CN101234785A - Method for preparing nano molybdenum disulfide with fullerene structure - Google Patents
Method for preparing nano molybdenum disulfide with fullerene structure Download PDFInfo
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- CN101234785A CN101234785A CNA2008100175320A CN200810017532A CN101234785A CN 101234785 A CN101234785 A CN 101234785A CN A2008100175320 A CNA2008100175320 A CN A2008100175320A CN 200810017532 A CN200810017532 A CN 200810017532A CN 101234785 A CN101234785 A CN 101234785A
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Abstract
The invention discloses a method for preparing nano molybdenum disulphide with a fullerene structure. The method comprises the following steps sequentially: by using industrial molybdenum trioxide as raw material, argon as carrier gas and hydrogen as reducing agent, molybdenum dioxide nano particle is generated by gas-phase reaction; the nano molybdenum disulphide and elemental sulfur are reacted under the condition of high temperature self-pressurization to produce powder material of the nano molybdenum disulphide with the fullerene structure; the molybdenum dioxide is nano particle generated directly by the reaction of the molybdenum trioxide after gasification under 700 to 1,000 DEG C with the hydrogen under 400 to 950 DEG C; the molybdenum disulphide with the fullerene structure is compound molybdenum disulphide by the self-pressurization reaction of the nano molybdenum dioxide and elemental sulfur in a vessel under 500 to 950 DEG C. The method for preparing the nano molybdenum disulphide with the fullerene structure has the advantages of simple process, high production efficiency, low cost of the raw material and product and short reaction time and the method can easily control the size of the molybdenum dioxide nano particle.
Description
Technical field
The present invention relates to a kind of preparation method with nano molybdenum disulfide of fullerene structure.
Background technology
As everyone knows, be subjected to the inspiration of carbon nanotube, the scientist R.Tenne of Israel Zi Man Wei academy of sciences leader's research group has started the frontier of non-carbon inorganic fullerene nano materials research, and to adopt fluidized-bed process be presoma with corresponding nano grade transition metal oxide compound, realized that inorganic fullerene transient metal sulfide nano material maroscopic quantity is synthetic.
Prior art is except that the solid and gas reaction synthesis method, and its synthesis of carbon/molybdenum disulfide nano material also has a lot of methods, for example laser splash and arc discharge method, ultrasonic wave electrochemical synthesis method, hydrothermal synthesis method, template, self-assembly method or the like.
In all aforesaid methods, the solid and gas reaction method has the possibility of industrialization, so be the important research method of industrialization.The patented technology that the Israel scientist has applied for relevant this respect in China, wherein 01806119.2 relates to a kind of reactor and method that is used to produce inorganic fullerene (IF) nano particle and nanotube.Described equipment comprises a chemical reactor, and further with in apparatus for feeding and the controlling reactor links to each other along the temperature controlling instruments of the temperature of reaction channel, and is constant basically to cause temperature maintenance.This invention also relates to a kind of synthetic IF-WS
2The method of nano particle and nanotube, described nano particle are spherical, and it is of a size of 0.01 until 0.5 micron, and the length of described nanotube is 0.1 up to hundreds of microns, and its sectional dimension is up to 200 nanometers.This equipment is for being arranged vertically structure, and is the apparatus and method of producing WS2 fullerene structure material.This method distinct issues are long reaction times, the cost height.
The method of application (patent) number a kind of mass production molybdenumdisulphide fullerene nano structural material of 03110897.0 proposition, it is characterized in that: with metal molybdenum nano powder and commercial sulphur powder is raw material, at 500-950 ℃, under the 1000-15000Pa pressure atmosphere, solid state reaction prepares MoS
2The fullerene nano structural material; Described atmosphere is Ar and H
2S or Ar and H
2Gas mixture, wherein Ar accounts for 1-20%; The mol ratio of described metal molybdenum nano powder and sulphur powder is between 10-0.05.This invention production rate is fast, and it is few to consume hydrogen sulfide, the product epigranular.This method distinct issues are will obtain the metal molybdenum of nanometer and be not easy, and the cost height, the easy spontaneous combustion of nanometer molybdenum powder, and difficulty operates.
Application (patent) number: 01817955.X enumerates the method and apparatus that is used to prepare the inorganic fullerene nanostructure.Under predetermined temperature condition, make the metal oxide vaporization, and deliver to conversion zone, simultaneously first and second reagents are sent into conversion zone.Therefore the metal oxide of vaporization and first reagent interact, and change into metal suboxide nanoparticles in gas phase.The metal suboxide nanoparticles of condensing in gas phase and second reagent interact, and generate the inorganic fullerene-like nanoparticles of pure phase basically.The problem of this method still is a long reaction time, the cost height.
Application (patent) number: 200510050405.7 disclose the preparation method and the application of inorganic fullerene molybdenum disulfide.Preparation method's step is as follows: 1) that sodium sulphite and molybdenum acid ammonia 1: 5 by mass percentage～8 is soluble in water, two kinds of compounds are fully reacted, the polyoxyethylene glycol aqueous solution of concentration 5～10% that adds 10～30 times of theoretical obtainable molybdenum trisulfide quality simultaneously is as dispersion agent, with the above-mentioned solution of salt acidometric titration, obtain the brown precipitate molybdenum trisulfide; 2) with the molybdenum trisulfide precipitation and centrifugal separation; after the vacuum-drying, in quartz tube furnace under the argon shield atmosphere, hydrogen desulfurization under 500～1000 ℃ of temperature; and be incubated 5～10 hours, obtain to have the inorganic spherical fullerene molybdenum disulfide nano particle of nested stratiform enclosed construction.The inorganic fullerene molybdenum disulfide additive in lubricating oil, can be improved the fastness to wear of lubricating oil, reduce its frictional coefficient, reduce energy consumption, the work-ing life of prolonged mechanical part.The outstanding problem of this method is to use industrial chemicals, complex process, cost height.
Application (patent) number: the preparation method of the inorganic fullerene structured molybdenium disulfide in 200510028674.3 1 kinds of material technology fields, with four thio ammonium molybdate is raw material, with the four thio ammonium molybdate aqueous solution with spray-dired method drying, make the ultra-fine forerunner's particle of molybdenum trisulfide, then the molybdenum trisulfide particle is heated under the environment of hydrogen and argon gas mixed gas, molybdenum trisulfide is reduced to fullerene structure molybdenumdisulphide particle.The present invention has prepared the inorganic fullerene molybdenum disulfide particle of magnanimity by simple and effective chemical synthesis process, and method is simply quick, and granularity is convenient to control, for it provides in tribology and otherwise widespread use may.This method is used industrial chemicals, complex process, cost height.
It more than is the relevant patent of up-to-date molybdenum disulfide nano material synthetic, therefrom as can be seen, realize that large-scale fullerene structure molybdenumdisulphide compound industryization also has certain distance, all having distinct issues in above-mentioned all patents is that cost is too high, is unfavorable for defectives such as industrialization production.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, and a kind of preparation method with nano molybdenum disulfide of fullerene structure that a kind of cost is low, be suitable for scale operation is provided.
In order to overcome the defective that prior art exists, technical scheme of the present invention is to solve like this: a kind of preparation method with nano molybdenum disulfide of fullerene structure, and its special character is that its preparation process is to adopt two-step approach, is undertaken by following step successively:
1) being raw material with industrial molybdic oxide, at first, is carrier gas with the argon gas, and hydrogen is reductive agent, generates the molybdenum dioxide particle of nanometer through gas-phase reaction;
2), the molybdenumdisulphide and the elemental sulfur of nanometer reacted, generate nano molybdenum disulfide powder body material with fullerene structure under the condition of high temperature self-pressurization;
3), described molybdenum dioxide is that molybdic oxide is after 700-1000 ℃ of gasification, react the nano particle that directly generates with hydrogen at 400-950 ℃, next, the molybdenumdisulphide of fullerene structure is that the molybdenum dioxide and the elemental sulfur of nanometer reacts synthetic by self-pressurization in container under 500-950 ℃ temperature;
4), the building-up reactions of described nanometer titanium dioxide molybdenum is carried out in the silica tube in stove, adopt two independently silica tube be respectively applied for hydrogen and transport with molybdic oxide and gasify, molybdic oxide that gasifies in reaction chamber and hydrogen mix, reduction reaction takes place, and nanometer titanium dioxide molybdenum product is that the interior porcelain filter of the silica tube in the reduction reaction furnace obtains;
5), the molybdenum dioxide of its nanometer and elemental sulfur produce the molybdenumdisulphide of the final fullerene synthesis structure of self-pressurization by the gasification of elemental sulfur in closed reactor under 500-950 ℃ temperature in heatable metal vessel.The consumption of the Heating temperature of the pressure of above-mentioned said self-pressurization and compressive reaction container, vessel volume, elemental sulfur is relevant.
The present invention compared with prior art has following characteristics:
Method of the present invention utilizes low-cost commodity molybdic oxide to be raw material, and argon gas is carrier gas, and hydrogen is reductive agent, and the synthetic molybdenum dioxide cost of adopting quartz glass reactor is low, the reaction efficiency height, and the molybdenum dioxide nanoparticle size is controlled easily.
Adopt high temperature self-pressurization method, utilize the reaction of nanometer titanium dioxide molybdenum and elemental sulfur, raw materials cost is low, the reaction yield height, and the reaction times is short.
Processing method of the present invention, overcome long drawback of fullerene structure gas-phase reaction time, make an external step gas phase synthesis method into two-step approach, promptly utilize vapor phase process synthesis oxide nanoparticle size to control easily, it is the first step that the fast advantage of reduction reaction is synthesized molybdenum dioxide; Utilize the each charging capacity of high temperature self-pressurization method big, sufficient reacting, the advantage synthesis of carbon/molybdenum disulfide that productive rate is high was second step, pass through two-step approach, can realize fully that magnanimity prepares the nano molybdenum disulfide of fullerene structure, reduced preparation cost, significant for the industrialization preparation of fullerene structure molybdenumdisulphide with application.
Description of drawings
Fig. 1 is the preparation facilities structural representation of nanometer titanium dioxide molybdenum;
Fig. 2 is a fullerene structure nano molybdenum disulfide synthesizer synoptic diagram.
Embodiment
Accompanying drawing is embodiments of the invention.
Below in conjunction with drawings and Examples summary of the invention is described further:
Figure 1 shows that the preparation facilities structural representation of nanometer titanium dioxide molybdenum, this device is made up of the tube furnace of two platform independent heating, and wherein the 1# stove is the vapourizing furnace of molybdic oxide, and the 2# stove is the reduction reaction furnace of molybdenum dioxide.
Two quartz glass tubes pass after the 1# stove, in the 2# stove, join, the 1# stove provides molybdic oxide gas, control the amount of vaporization of molybdic oxide by the gasification temperature of control carrier gas flux and 1# stove, control the reduction reaction temperature condition of molybdenum dioxide by the temperature of control 2# stove, the molybdenum dioxide of generation deposits on the porcelain filter in the silica tube in the 2# stove, after reduction reaction is finished, the 2# stove takes out after cooling to room temperature, obtains nanometer titanium dioxide molybdenum product.
Fullerene structure nano molybdenum disulfide synthesis process is as follows:
Shown in Figure 2, at first with in the self-pressurization reaction vessel among elemental sulfur and nanometer titanium dioxide molybdenum placement Fig. 2, after adopting nitrogen or argon gas to drive the interior air of container out of, encloses container, the airtight self-pressurization reaction vessel that elemental sulfur and nanometer titanium dioxide molybdenum will be housed again places High Temperature Furnaces Heating Apparatus, by High Temperature Furnaces Heating Apparatus is heated up, is incubated and cooling, take out reaction vessel, open the molybdenumdisulphide product that can obtain fullerene structure.
Embodiment 1
A kind of preparation method with nano molybdenum disulfide of fullerene structure, its preparation process adopt two-step approach, are undertaken by following step successively:
1) being raw material with industrial molybdic oxide, at first, is carrier gas with the argon gas, and hydrogen is reductive agent, generates the molybdenum dioxide particle of nanometer through gas-phase reaction;
2), the molybdenumdisulphide and the elemental sulfur of nanometer reacted, generate nano molybdenum disulfide powder body material with fullerene structure under the condition of high temperature self-pressurization;
3), described molybdenum dioxide is that molybdic oxide is after 700-1000 ℃ of gasification, react the nano particle that directly generates with hydrogen at 400-950 ℃, next, the molybdenumdisulphide of fullerene structure is that the molybdenum dioxide and the elemental sulfur of nanometer reacts synthetic by self-pressurization in container under 500-950 ℃ temperature;
4), the building-up reactions of described nanometer titanium dioxide molybdenum is carried out in the silica tube in stove, adopt two independently silica tube be respectively applied for hydrogen and transport with molybdic oxide and gasify, molybdic oxide that gasifies in reaction chamber and hydrogen mix, reduction reaction takes place, and nanometer titanium dioxide molybdenum product is that the interior porcelain filter of the silica tube in the reduction reaction furnace obtains;
5), the molybdenum dioxide of its nanometer and elemental sulfur produce the molybdenumdisulphide of the final fullerene synthesis structure of self-pressurization by the gasification of elemental sulfur in closed reactor under 500-950 ℃ temperature in heatable metal vessel.
Embodiment 2
Described a kind of preparation method with nano molybdenum disulfide of fullerene structure, undertaken by following step successively:
1) being raw material with industrial molybdic oxide, at first, is carrier gas with the argon gas, and hydrogen is reductive agent, generates the molybdenum dioxide particle of nanometer through gas-phase reaction;
2), the molybdenumdisulphide and the elemental sulfur of nanometer reacted, generate nano molybdenum disulfide powder body material with fullerene structure under the condition of high temperature self-pressurization;
3), described molybdenum dioxide is that molybdic oxide is after 720-980 ℃ of gasification, react the nano particle that directly generates with hydrogen at 420-930 ℃, next, the molybdenumdisulphide of fullerene structure is that the molybdenum dioxide and the elemental sulfur of nanometer reacts synthetic by self-pressurization in container under 550-930 ℃ temperature;
4), the building-up reactions of described nanometer titanium dioxide molybdenum is carried out in the silica tube in stove, adopt two independently silica tube be respectively applied for hydrogen and transport with molybdic oxide and gasify, molybdic oxide that gasifies in reaction chamber and hydrogen mix, reduction reaction takes place, and nanometer titanium dioxide molybdenum product is that the interior porcelain filter of the silica tube in the reduction reaction furnace obtains;
5), the molybdenum dioxide of its nanometer and elemental sulfur produce the molybdenumdisulphide of the final fullerene synthesis structure of self-pressurization by the gasification of elemental sulfur in closed reactor under 580-930 ℃ temperature in heatable metal vessel.
Embodiment 3
The preparation of the first step molybdenum dioxide:
Taking by weighing of raw material: molybdic oxide 20g
Furnace temperature is set: 800 ℃ in 1# stove, and 800 ℃ in 2# stove,
Soaking time: 60 minutes.
Airshed is set: each silica tube carrier gas flux is 1500ml/min.Reducing gas is the mixed gas of 95%Ar and 5%H2.
Molybdenum dioxide content: 100%
Molybdenum dioxide particle mean size: 20 nanometers.
The preparation of the second step molybdenumdisulphide:
Adopt 50 milliliters stainless steel reaction container, 10 gram nanometer titanium dioxide molybdenums and 30 gram sulphur are raw material, and encloses container places 700 ℃ High Temperature Furnaces Heating Apparatus internal reaction 1 hour, and can obtain median size is the curing aluminium of the fullerene structure about 20 nanometers.
Embodiment 4
The preparation of the first step molybdenum dioxide:
Taking by weighing of raw material: molybdic oxide 30g
Furnace temperature is set: 900 ℃ in 1# stove, and 700 ℃ in 2# stove,
Soaking time: 60 minutes.
Airshed is set: each silica tube carrier gas flux is 1500ml/min.Reducing gas is the mixed gas of 95%Ar and 5%H2.
Molybdenum dioxide content: 100%
Molybdenum dioxide particle mean size: 17 nanometers.
The preparation of the second step molybdenumdisulphide:
Adopt 50 milliliters stainless steel reaction container, 10 gram nanometer titanium dioxide molybdenums and 40 gram sulphur are raw material, and encloses container places 850 ℃ High Temperature Furnaces Heating Apparatus internal reaction 1 hour, can obtain the molybdenumdisulphide that median size is the fullerene structure about 15 nanometers.
Embodiment 5
The preparation of the first step molybdenum dioxide:
Taking by weighing of raw material: molybdic oxide 30g
Furnace temperature is set: 850 ℃ in 1# stove, and 550 ℃ in 2# stove,
Soaking time: 60 minutes.
Airshed is set: each silica tube carrier gas flux is 1500ml/min.Reducing gas is the mixed gas of 95%Ar and 5%H2.
Molybdenum dioxide content: 100%
Molybdenum dioxide particle mean size: 10 nanometers.
The preparation of the second step molybdenumdisulphide:
Adopt 50 milliliters stainless steel reaction container, 10 gram nanometer titanium dioxide molybdenums and 35 gram sulphur are raw material, and encloses container places 900 ℃ High Temperature Furnaces Heating Apparatus internal reaction 1 hour, can obtain the molybdenumdisulphide that median size is the fullerene structure about 10 nanometers.
Embodiment 6
The preparation of the first step molybdenum dioxide:
Taking by weighing of raw material: molybdic oxide 30g
Furnace temperature is set: 850 ℃ in 1# stove, and 950 ℃ in 2# stove,
Soaking time: 60 minutes.
Airshed is set: each silica tube carrier gas flux is 1500ml/min.Reducing gas is the mixed gas of 95%Ar and 5%H2.
Molybdenum dioxide content: 100%
Molybdenum dioxide particle mean size: 50 nanometers.
The preparation of the second step molybdenumdisulphide:
Adopt 50 milliliters stainless steel reaction container, 5 gram nanometer titanium dioxide molybdenums and 20 gram sulphur are raw material, and encloses container places 950 ℃ High Temperature Furnaces Heating Apparatus internal reaction 1 hour, can obtain the molybdenumdisulphide that median size is the fullerene structure about 50 nanometers.
In sum, described molybdenum dioxide and elemental sulfur are with 1: the molar ratio of 2-20 places in the metal encloses container, by after heating airtight metal vessel temperature and reaching 600-950 ℃, material gasification in the container generates the nano molybdenum disulfide of fullerene structure through the self-pressurization reaction.
Described molybdenum dioxide and elemental sulfur are with 1: the molar ratio of 2.5-18 places in the metal encloses container, and by after heating airtight metal vessel temperature and reaching 580-930 ℃, material gasification in the container generates the nano molybdenum disulfide of fullerene structure through the self-pressurization reaction.
Used molybdic oxide is the commodity industry molybdenum trioxide, and the particle diameter of the molybdenum dioxide that hydrogen reducing generates is the 5-100 nanometer.
Raw materials used elemental sulfur is commercially available sulphur.
Claims (7)
1, a kind of preparation method with nano molybdenum disulfide of fullerene structure is characterized in that its preparation process is to adopt two-step approach, is undertaken by following step successively:
1) being raw material with industrial molybdic oxide, at first, is carrier gas with the argon gas, and hydrogen is reductive agent, generates the molybdenum dioxide particle of nanometer through gas-phase reaction;
2), the molybdenumdisulphide and the elemental sulfur of nanometer reacted, generate nano molybdenum disulfide powder body material with fullerene structure under the condition of high temperature self-pressurization;
3), described molybdenum dioxide is that molybdic oxide is after 700-1000 ℃ of gasification, react the nano particle that directly generates with hydrogen at 400-950 ℃, next, the molybdenumdisulphide of fullerene structure is that the molybdenum dioxide and the elemental sulfur of nanometer reacts synthetic by self-pressurization in container under 500-950 ℃ temperature;
4), the building-up reactions of described nanometer titanium dioxide molybdenum is carried out in the silica tube in stove, adopt two independently silica tube be respectively applied for hydrogen and transport with molybdic oxide and gasify, molybdic oxide that gasifies in reaction chamber and hydrogen mix, reduction reaction takes place, and nanometer titanium dioxide molybdenum product is that the interior porcelain filter of the silica tube in the reduction reaction furnace obtains;
5), described its nanometer titanium dioxide molybdenum and elemental sulfur produce the molybdenumdisulphide of the final fullerene synthesis structure of self-pressurization by the gasification of elemental sulfur in closed reactor under 500-950 ℃ temperature in heatable metal vessel.
2, a kind of preparation method with nano molybdenum disulfide of fullerene structure according to claim 1 is characterized in that being undertaken by following step successively:
1) being raw material with industrial molybdic oxide, at first, is carrier gas with the argon gas, and hydrogen is reductive agent, generates the molybdenum dioxide particle of nanometer through gas-phase reaction;
2), the molybdenumdisulphide and the elemental sulfur of nanometer reacted, generate nano molybdenum disulfide powder body material with fullerene structure under the condition of high temperature self-pressurization;
3), described molybdenum dioxide is that molybdic oxide is after 720-980 ℃ of gasification, react the nano particle that directly generates with hydrogen at 420-930 ℃, next, the molybdenumdisulphide of fullerene structure is that the molybdenum dioxide and the elemental sulfur of nanometer reacts synthetic by self-pressurization in container under 550-930 ℃ temperature;
4), the building-up reactions of described nanometer titanium dioxide molybdenum is carried out in the silica tube in stove, adopt two independently silica tube be respectively applied for hydrogen and transport with molybdic oxide and gasify, molybdic oxide that gasifies in reaction chamber and hydrogen mix, reduction reaction takes place, and nanometer titanium dioxide molybdenum product is that the interior porcelain filter of the silica tube in the reduction reaction furnace obtains;
5), described its nanometer titanium dioxide molybdenum and elemental sulfur produce the molybdenumdisulphide of the final fullerene synthesis structure of self-pressurization by the gasification of elemental sulfur in closed reactor under 580-930 ℃ temperature in heatable metal vessel.
3. a kind of preparation method according to claim 1 with nano molybdenum disulfide of fullerene structure, it is characterized in that described molybdenum dioxide and elemental sulfur are with 1: the molar ratio of 2-20 places in the metal encloses container, by after heating airtight metal vessel temperature and reaching 600-950 ℃, material gasification in the container is through the nano molybdenum disulfide of self-pressurization reaction generation fullerene structure.
4, a kind of preparation method according to claim 3 with nano molybdenum disulfide of fullerene structure, it is characterized in that described molybdenum dioxide and elemental sulfur are with 1: the molar ratio of 2.5-18 places in the metal encloses container, by after heating airtight metal vessel temperature and reaching 580-930 ℃, material gasification in the container is through the nano molybdenum disulfide of self-pressurization reaction generation fullerene structure.
5. a kind of preparation method with nano molybdenum disulfide of fullerene structure according to claim 1 and 2 is characterized in that used molybdic oxide is the commodity industry molybdenum trioxide, and the particle diameter of the molybdenum dioxide that hydrogen reducing generates is the 5-100 nanometer.
6. the preparation method of a kind of fullerene structure nano molybdenum disulfide according to claim 1 and 2 is characterized in that raw materials used elemental sulfur is commercially available sulphur.
7. a kind of preparation method with nano molybdenum disulfide of fullerene structure according to claim 1 and 2 is characterized in that institute's synthetic fullerene structure molybdenumdisulphide is spheroidal particle, and grain graininess is the 5-100 nanometer.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103924213A (en) * | 2014-04-29 | 2014-07-16 | 清华大学 | Method for preparing molybdenum disulfide film for field emission device |
| CN105514403A (en) * | 2016-01-13 | 2016-04-20 | 陕西科技大学 | Three-dimensional core-shell structure MoO2-MoS2 lithium ion battery cathode material and preparing method thereof |
| CN106558475A (en) * | 2016-11-16 | 2017-04-05 | 中国科学院物理研究所 | Wafer scale monolayer molybdenum bisuphide film and preparation method thereof |
| CN110436525A (en) * | 2019-07-22 | 2019-11-12 | 金堆城钼业股份有限公司 | A kind of preparation method of micro-/ nano molybdenum disulfide |
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2008
- 2008-02-22 CN CN2008100175320A patent/CN101234785B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103924213A (en) * | 2014-04-29 | 2014-07-16 | 清华大学 | Method for preparing molybdenum disulfide film for field emission device |
| US9659733B2 (en) | 2014-04-29 | 2017-05-23 | Tsinghua University | Method for preparing a molybdenum disulfide film used in a field emission device |
| CN105514403A (en) * | 2016-01-13 | 2016-04-20 | 陕西科技大学 | Three-dimensional core-shell structure MoO2-MoS2 lithium ion battery cathode material and preparing method thereof |
| CN105514403B (en) * | 2016-01-13 | 2018-07-17 | 陕西科技大学 | A kind of three-dimensional nucleocapsid MoO2-MoS2Lithium ion battery negative material and preparation method thereof |
| CN106558475A (en) * | 2016-11-16 | 2017-04-05 | 中国科学院物理研究所 | Wafer scale monolayer molybdenum bisuphide film and preparation method thereof |
| CN106558475B (en) * | 2016-11-16 | 2019-11-05 | 中国科学院物理研究所 | Wafer scale single layer molybdenum disulfide film and preparation method thereof |
| CN110436525A (en) * | 2019-07-22 | 2019-11-12 | 金堆城钼业股份有限公司 | A kind of preparation method of micro-/ nano molybdenum disulfide |
| CN110436525B (en) * | 2019-07-22 | 2021-09-28 | 金堆城钼业股份有限公司 | Preparation method of micro/nano molybdenum disulfide |
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