CN108640154A - A kind of molybdenum disulfide nano material and preparation method thereof - Google Patents

A kind of molybdenum disulfide nano material and preparation method thereof Download PDF

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CN108640154A
CN108640154A CN201810619271.3A CN201810619271A CN108640154A CN 108640154 A CN108640154 A CN 108640154A CN 201810619271 A CN201810619271 A CN 201810619271A CN 108640154 A CN108640154 A CN 108640154A
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molybdenum disulfide
preparation
nano material
ionic liquid
molybdenum
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樊小强
严涵
付汉敏
李文
朱旻昊
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Southwest Jiaotong University
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Abstract

The invention discloses a kind of molybdenum disulfide nano materials and preparation method thereof, belong to molybdenum disulfide preparing technical field.The present invention is using multipurpose green solvent --- the aqueous solution of ionic liquid is as electrolyte and dressing agent, and stripping layer by layer prepares the molybdenum disulfide nano material of functionalization in situ from molybdenum disulfide bar or bulk under external voltage auxiliary.Preparation method not only energy conservation and environmental protection but also the efficient high yield of the present invention has many advantages, such as low consumption, low cost, high yield, environmentally protective;Simultaneously, the present invention not only realizes the extensive preparation of high quality molybdenum disulfide nano material, and it is in-situ modified by physical absorption and chemical bond in its preparation process intermediate ion liquid functional group, the two big bottleneck problems for solving the extensive use of limitation molybdenum disulfide and performance regulation and control, are conducive to molybdenum disulfide in multi-field application.

Description

A kind of molybdenum disulfide nano material and preparation method thereof
Technical field
The present invention relates to molybdenum disulfide preparing technical fields, and in particular to a kind of molybdenum disulfide nano material and its preparation side Method.
Background technology
Prepare MoS2The method of material, can be mainly divided into two major classes:Physical method and chemical method.Physical mainly wraps It has included:Physical vaporous deposition (PVD), micromechanical forces stripping method and liquid phase stripping method etc..Chemical method is mainly:Hydro-thermal method, Chemical vapour deposition technique (CVD), vulcanization, electrochemical deposition method etc..But these methods have the following disadvantages:Preparation process is numerous It is trivial, low yield, of high cost, not environmentally, seriously hinder MoS2Extensive, the mass production of material, are applied so as to cause it Range is limited.
Invention content
The purpose of the present invention is to provide a kind of molybdenum disulfide nano materials and preparation method thereof, to solve existing preparation work Skill process is cumbersome, low yield, it is of high cost, not environmentally the problem of.
The technical solution that the present invention solves above-mentioned technical problem is as follows:
A kind of preparation method of molybdenum disulfide nano material, the preparation method by using two curing molybdenum bars as Positive and negative electrode is placed in ionic liquid aqueous solution and is electrolysed under external voltage effect, removes curing molybdenum bar, molybdenum disulfide is made Nano material.
Raw material of the present invention is curing molybdenum bar (block), and electrolyte is ionic liquid aqueous solution, then additional one DC power supply or direct current pulse power source, energy green efficiently prepare nano molybdenum disulfide material.
The present invention can realize two-dimensional layer curing by regulating and controlling the concentration of ionic liquid aqueous solution and the size of external voltage The structure of molybdenum nano material and the high efficiency regulatory of performance, and realize that mass prepares surface-functionalized single layer or few layer curing Molybdenum nano-powder, and there is very high yield.
It is in preparation process middle-high density in-situ modified that the present invention realizes molybdenum disulfide nano powder, solves its and easily rolls into a ball The technical issues of poly- and difficult dispersion, and its controllable physicochemical properties are modified by high density, meet the use of different field Performance requirement.
In addition, the ionic liquid aqueous solution that the present invention uses can be recycled, and under external voltage auxiliary, prepare in situ repair The molybdenum disulfide nano material of decorations, not only energy conservation and environmental protection but also efficient high yield, had low consumption, low cost, high yield, environmentally protective etc. Advantage;Meanwhile the present invention not only realizes the extensive preparation of high quality molybdenum disulfide nano material, but also in its preparation process Intermediate ion liquid functional group is in-situ modified by physical absorption and chemical bond, solves limitation molybdenum disulfide extensive use And two big bottleneck problems of performance regulation and control, be conducive to molybdenum disulfide in multi-field application.
Further, in preferred embodiments of the present invention, above-mentioned preparation method includes step in detail below:
(1) ionic liquid is added in deionized water, is stirred evenly, ionic liquid aqueous solution is made;
(2) two curing molybdenum bars are inserted into the ionic liquid aqueous solution, and two two is fixed using dielectric holder Vulcanize molybdenum bar to ensure constant distance between positive and negative electrode, with conducting wire by two curing molybdenum bars respectively with the anode of DC power supply It is connected with cathode, sets operating voltage≤20V, removed;As reaction carries out, there is sediment in solution, the sediment For molybdenum disulfide nano material.
For the present invention when preparing ionic liquid aqueous solution, ionic liquid and deionized water can be arbitrarily than mixing, Ke Yitong Magnetic force or mechanical agitation are crossed, uniform ionic liquid aqueous solution is formed.
When removing, splitting time can also be arbitrarily arranged the present invention, as long as meeting has sediment generation. Operating voltage when stripping is set smaller than equal to 20V, causes ionic liquid to crosslink, polymerize to avoid voltage is excessive, from And it influences the performance of ionic liquid aqueous solution and leads to not normally remove.Preferably, operating voltage 10V.
Further, in preferred embodiments of the present invention, in step (1), the volume ratio of ionic liquid and deionized water It is 1:(4-8).
In view of the time cost and cost of material of reaction process, the volume ratio of preferred ion liquid and deionized water is 1: (4-8)。
Further, in preferred embodiments of the present invention, in step (1), the volume ratio of ionic liquid and deionized water It is 1:6.
Further, in preferred embodiments of the present invention, above-mentioned ionic liquid is water soluble ion liquid.
Further, in preferred embodiments of the present invention, above-mentioned ionic liquid be imidazolium ionic liquid, quaternary alkylphosphonium salts from One or more combinations in sub- liquid and quaternary ammonium salt ionic liquid.
Further, in preferred embodiments of the present invention, above-mentioned ionic liquid be tetrafluoroborate, hexafluoro-phosphate radical, One or more combinations in sulfonate radical, halogen and amine root.
These ionic liquids play modification while being removed to the structure of molybdenum disulfide.
Further, in preferred embodiments of the present invention, above-mentioned ionic liquid is LB104 ionic liquids.
Further, in preferred embodiments of the present invention, in step (2), operating voltage 5-15V, splitting time is 4-6h。
Further, in preferred embodiments of the present invention, in step (2), operating voltage 5V, splitting time 5h.
The present invention can realize prepared MoS by regulating and controlling the concentration of ionic liquid aqueous solution and the size of external voltage2 Properity and yield effective control.
Further, in preferred embodiments of the present invention, above-mentioned preparation method further includes:(3) when sediment is not producing It when raw, cuts off the power, collects sediment, the sediment is subjected to eccentric cleaning.
Further, in preferred embodiments of the present invention, in step (3), the solvent of eccentric cleaning is ethyl alcohol, acetic acid second Ester or deionized water;The method of eccentric cleaning is:It puts the precipitate in and centrifuges 5-15min in centrifuge tube, institute is then added Solvent supersonic dispersion 5-15min is stated, abovementioned steps are repeated 6-10 times after the completion of dispersion.
Preferably, in eccentric cleaning, centrifugal speed is 4000 turns/min.
It, can be according to the control of centrifugal speed and centrifugation time, to obtain different layers by the sediment eccentric cleaning of acquisition Several functionalization MoS2Nano material.The molybdenum disulfide of the bigger acquisition of centrifugal speed is thinner, and the number of plies is fewer.For example, 4000 Turn/rotating speed of min under can obtain 10 layers or more of multilayer molybdenum disulfide, the number of plies can be obtained under the rotating speed of 8000r/min Molybdenum disulfide less than ten layers can obtain molybdenum disulfide of the number of plies within four layers under the rotating speed of 12000r/min.Specifically Rotating speed is arranged, and those skilled in the art can suitably be adjusted according to the performance or application scenarios of required molybdenum disulfide, to The molybdenum disulfide of different function is obtained, realizes the functionalization of molybdenum disulfide nano material.
Further, in preferred embodiments of the present invention, above-mentioned preparation method further includes:(4) after step (3) being cleaned Drying precipitate, drying mode be vacuum drying, air-dry or freeze-drying.
Molybdenum dioxide nano material made from above-mentioned preparation method.
The invention has the advantages that:
The electrochemistry up-stripping of the present invention prepares MoS2Nano material, preparation process is simple, and required instrument and equipment is simple. The present invention uses in ionic liquid aqueous solution, and external voltage up-stripping prepares MoS2Nanometer sheet is MoS2Nano material provides one Green, simple, the efficient preparation method of kind.
The present invention can be used for efficiently preparing the solid molybdenum disulfide nano material of functionalization, solve its easily reunion, difficult dispersion The problem of, to provide material and technical guarantee to prepare the composite material of solid nano material reinforcement, as molybdenum disulfide moistens Lubricating oil fat, molybdenum disulfide organic composite material, molybdenum-disulfide radical catalyst etc..
Description of the drawings
Fig. 1 (a) is that ionic liquid concentration is 1:6, MoS when operating voltage is 5V2The transmission electron microscope picture of nano material;
Fig. 1 (b) is that ionic liquid concentration is 1:6, MoS when operating voltage is 10V2The transmission electron microscope picture of nano material;
Fig. 1 (c) is that ionic liquid concentration is 1:6, MoS when operating voltage is 15V2The transmission electron microscope picture of nano material;
Fig. 2 is that ionic liquid concentration is 1:6, operating voltage is the MoS of 15V2The selected diffraction style figure of nano material;
Fig. 3 is the MoS for preparing under the conditions of different operating voltage value2X-ray diffraction (XRD) collection of illustrative plates;
Fig. 4 (a) is operating voltage when being 5V, and ionic liquid volume is 1 with deionized water volume ratio:MoS when 62It receives The transmission electron microscope picture of rice material;
Fig. 4 (b) is operating voltage when being 5V, and ionic liquid volume is 1 with deionized water volume ratio:MoS when 82It receives The transmission electron microscope picture of rice material;
Fig. 4 (c) is operating voltage when being 5V, and ionic liquid volume is 1 with deionized water volume ratio:MoS when 42It receives The transmission electron microscope picture of rice material;
Fig. 5 is operating voltage when being 5V, volume ratio 1:8 MoS2The selected diffraction style figure of material;
Fig. 6 (a) is the functionalization MoS that different ionic liquid concentration of aqueous solution is prepared under the conditions of 5V operating voltages2X penetrate Line diffraction (XRD) figure;
Fig. 6 (b) is the functionalization MoS that different ionic liquid concentration of aqueous solution is prepared under the conditions of 5V operating voltages2It is red Outer absorption spectrum (FTIR) figure.
Specific implementation mode
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and It is non-to be used to limit the scope of the present invention.The person that is not specified actual conditions in embodiment, the item suggested according to normal condition or manufacturer Part carries out.Reagents or instruments used without specified manufacturer is the conventional products that can be obtained by commercially available purchase.
Embodiment 1:
It takes 60mL deionized waters to be put into 100mL beakers, then 10mL ionic liquids (LB104) is measured by suction pipe and are slowly dripped Enter in the beaker equipped with deionized water, glass bar is used in combination to be stirred until homogeneous, forms ionic liquid aqueous solution.By two high-purity MoS2 Stick is inserted perpendicularly into as two electrodes into above-mentioned electrolyte beaker, and against the inner wall of beaker, is pressed from both sides using nonconducting fixture Hold MoS2Stick ensure during the experiment two working electrodes it is constant this apart from constant.Then with two conducting wires by two electrode MoS2Stick It is connected to the positive and negative electrode of DC power supply, to provide operating voltage (5V), splitting time is 5 hours.After prepared by stripping, burn Contain a large amount of sediments in cup.The sediment of acquisition is positioned in centrifuge tube and is centrifuged 10 minutes with 4000r/min rotating speeds. Sediment, which continuously adds excessive EtOH Sonicate, to be disperseed 10 minutes, is centrifuged again with 4000r/min rotating speeds after the completion of dispersion, such as This product for operating 8 acquisitions repeatedly is put into 40 DEG C of vacuum drying chamber drying, obtains powder sample.
Embodiment 2:
It takes 60mL deionized waters to be put into 100mL beakers, then 10mL ionic liquids (LB104) is measured by suction pipe and are slowly dripped Enter in the beaker equipped with deionized water, glass bar is used in combination to be stirred until homogeneous, forms ionic liquid aqueous solution.By two high-purity MoS2 Stick is inserted perpendicularly into as two electrodes into above-mentioned electrolyte beaker, and against the inner wall of beaker, is pressed from both sides using nonconducting fixture Hold MoS2Stick ensure during the experiment two working electrodes it is constant this apart from constant.Then with two conducting wires by two electrode MoS2Stick It is connected to the positive and negative electrode of DC power supply, to provide operating voltage (10V), splitting time is 5 hours.After prepared by stripping, burn Contain a large amount of sediments in cup.The sediment of acquisition is positioned in centrifuge tube and centrifuges 10 with 4000r/min rotating speeds
Minute.Sediment, which continuously adds excessive EtOH Sonicate, to be disperseed 10 minutes, is turned again with 4000r/min after the completion of dispersion Speed centrifuges, and the product for operating 8 acquisitions repeatedly is put into 40 DEG C of vacuum drying chamber drying, obtains powder sample.
Embodiment 3:
It takes 60mL deionized waters to be put into 100mL beakers, then 10mL ionic liquids (LB104) is measured by suction pipe and are slowly dripped Enter in the beaker equipped with deionized water, glass bar is used in combination to be stirred until homogeneous, forms ionic liquid aqueous solution.By two high-purity MoS2 Stick is inserted perpendicularly into as two electrodes into above-mentioned electrolyte beaker, and against the inner wall of beaker, is pressed from both sides using nonconducting fixture Hold MoS2Stick ensure during the experiment two working electrodes it is constant this apart from constant.Then with two conducting wires by two electrode MoS2Stick It is connected to the positive and negative electrode of DC power supply, to provide operating voltage (15V), splitting time is 5 hours.After prepared by stripping, burn Contain a large amount of sediments in cup.The sediment of acquisition is positioned in centrifuge tube and is centrifuged 10 minutes with 4000r/min rotating speeds. Sediment, which continuously adds excessive EtOH Sonicate, to be disperseed 10 minutes, is centrifuged again with 4000r/min rotating speeds after the completion of dispersion, such as This product for operating 8 acquisitions repeatedly is put into 40 DEG C of vacuum drying chamber drying, obtains powder sample.
Above-described embodiment 1,2,3 is mainly using operating voltage as variable, respectively using 5V, 10V, 15V as operating voltage.
Embodiment 4:
It takes 40mL deionized waters to be put into 100mL beakers, then 10mL ionic liquids (LB104) is measured by suction pipe and are slowly dripped Enter in the beaker equipped with deionized water, glass bar is used in combination to be stirred until homogeneous, forms ionic liquid aqueous solution.By two high-purity MoS2 Stick is inserted perpendicularly into as two electrodes into above-mentioned electrolyte beaker, and against the inner wall of beaker, is pressed from both sides using nonconducting fixture Hold MoS2Stick ensure during the experiment two working electrodes it is constant this apart from constant.Then with two conducting wires by two electrode MoS2Stick It is connected to the positive and negative electrode of DC power supply, to provide operating voltage (5V), splitting time is 5 hours.After prepared by stripping, burn Contain a large amount of sediments in cup.The sediment of acquisition is positioned in centrifuge tube and is centrifuged 10 minutes with 4000r/min rotating speeds. Sediment, which continuously adds excessive EtOH Sonicate, to be disperseed 10 minutes, is centrifuged again with 4000r/min rotating speeds after the completion of dispersion, such as This product for operating 8 acquisitions repeatedly is put into 40 DEG C of vacuum drying chamber drying, obtains powder sample.
Embodiment 5:
It takes 80mL deionized waters to be put into 100mL beakers, then 10mL ionic liquids (LB104) is measured by suction pipe and are slowly dripped Enter in the beaker equipped with deionized water, glass bar is used in combination to be stirred until homogeneous, forms ionic liquid aqueous solution.By two high-purity MoS2 Stick is inserted perpendicularly into as two electrodes into above-mentioned electrolyte beaker, and against the inner wall of beaker, is pressed from both sides using nonconducting fixture Hold MoS2Stick ensure during the experiment two working electrodes it is constant this apart from constant.Then with two conducting wires by two electrode MoS2Stick It is connected to the positive and negative electrode of DC power supply, to provide operating voltage (5V), splitting time is 5 hours.After prepared by stripping, burn Contain a large amount of sediments in cup.The sediment of acquisition is positioned in centrifuge tube and is centrifuged 10 minutes with 4000r/min rotating speeds. Sediment, which continuously adds excessive EtOH Sonicate, to be disperseed 10 minutes, is centrifuged again with 4000r/min rotating speeds after the completion of dispersion, such as This product for operating 8 acquisitions repeatedly is put into 40 DEG C of vacuum drying chamber drying, obtains powder sample.
Embodiment 1,4,5 is mainly using the volume ratio of ionic liquid and water as variable, and respectively 1:6、1:4、1:8.
Test example 1:Operating voltage is to preparing the influence of molybdenum disulfide
According to the size (5V, 10V and 15V) of operating voltage value, by the MoS of preparation2Nano material is abbreviated as MoS25V、 MoS210V and MoS215V:
It is 1 that Fig. 1 (a)-(c), which gives LB104 ionic liquid concentrations,:When 6, the MoS of operating voltage 5V, 10V and 15V2 The transmission electron microscope picture of nano material, Fig. 2 are that ionic liquid concentration is 1:6, operating voltage is the MoS of 15V2The constituency of nano material Diffraction pattern figure.
According to two-dimentional MoS2The transmission picture and selective electron diffraction striped of piece, which can be seen that, forms polycrystalline structure, MoS2 Hexagonal system structure be not destroyed during electrochemical stripping;When LB104 ionic liquid concentrations are 1:When 6, MoS25V Transmission picture (Fig. 1 (a)) show the MoS of stripping2Nano material is typical two-dimensional layered structure;Meanwhile MoS210V's Transmission plot (Fig. 1 (b)) illustrates to obtain the good two dimension MoS of crystallinity under 10V operating voltages2Nanometer sheet;From operating voltage For the MoS of 15V2Product (MoS2From the point of view of transmission plot (Fig. 1 (c)) 15V), nanometer MoS2It is two-dimensional slice structure, ionic liquid is repaiied Decorations group inlays interlayer, forms sandwich structure, so lamella is relatively thick.
Fig. 3 is the MoS for preparing under the conditions of different operating voltage value2X-ray diffraction (XRD) collection of illustrative plates.As shown in Fig. 2, Ionic liquid volume is 1 with deionized water volume ratio:When 6, the MoS of acquisition is removed under 5V, 10V and 15V operating voltage2Product X ray diffracting spectrum characteristic peak it is almost consistent, wherein 2 θ=14.4 ° peak positions are most strong, secondary strong peak position is set to 2 θ=39.6 °, The strong peak of third is located at 2 θ=49.8 °, this is completely the same with the three strongest peak in standard PDF (37-1492) card, this three strongest peak difference It is that (002) (2 θ=14.4 °), (103) (2 θ=39.6 °) and (105) (2 θ=49.8 °) crystal face diffraction generates, it was demonstrated that obtain Product be MoS2Material.
Test example 2:Ionic liquid concentration is to preparing the influence of molybdenum disulfide
The MoS prepared when operating voltage is 5V2Nano material is abbreviated as MoS25V.The volume of LB104 ionic liquids and water Than being labeled in figure.
Fig. 4 (a), Fig. 4 (b), Fig. 4 (c) are operating voltage when being 5V, LB104 ionic liquids volume and deionized water volume Ratio is respectively a concentration of 1:6、1:8、1:MoS when 42The transmission electron microscope picture of nano material.Fig. 5 is operating voltage when being 5V, Volume ratio is 1:8 MoS2The selected diffraction style figure of material.
As shown in Fig. 4 (b), when operating voltage is 5V, volume ratio 1:8 MoS2The high-resolution-ration transmission electric-lens figure of material Piece shows typical two-dimensional slice structure, and lamella edge is relatively thin, and transmission picture shows MoS2Lamella is about 5 layers, meanwhile, such as Shown in Fig. 5, selective electron diffraction style also shows MoS2Typical six sides symmetric crystal lattice, crystallinity are preferable.And when in this voltage Under, volume ratio 1:MoS when 62The transmission electron microscope of sample, as shown in Fig. 4 (a), the non-crystalline areas of large stretch of area occurs, this is Caused by being modified due to LB104 ionic liquid high density, for this explanation under the conditions of 5V operating voltages, LB104 ionic liquids are water-soluble Liquid concentration increases, the enhancing of functional modification density.Under this voltage, volume ratio 1:MoS when 42The transmission electron microscope of sample, As shown in Fig. 4 (c), the MoS of preparation2It is enough for multilayer knot.
Fig. 6 (a) is the functionalization MoS that different LB104 ionic liquid aqueous solutions concentration are prepared under the conditions of 5V operating voltages2 X-ray diffraction (XRD) figure.Fig. 6 (b) is that different LB104 ionic liquid aqueous solutions concentration are prepared under the conditions of 5V operating voltages Functionalization MoS2Infrared absorption spectrum (FTIR) figure.
From Fig. 6 (a) it is found that LB104 ionic liquids and deionized water volume ratio are 1:When 6, the MoS prepared is removed2Sample The value of 2 θ of product XRD is about 14.1 °, 32.6 °, 33.6 °, 35.9 °, 39.5 °, 43.3 °, 49.8 °, 58.3 °, 60.2 °, and 70.2, 72.8 ° and 75.9 °, through Jade softwares analysis (PDF#65-0160) it is found that its corresponding diffraction maximum is respectively 2H types MoS2's (002), (100), (101), (102), (103), (006), (105), (110), (008), (108), (203) and (116) crystal face Diffraction maximum, this explanation operating voltage be 5V when, higher ionic liquid concentration (1:4) MoS prepared2For multilayered structure. LB104 ionic liquid aqueous solution volume ratios are 1:When 6, the MoS for preparing2For the less number of plies, and crystallinity is preferable, also illustrates The MoS of preparation2For 2H type hexagonal crystal systems, the transmission electron microscope and its selective electron diffraction style of this and Fig. 4 (a), (b) and Fig. 5 Analysis result match.
Infrared spectrum (FTIR) figure of difference LB104 ionic liquid concentrations when Fig. 6 (b) gives 5V operating voltages, into one Step demonstrates LB104 ionic liquids original position functional modification MoS2Material.Above-mentioned FTIR the result shows that LB104 ionic liquids or Its functional group of person does exist in multilayer MoS2Between lamellar structure.
By above-described embodiment result it is found that successfully function has been prepared in stripping in external voltage assisting ion liquid aqueous solution The molybdenum disulfide nano material of change, the number of plies, structure and the performance of molybdenum disulfide can be by controlling preparation technology parameter regulation and control.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of preparation method of molybdenum disulfide nano material, which is characterized in that the preparation method is by by two molybdenum disulfide Stick is placed in ionic liquid aqueous solution respectively as positive and negative electrode and is electrolysed under external voltage effect, removes curing molybdenum bar, system Obtain molybdenum disulfide nano material.
2. the preparation method of molybdenum disulfide nano material according to claim 1, which is characterized in that the preparation method packet Include step in detail below:
(1) ionic liquid is added in deionized water, is stirred evenly, ionic liquid aqueous solution is made;
(2) two curing molybdenum bars are inserted into the ionic liquid aqueous solution, and two curing is fixed using dielectric holder Molybdenum bar is positive and negative with DC power supply respectively by two curing molybdenum bars with conducting wire to ensure constant distance between positive and negative electrode Pole connects, and sets operating voltage≤20V, is removed;As reaction carries out, there is sediment in solution, which is two Molybdenum sulfide nano material.
3. the preparation method of molybdenum disulfide nano material according to claim 2, which is characterized in that in step (1), ion The volume ratio of liquid and deionized water is 1:(4-8).
4. the preparation method of molybdenum disulfide nano material according to claim 3, which is characterized in that in step (1), ion The volume ratio of liquid and deionized water is 1:6.
5. the preparation method of molybdenum disulfide nano material according to claim 2, which is characterized in that the ionic liquid is Water soluble ion liquid.
6. the preparation method of molybdenum disulfide nano material according to claim 5, which is characterized in that the ionic liquid is One or more combinations in imidazolium ionic liquid, quaternary phosphonium salt ionic liquids and quaternary ammonium salt ionic liquid.
7. the preparation method of molybdenum disulfide nano material according to claim 5, which is characterized in that the ionic liquid is One or more combinations in tetrafluoroborate, hexafluoro-phosphate radical, sulfonate radical, halogen and amine root.
8. according to the preparation method of claim 2-7 any one of them molybdenum disulfide nano materials, which is characterized in that step (2) in, operating voltage 5-15V, splitting time 4-6h.
9. the preparation method of molybdenum disulfide nano material according to claim 8, which is characterized in that in step (2), work Voltage is 5V, splitting time 5h.
10. molybdenum dioxide nano material made from claim 1-9 any one of them preparation methods.
CN201810619271.3A 2018-06-15 2018-06-15 A kind of molybdenum disulfide nano material and preparation method thereof Pending CN108640154A (en)

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CN112635620A (en) * 2020-12-21 2021-04-09 昆明理工大学 Gr/MX2Preparation method of/Si solar cell

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