultrahigh-pressure microwave digestion instrument, controlling the microwave hydrothermal temperature at 180 ℃, the pressure at 0.5MPa and the reaction time at 3h, and naturally cooling to room temperature after the reaction is finished.
Step (ii) ofSixthly, the method comprises the following steps: opening the microwave reaction kettle, taking out the product, sequentially washing with anhydrous ethanol and deionized water, centrifuging, repeatedly washing for 6 times, drying in a freeze dryer at-70 deg.C and vacuum degree of 15Pa for 12 hr to obtain black WO3a/GO composite material.
Step seven: taking the obtained WO3The tungsten source is 0.3g, the calcination temperature is 800 ℃, the heat preservation time is 1h, and the WS is obtained2a/GO composite material.
The invention takes sodium tungstate dihydrate as a tungsten source, and a sulfur source as thioacetamide; adopts a two-step method to prepare WS2the/GO composite material has simple preparation process, easily controlled process parameters and high repeatability, and the WS prepared by the method2the/GO composite material has wide research value and application value in the electrochemical field.

Claims (6)

1. A preparation method of a tungsten disulfide/GO composite electrode material is characterized by comprising the following steps:
the method comprises the following steps: adding GO into deionized water, performing ultrasonic treatment to form a uniform solution A, adding sodium tungstate dihydrate, stirring uniformly, adding hexadecyl trimethyl ammonium bromide, adjusting the pH value to be 1.3-1.7, performing microwave hydrothermal reaction for 0.5-4 h at the pressure of 0-10 MPa and the temperature of 120-180 ℃, washing, and drying to obtain WO3GO powder;
step two: according to the molar ratio of 1 (10-20), adding WO3mixing/GO powder with thioacetamide, and then calcining to obtain a tungsten disulfide/GO composite electrode material;
the concentration of GO in the solution A is 0.5-3 mol/L; the mass ratio of sodium tungstate dihydrate to GO is 0.618-1.65 g: 25-75 mg; the mass ratio of the sodium tungstate dihydrate to the hexadecyl trimethyl ammonium bromide is 10 (1-3).
2. The preparation method of the tungsten disulfide/GO composite electrode material as claimed in claim 1, wherein the stirring speed is 400-600 r/min and the stirring time is 0.5-1 h.
3. The preparation method of the tungsten disulfide/GO composite electrode material as claimed in claim 1, wherein the power of ultrasound is 300-1000W, and the time is 2-5 h.
4. The preparation method of the tungsten disulfide/GO composite electrode material as claimed in claim 1, wherein 1-3 mol/L nitric acid is used to adjust the pH value to 1.3-1.7.
5. The preparation method of the tungsten disulfide/GO composite electrode material according to claim 1, wherein the microwave hydrothermal reaction is carried out in a high-throughput ultrahigh-pressure microwave digestion instrument.
6. The preparation method of the tungsten disulfide/GO composite electrode material as claimed in claim 1, wherein the calcination temperature is 600-900 ℃ and the time is 1-3 h.
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Citations (5)

* Cited by examiner, † Cited by third party
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
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

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016122741A2 (en) * 2014-11-11 2016-08-04 William March Rice University A new class of electrocatalysts

Patent Citations (5)

* Cited by examiner, † Cited by third party
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
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

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