CN102701283A - Preparation method of tungsten disulfide nanorods - Google Patents
Preparation method of tungsten disulfide nanorods Download PDFInfo
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- CN102701283A CN102701283A CN2012101496170A CN201210149617A CN102701283A CN 102701283 A CN102701283 A CN 102701283A CN 2012101496170 A CN2012101496170 A CN 2012101496170A CN 201210149617 A CN201210149617 A CN 201210149617A CN 102701283 A CN102701283 A CN 102701283A
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Abstract
The invention relates to a preparation method of tungsten disulfide nanorods, belonging to the technical field of nano material preparation. The method provided by the invention comprises the following steps: (1) preparing a solution, that is, dissolving (NH4) 2WO4, CS (NH2) 2, NH2OH.HCl and a surfactant in water to obtain a solution, and then adjusting the pH value of the solution by acid to 5 to 6.5; (2) after stirring the solution obtained in the step (1), moving the solution into a stainless steel reaction kettle, sealing the solution, after thermostatic reaction, cooling the solution to room temperature, and obtaining a reaction product; and (3) separating, washing and drying the above reaction product to obtain tungsten disulfide nanorods. The tungsten disulfide nanorod prepared by the invention is uniform and controllable in particle size. The method disclosed by the invention is simple in process, low in cost, high in the purity of the obtained product, and high in yield, and has important applications in tribology, photochemistry and the like, and can be used for large-scale industrial production hopefully.
Description
Technical field
The invention belongs to the nano material preparation technical field, particularly, the present invention relates to a kind of preparation method of Wolfram disulfide nano bar.
Background technology
Nano structural material has unique physics, chemistry, electricity, magnetics and mechanical property.Because it has advantages such as density is little, specific surface area is big, it has the potential application prospect in fields such as packing material, medicine transmission, catalysis.Therefore, carry out the preparation research of this type of material, have very important significance.Existing research shows, the disulphide of transition metal has unique character, and they can be used as the cathode material etc. of photochromics, catalyzer, lubricant, high energy battery.
Tungsten disulfide (WS
2) have the laminate structure of similar graphite flake layer, be very strong covalent linkage in the layer, interlayer then is very weak Van der Waals Er Sili, layer is easy to peel off with layer, has good anisotropy and lower frictional coefficient.WS
2Because of it has unique physicochemical property, and in industrial production, be used widely, for example solid lubricant, petrochemical complex are produced desulfurization catalyst, elastic coating material, hydrogen storage material, storage lithium electrode material, shortening etc.
Be used to prepare nanometer WS so far
2Method mainly contain elevated temperature heat reaction (gas-solid reaction, solid state sintering etc.) and low-temperature solvent thermal synthesis method (hydrothermal method, solution chemistry reaction etc.).People adopt the elevated temperature heat reaction method to prepare WS
2Nanotube, nanometer sheet, nanometer flower etc., and WS
2The pertinent literature report of nanometer rod is less, and the prior art cost is high, complex process; And adopting the synthetic cost of low temperature lower, pattern is controlled relatively, but relevant report is less.
CN1793304A has announced and has a kind ofly utilized solvent-induced effect to prepare WS
2The method of nanometer rod.This method adopts planetary high-energy ball mill, with the WS of common micron order laminate structure
2Powder and micron order S powder mixing and ball milling obtain nanometer lamella form presoma, in reaction kettle, add the dispersion agent polyoxyethylene glycol then, and controlled temperature to room temperature, has synthesized WS at 10～30 hours postcooling of 200 ℃～260 ℃ insulations
2Nanometer rod.
Zhang Lili is at its Master's thesis (Zhang Lili, WS
2The preparation of nanometer rod and as the tribological property of oil dope, Zhejiang University's Master's thesis, 2006) reported a kind of preparation method of Wolfram disulfide nano bar.Adopt chemical precipitation-doctor treatment and ball milling-doctor treatment, prepare inorganic fullerene abbreviation IF tungsten disulfide ball milling-transform legal system certainly and be equipped with WS
2Nanometer rod is promptly used ball milling WS
2Prepare presoma with the method for the mixed powder of S, in autoclave, under the condition of 240 ℃ of insulation 24h, prepare WS then
2Nanometer rod.
Prior art processes needs preparation presoma earlier, technology more complicated, and WS usually
2The particle diameter heterogeneity of nanometer rod, and the pattern controllable degree is poor, influences it in Application for Field such as tribology, photochemistry.
Summary of the invention
To the deficiency of prior art, one of the object of the invention is to provide a kind of preparation method of Wolfram disulfide nano bar.
The present invention adopts hydrothermal synthesis method, and the preparation method of said Wolfram disulfide nano bar may further comprise the steps:
(1) obtain solution: with (NH
4)
2WO
4, CS (NH
2)
2, NH
2OHHCl and tensio-active agent are soluble in water, and dissolving obtains solution, and the pH value of using acid-conditioning solution again is 5 ~ 6.5;
(2) after the solution stirring that step (1) is obtained, move into stainless steel cauldron, sealing after the isothermal reaction, is cooled to room temperature, obtains reaction product;
(3) separate above-mentioned reaction product, washing, drying obtain the Wolfram disulfide nano bar of black.
(NH
4)
2WO
4Be tungsten source, CS (NH
2)
2Be sulphur source, (NH
4)
2WO
4With CS (NH
2)
2Reaction generates sulfo-ammonium tungstate, NH
2OHHCl reacts as reductive agent and sulfo-ammonium tungstate, obtains tungsten disulfide.Said (NH
4)
2WO
4, CS (NH
2)
2, NH
2The ratio of OHHCl amount of substance is 0.5 ~ 1.5:2.5 ~ 3.5:1.5 ~ 2.5; For example 0.6:2.6:1.6,0.7:2.7:1.7,0.8:2.8:1.8,0.9:2.9:1.9,1.4:3.4:2.4,1.3:3.3:2.3,1.2:3.2:2.2; Preferred 1.0 ~ 1.5:3.0 ~ 3.5:2.0 ~ 2.5, further preferred 1:3:2.
Tensio-active agent can play the effect that suppresses nanoparticle agglomerates as dispersion agent.Said tensio-active agent and (NH
4)
2WO
4The ratio of amount of substance be 1:4 ~ 11, for example 1:4.5,1:5,1:5.5,1:6,1:6.5,1:7:, 1:7.5,1:8,1:8.5,1:9,1:10, preferred 1:5 ~ 11, further preferred 1:11.Said tensio-active agent is selected from the mixture of a kind of in non-ionics, cats product, the AS or at least two kinds.Said mixture is non-ionics/cats product, nonionogenic tenside/AS, cats product/AS for example, non-ionics/cats product/AS.Said non-ionics, cats product, AS do not have concrete restriction, and the non-ionics that those skilled in the art can be known, cats product, AS all can be realized the present invention.For example can select non-ionics PEG for use, cats product CTAB, AS SDBS.
Need the pH value with acid-conditioning solution among the present invention, wherein, said acid is hydrochloric acid, and the amount concentration of preferred substance is the hydrochloric acid of 2mol/L.
The time of said stirring is 20 ~ 50min, for example 22min, 24min, 26min, 28min, 48min, 46min, 44min, preferred 25 ~ 45min, further preferred 30min.The temperature of said isothermal reaction is 140 ℃ ~ 200 ℃, for example 145 ℃, 155 ℃, 160 ℃, 165 ℃, 170 ℃, 175 ℃, 185 ℃, 195 ℃, and preferred 180 ℃ ~ 200 ℃, further preferred 180 ℃.
The time of isothermal reaction is 24h at least, for example 25h, 25.5h, 26h, 26.5h, 27h, 27.5h, 28h, 28.5h, 29h, 29.5h, 35h, 38h, preferred 24h ~ 30h, further preferred 24h.
Preferred said isothermal reaction is carried out under vacuum condition.
The volume of said water is 60% ~ 90% of a reaction kettle volume, for example 62%, 64%, 66%, 68%, 88%, 86%, 84%, 82%, and preferred 60% ~ 80%, further preferred 70%.
The mode of said sealing is restriction not, and any mode that can reach sealed reactor that those skilled in the art can be known all can realize the present invention, for example, can adopt teflon seal among the present invention.
Said separation is selected from the combination of a kind of in filtration, deposition, centrifugal, the distillation or at least two kinds.Said combination for example precipitates and filtering combination, filters and the centrifugal combination, and centrifugal and distillatory combination, filtration, deposition and centrifugal combination, deposition, centrifugal and distillatory combination, preferably centrifugal and filtering combination, further preferably centrifugal.
Those skilled in the art can select cleaning solvent based on the knowledge of oneself grasping, and among the present invention, as preferred version, deionized water and absolute ethanol washing are adopted in said washing.
Preferably; Said drying is selected from the combination of a kind of in spraying drying, forced air drying, microwave drying, infrared drying, the vacuum-drying or at least two kinds, and said combination is the combination of spraying drying and forced air drying for example, the combination of forced air drying and microwave drying; The combination of microwave drying and infrared drying; Infrared drying and vacuum drying combination, the combination of preferred vacuum-drying and forced air drying, further preferred vacuum-drying.
Preferably, said vacuum drying temperature is 50 ℃ ~ 90 ℃, preferred 60 ~ 80 ℃, and further preferred 80 ℃.
Another object of the present invention is to provide a kind of Wolfram disulfide nano bar that obtains by method for preparing, said nanometer rod uniform particle diameter, particle diameter and pattern are controlled.
Six side's laminate structure characteristics of the Wolfram disulfide nano bar for preparing through the present invention are distinct, and crystallization is complete.The nanometer rod uniform particle diameter, and in the preparation process, do not have agglomeration.
The Wolfram disulfide nano bar for preparing through the present invention has very low frictional coefficient; Higher anti-extreme pressure ability and antioxidant property; It is applicable to lubricating under the various severe condition such as high temperature, high pressure, high vacuum, high loading, high rotating speed, high radiation, deep-etching, very low temperature as lubricant.
The inventive method technology is simple, and raw material is easy to get, and is with low cost, and the product purity for preparing is high, productive rate is high, and in fields such as tribology, photochemistry, has important use, is expected to be used for large-scale industrial production.
Compared with prior art, the present invention has following advantage:
(1) the present invention adopts one step hydro thermal method synthetic, and introduces tensio-active agent, has simplified process step;
(2) the present invention selects NH for use
2OHHCl is a reductive agent, and in reaction, it is oxidized to gases such as nitrogen, water and nitrogen protoxide, can not bring impurity to reaction, has improved the purity of final product;
(3) adding of tensio-active agent makes WS among the present invention
2The particle diameter of nanometer rod and pattern can be controlled, and laminate structure is obvious, and have higher specific surface area and frictional behaviour.
Description of drawings
Be further described below in conjunction with the accompanying drawing specific embodiments of the invention.
Fig. 1: the XRD spectra of the Wolfram disulfide nano bar that the embodiment of the invention 1 prepares;
Fig. 2: the microscopic appearance picture of the Wolfram disulfide nano bar that the embodiment of the invention 1 prepares; Wherein Fig. 2 a and Fig. 2 b are field emission scanning electron microscope (SEM) photo of Wolfram disulfide nano bar, and Fig. 2 c and 2d are transmission electron microscope (TEM) photo of Wolfram disulfide nano bar;
Fig. 3: the Wolfram disulfide nano bar that the present invention prepares is as the tribological property comparison diagram of oil dope, and Fig. 3 a is the frictional coefficient figure under the different loads, and Fig. 3 b is the frictional coefficient figure under the different rotating speeds.
Embodiment
For ease of understanding the present invention, it is following that the present invention enumerates embodiment.Those skilled in the art should understand, and said embodiment helps to understand the present invention, should not be regarded as concrete restriction of the present invention.Can know that by technological general knowledge the present invention also can describe through other the scheme that does not break away from technical characterictic of the present invention, thus all within the scope of the present invention or the change that is equal in the scope of the invention all comprised by the present invention.
0.18g CTAB is dissolved in the zero(ppm) water of 70ml, adds 1.40g CS (NH then
2)
2, 0.725gNH
2OHHCl and 1.56g (NH
4)
2WO
4After the dissolving, use 2molL more fully
-1HCl regulate about pH value to 6.After stirring 30min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven, be cooled to room temperature in 180 ℃ of insulation 24h.Reaction product is used deionized water and absolute ethyl alcohol repetitive scrubbing respectively after spinning, last under vacuum condition 80 ℃ of dry 10h obtain the product powder of grey black, be Wolfram disulfide nano bar.
XRD figure spectrum explanation XRD peak position and the standard diffractogram (JCPDS84-1398) of Fig. 1 are consistent, and product is pure WS
2Hexagonal, the XRD peak value of (002) face among the figure is very strong, and WS is explained in other peak position reductions
2Six side's laminate structure characteristics distinct, more complete along the crystallization of (002) face.Fig. 2 (a, b) is the SEM photo of product, can see obviously that the nanometer rod of a large amount of homogeneous generates no agglomeration.Fig. 2 (c, d) is the TEM photo of product, and further specifying product is that diameter is about 20～100nm, the WS between length 0.1～2um
2Nanometer rod, and laminate structure is obvious.
Embodiment 2:
0.30g PEG600 is dissolved in the zero(ppm) water of 70ml, adds 1.40g CS (NH then
2)
2, 0.725gNH
2OHHCl and 1.56g (NH
4)
2WO
4After the dissolving, use 2molL more fully
-1HCl regulate about pH value to 6.After stirring 30min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven, be cooled to room temperature in 180 ℃ of insulation 24h.Reaction product is used deionized water and absolute ethyl alcohol repetitive scrubbing respectively after spinning, last under vacuum condition 80 ℃ of dry 10h obtain the product powder of grey black, be Wolfram disulfide nano bar.
Embodiment 3:
0.17g SDBS is dissolved in the zero(ppm) water of 70ml, adds 1.40g CS (NH then
2)
2, 0.725gNH
2OHHCl and 1.56g (NH
4)
2WO
4After the dissolving, use 2molL more fully
-1HCl regulate about pH value to 6.After stirring 30min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven, be cooled to room temperature in 180 ℃ of insulation 24h.Reaction product is used deionized water and absolute ethyl alcohol repetitive scrubbing respectively after spinning, last under vacuum condition 80 ℃ of dry 10h obtain the product powder of grey black, be Wolfram disulfide nano bar.
Embodiment 4
0.44g SDBS is dissolved in the zero(ppm) water of 60ml, adds 1.90g CS (NH then
2)
2, 1.09gNH
2OHHCl and 1.45g (NH
4)
2WO
4After the dissolving, use 2molL more fully
-1HCl regulate about pH value to 5.After stirring 20min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven, be cooled to room temperature in 140 ℃ of insulation 30h.After product is separated after filtration, use deionized water and absolute ethyl alcohol cyclic washing respectively, last under vacuum condition 50 ℃ of dry 12h obtain the product powder of grey black.
0.68g CTAB is dissolved in the zero(ppm) water of 90ml, adds 2.66g CS (NH then
2)
2, 1.81gNH
2OHHCl and 4.34g (NH
4)
2WO
4After the dissolving, use 2molL more fully
-1HCl regulate about pH value to 6.5.After stirring 50min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven, be cooled to room temperature in 200 ℃ of insulation 28h.Reaction product is used deionized water and absolute ethyl alcohol repetitive scrubbing respectively after spinning, last under vacuum condition 90 ℃ of dry 8h obtain the product powder of grey black, be Wolfram disulfide nano bar.
Embodiment 6
0.44g SDBS is dissolved in the zero(ppm) water of 60ml, adds 1.90g CS (NH then
2)
2, 1.09gNH
2OHHCl and 1.45g (NH
4)
2WO
4After the dissolving, use 2molL more fully
-1HCl regulate about pH value to 5.2.After stirring 40min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven, be cooled to room temperature in 160 ℃ of insulation 32h.Reaction product is used deionized water and absolute ethyl alcohol repetitive scrubbing respectively after filtering separation, forced air drying obtains the product powder of grey black, is Wolfram disulfide nano bar.
The frictional behaviour test
Utilize ultrasonic generator with dispersion agent span 80 and WS
2Nanometer rod is distributed in the base oil uniformly, is mixed with to contain WS
2Massfraction is that 1% muddy liquid oil sample frictional experiment carries out on CETR UMT-2 multifunction friction wear testing machine.Adopt ball-disc type contact, rotating speed is 5～25mmin
-1, load is 0.6kg～4.1kg, experimental period is 30min.Testing used Stainless Steel Ball model is 440-C (9Cr18), and diameter is 3mm, and hardness is HRC62.
Fig. 3 is that the Wolfram disulfide nano bar that the present invention prepares adds in the base oil and base oil, and is identical in load, that rotating speed is different is identical with rotating speed, frictional behaviour experiment comparison diagram under the load various conditions.Experimental data explanation WS among the figure
2Nanometer rod can effectively reduce frictional coefficient as oil dope, has played the effect that improves the lubricating oil frictional behaviour.
Applicant's statement; The present invention explains detailed process equipment of the present invention and technical process through the foregoing description; But the present invention is not limited to above-mentioned detailed process equipment and technical process, does not mean that promptly the present invention must rely on above-mentioned detailed process equipment and technical process could be implemented.The person of ordinary skill in the field should understand, and to any improvement of the present invention, to the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (10)
1. the preparation method of a Wolfram disulfide nano bar is characterized in that, said method comprising the steps of:
(1) obtain solution: with (NH
4)
2WO
4, CS (NH
2)
2, NH
2OHHCl and tensio-active agent are soluble in water, and dissolving obtains solution, and the pH value of using acid-conditioning solution again is 5 ~ 6.5;
(2) after the solution stirring that step (1) is obtained, move into stainless steel cauldron, sealing after the isothermal reaction, is cooled to room temperature, obtains reaction product;
(3) separate above-mentioned reaction product, washing, drying obtain Wolfram disulfide nano bar.
2. method according to claim 1 is characterized in that, said (NH
4)
2WO
4, CS (NH
2)
2, NH
2The ratio of the amount of substance of OHHCl is 0.5 ~ 1.5:2.5 ~ 3.5:1.5 ~ 2.5, preferred 1.0 ~ 1.5:3.0 ~ 3.5:1.0 ~ 2.5, further preferred 1:3:2.
3. method according to claim 1 and 2 is characterized in that, said tensio-active agent and (NH
4)
2WO
4The ratio of amount of substance be 1:4 ~ 11, preferred 1:5 ~ 11, further preferred 1:11;
Preferably, said tensio-active agent is selected from the mixture of a kind of in non-ionics, cats product, the AS or at least two kinds.
4. according to each described method of claim 1-3, it is characterized in that said acid is hydrochloric acid, the amount concentration of preferred substance is the hydrochloric acid of 2mol/L.
5. according to each described method of claim 1-4, it is characterized in that said churning time is 20 ~ 50min, preferred 25 ~ 45min, further preferred 30min;
Preferably, the temperature of said isothermal reaction is 140 ℃ ~ 200 ℃, preferred 180 ℃ ~ 200 ℃, and further preferred 180 ℃.
6. according to each described method of claim 1-5, it is characterized in that the time of said isothermal reaction is 24h at least, preferred 24h ~ 30h, further preferred 24h;
Preferably, said isothermal reaction is carried out under vacuum condition.
7. according to each described method of claim 1-6, it is characterized in that the volume of said water is 60% ~ 90% of a reaction kettle volume, preferred 60% ~ 80%, further preferred 70%.
8. according to each described method of claim 1-7, it is characterized in that said separation is selected from the combination of a kind of in filtration, deposition, centrifugal, the distillation or at least two kinds, preferred centrifugal and filtering combination is further preferably centrifugal;
Preferably, deionized water and absolute ethanol washing are adopted in said washing.
9. according to each described method of claim 1-8; It is characterized in that; Said drying is selected from the combination of a kind of in spraying drying, forced air drying, microwave drying, infrared drying, the vacuum-drying or at least two kinds; The combination of preferred vacuum-drying and forced air drying, further preferred vacuum-drying;
Preferably, said vacuum drying temperature is 50 ℃ ~ 90 ℃, preferred 60 ~ 80 ℃, and further preferred 80 ℃.
10. a Wolfram disulfide nano bar that is prepared by each said method of claim 1-9 is characterized in that, said nanometer rod uniform particle diameter, and particle diameter and pattern are controlled.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925866A (en) * | 2015-06-08 | 2015-09-23 | 陕西科技大学 | Preparation method of rod-like WS2 nanocrystal with high length-diameter ratio |
| CN104953119A (en) * | 2015-06-08 | 2015-09-30 | 陕西科技大学 | Preparation method for two-dimensional matrix rod-like WS2 anode material |
| CN104993141A (en) * | 2015-06-08 | 2015-10-21 | 陕西科技大学 | Preparation method for one-dimensional WS2 nanotube negative electrode material for sodium-ion battery |
| CN104993140A (en) * | 2015-06-08 | 2015-10-21 | 陕西科技大学 | Preparation method of fibriform WS2 nanometer anode material |
| CN105502502A (en) * | 2016-01-07 | 2016-04-20 | 重庆文理学院 | Preparation method of tungsten disulfide nanorod |
| CN108773855A (en) * | 2018-05-07 | 2018-11-09 | 昆明理工大学 | A kind of preparation method of tungsten sulfide positive electrode |
| CN108822937A (en) * | 2018-07-17 | 2018-11-16 | 昆山中润信息科技有限公司 | High abrasion resistant extreme-pressure and antiwear and antifriction lubricating oil |
| CN109019689A (en) * | 2018-07-11 | 2018-12-18 | 昆明理工大学 | A kind of preparation method and application of nanometer of tungsten trisulfide |
| CN109378470A (en) * | 2018-09-19 | 2019-02-22 | 昆明理工大学 | A kind of preparation method of vanadium doping tungsten disulfide negative electrode material |
| CN110683581A (en) * | 2018-07-04 | 2020-01-14 | 湖北大学 | Self-assembly thousand-layer-shaped WS2Method for preparing nano structure |
| CN111661877A (en) * | 2020-07-01 | 2020-09-15 | 松山湖材料实验室 | Preparation method of tungsten disulfide/carbon composite nanorod, product and application thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925866A (en) * | 2015-06-08 | 2015-09-23 | 陕西科技大学 | Preparation method of rod-like WS2 nanocrystal with high length-diameter ratio |
| CN104953119A (en) * | 2015-06-08 | 2015-09-30 | 陕西科技大学 | Preparation method for two-dimensional matrix rod-like WS2 anode material |
| CN104993141A (en) * | 2015-06-08 | 2015-10-21 | 陕西科技大学 | Preparation method for one-dimensional WS2 nanotube negative electrode material for sodium-ion battery |
| CN104993140A (en) * | 2015-06-08 | 2015-10-21 | 陕西科技大学 | Preparation method of fibriform WS2 nanometer anode material |
| CN104993140B (en) * | 2015-06-08 | 2017-10-27 | 陕西科技大学 | A kind of fibrous WS2The preparation method of nanometer anode material |
| CN105502502A (en) * | 2016-01-07 | 2016-04-20 | 重庆文理学院 | Preparation method of tungsten disulfide nanorod |
| CN108773855A (en) * | 2018-05-07 | 2018-11-09 | 昆明理工大学 | A kind of preparation method of tungsten sulfide positive electrode |
| CN110683581A (en) * | 2018-07-04 | 2020-01-14 | 湖北大学 | Self-assembly thousand-layer-shaped WS2Method for preparing nano structure |
| CN109019689A (en) * | 2018-07-11 | 2018-12-18 | 昆明理工大学 | A kind of preparation method and application of nanometer of tungsten trisulfide |
| CN108822937A (en) * | 2018-07-17 | 2018-11-16 | 昆山中润信息科技有限公司 | High abrasion resistant extreme-pressure and antiwear and antifriction lubricating oil |
| CN109378470A (en) * | 2018-09-19 | 2019-02-22 | 昆明理工大学 | A kind of preparation method of vanadium doping tungsten disulfide negative electrode material |
| CN109378470B (en) * | 2018-09-19 | 2021-06-18 | 昆明理工大学 | Preparation method of vanadium-doped tungsten disulfide negative electrode material |
| CN111661877A (en) * | 2020-07-01 | 2020-09-15 | 松山湖材料实验室 | Preparation method of tungsten disulfide/carbon composite nanorod, product and application thereof |
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