CN106044856A - Method for preparing molybdenum disulfide nano-sheet from molybdenite through ultrasonic-sanding coupling stripping - Google Patents
Method for preparing molybdenum disulfide nano-sheet from molybdenite through ultrasonic-sanding coupling stripping Download PDFInfo
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Abstract
The invention belongs to the technical field of nanometer material processing, and particularly relates to a method for preparing a molybdenum disulfide nano-sheet from molybdenite through ultrasonic-sanding coupling stripping. The method comprises following steps: 1), molybdenite micropowder is dispersed in a stripping solvent, and a suspension liquid is formed; 2), a dispersing agent and a stripping assistant are dissolved in the suspension liquid obtained in the step 1) and subjected to ultrasonic dispersion; 3), the suspension liquid after subjected to the ultrasonic dispersion in the step 2) is subjected to continuous stripping under the ultrasonic-sanding coupling action, and the molybdenum disulfide nano-sheet is obtained. According to the designed novel method for preparing the molybdenum disulfide nano-sheets in a large scale from the molybdenite micropowder through ultrasonic-sanding coupling stripping, green transformation from a natural mineral to a high-performance function material is realized, and the method has important application value and economic benefit.
Description
Technical field
The invention belongs to nano material processing technique field, be specifically related to a kind of ultrasonic-sand milling coupling stripping molybdenite and prepare
The method of molybdenum disulfide nano sheet.
Background technology
MoS2Nanometer sheet and composite thereof have abundant physicochemical characteristics, clean at catalysis, energy conversion and storage, environment
There is important application in the fields such as change, lubrication.Block MoS2For indirect gap semiconductor (E g=1.2 eV), its single layer structure then becomes
Energy gap be 1.8 eV direct gap quasiconductor [Nano Lett.2011,11,5111-5116], there is fluorescent characteristic, can
Make biological label agent, be also efficient sunlight absorbent.Especially, MoS2Hydrogen catalysis is produced in the nanocrystalline electro-catalysis with excellence
Can, be expected to part and replace the noble metal such as Pt, will be greatly reduced use cost [Nano Lett. 2014, 14, 553-558]。
Additionally, MoS2Based nano composite material can do lithium (sodium) ion battery electrode [ACS Appl. Mater. Interfaces
2014, 6, 7084-7089].Few layer MoS2Nanometer sheet (Few-layer MoS2Nanoplates) controlled magnanimity preparation and
The regulation and control of its performance are focus and the forward positions of current international research.
Inexpensively, the preparation MoS of green controlled magnanimity2Nanometer sheet sill has most important theories and using value.MoS at present2
The preparation of nanometer sheet mainly has two kinds: from bottom to top with approach from top to bottom.Approach includes that hydro-thermal, chemical gaseous phase are heavy from bottom to top
The methods such as long-pending, thermal decomposition [Electrochimica Acta. 2014, 132, 397-403; Scientific reports,
2013, 3, 1866-1871; Small, 2012,8,966-971], the feature of these methods is pattern easy-regulating, but
Equipment, process are complicated, and condition is harsh, it is difficult to produce in enormous quantities.From top to bottom approach include micromechanics stripping, electrochemical stripping,
Ion insertion, liquid chromatography ultrasound etc. [Acc. Chem. Res. 2014, 47, 1067-1075; Materials Letters.
2014, 121, 31-35; Small. 2015, 11, 605-612; Science, 2013,340,1226419.], so far
There is the problems such as productivity is relatively low, intercalation degree difficulty controls, stripping process is the most green in these stripping means majorities modern, constrains two sulfur
Change the extensive application of molybdenio nano material.
Patent (201210512991.2 1 kinds of nanometer MOS 2 particles and preparation method and application) uses ionic liquid
Body or organic solvent are medium, first grind ultrasonic wave added process the most again and obtain nanometer MOS 2 particle.This grinding and super
The separate batch process of sound, exists that stripping cycle length, charge stripping efficiency be low, high in cost of production shortcoming, the simultaneously pattern of products therefrom
Wayward, it is difficult to obtain the molybdenum disulfide nano sheet structure of high radius-thickness ratio, high-specific surface area.
Summary of the invention
It is an object of the invention to provide a kind of employing sand milling and peel off the few layer two of molybdenite preparation on a large scale with ultrasonic coupling effect
The method of molybdenum sulfide nanometer sheet.
For achieving the above object, the present invention is by the following technical solutions:
The method that preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in ultrasonic-sand milling coupling, comprises the following steps: 1) molybdenite is micro-
Powder is scattered in stripping solvent and forms suspension；
2) dispersant, stripping auxiliary agent are dissolved in ultrasonic disperse in the suspension of step 1)；
3) step 2) suspension after ultrasonic disperse peels off continuously under ultrasonic, sand milling coupling simultaneously and obtains molybdenum bisuphide and receive
Rice sheet.During now molybdenum disulfide nano sheet is dispersed in suspension, the suspension after stripping can prepare through further work-up
The molybdenum disulfide nano sheet of powdery.Last handling process is: standing, centrifugal classification, washing, lyophilization.It is centrifuged during centrifugal classification
Rotating speed is 1500-10000 rpm.
Peeling off solvent is N-methyl pyrrole network alkanone, and dispersant is polyvinylpyrrolidone, and peeling off auxiliary agent is NaOH or NaCl.
The granularity of molybdenite micropowder is 5-50 micron, and the content of molybdenum bisuphide is more than 99.8%.
In step 1) suspension, the solid content of molybdenite micropowder is 10-60 g/L；Step 2) in dispersant (PVP repeats single
Body) it is 0.1-1 with the mol ratio of molybdenite micropowder, the mol ratio peeling off auxiliary agent and molybdenite micropowder is 0-1.
Power ultrasonic in step 3) is 200-350 W, and the rotating speed of sand mill is 1500-2250 rpm, coupling
Time is 0.5-6 h.
It is contemplated that develop a kind of low cost, high efficiency, magnanimity the most green, controlled prepare the side of molybdenum disulfide nano sheet
Method.The initiation material used is the molybdenite micropowder that China's reserves are big, physical and chemical performance abundant, application prospect is wide, designs " sand
Mill-ultrasonic " coupling peel off new method peel off molybdenite micropowder prepare molybdenum disulfide nano sheet on a large scale, it is achieved from natural minerals to
The green conversion of performance function material, has significant application value and economic benefit.
The present invention designs sand milling, many field of forces such as ultrasonic coupling stripping system, using molybdenite as starting material, by ultrasonic generation
The shearing coupling simultaneously that produces of cavitation and sand milling, it is achieved efficiently peel off.The abrading-ball of sand milling high speed operating clashes into brightness molybdenum
Ore deposit micropowder, shear action makes interlayer and layer edge curl split, produces defect；Meanwhile, ultrasonic cavitation promotes liquid
Molecule, stripping auxiliary agent etc. enter interlayer from the fault location split, and make molybdenite successively peel off, peel off auxiliary agent and dispersant in medium
It is to peel off the molybdenum disulfide nano sheet fine dispersion produced.The present invention peels off molybdenite with sand milling-ultrasonic coupling and prepares curing
Molybdenum nanometer sheet obtains productivity and can reach 21.6wt%, and gained widow's layer molybdenum disulfide nano sheet has in terms of electro-catalysis and electrochemical sensing
Important application.
Accompanying drawing explanation
Fig. 1 is the installation drawing of sand milling-ultrasonic coupling stripping system；
Fig. 2 is that sand milling-ultrasonic coupling peels off schematic diagram；
Fig. 3 is the digital photograph of embodiment 1 gained molybdenum disulfide nano sheet suspension；
Fig. 4 is the transmission electron microscope photo of embodiment 1 gained molybdenum disulfide nano sheet；
Fig. 5 is the atomic force microscopy of embodiment 1 gained molybdenum disulfide nano sheet；
Fig. 6 is the stereoscan photograph of embodiment 1 gained molybdenum disulfide nano sheet；
Fig. 7 is the X ray diffracting spectrum of embodiment 1 gained molybdenum disulfide nano sheet；
Fig. 8 is the N of embodiment 1 gained molybdenum disulfide nano sheet2Adsorption-desorption isothermal；
Fig. 9 is the UV-Visible absorption light of gained molybdenum disulfide nano sheet suspension under the splitting time that embodiment 1 is different
Spectrum；
Figure 10 is stripping productivity (left) and speed (the right) figure of gained molybdenum disulfide nano sheet under embodiment 1 different time；
Figure 11 is the stripping productivity figure of the different splitting time gained molybdenum disulfide nano sheet of embodiment 2；
Figure 12 is stripping productivity and the rate diagram of gained molybdenum disulfide nano sheet under embodiment 3 different time；
Figure 13 be the initial molybdenite solid content of embodiment 4 be 35 g/L, different splitting time gained molybdenum disulfide nano sheet suspends
The uv-visible absorption spectroscopy of liquid；
Figure 14 is embodiment 4 different initial molybdenite solid content stripping productivity in different splitting times and detachment rate figure；
Figure 15 be embodiment 5 ultrasonic power be the UV-Visible absorption light of gained molybdenum disulfide nano sheet suspension under 320 W
Spectrum；
Figure 16 is the stripping productivity of gained molybdenum disulfide nano sheet and detachment rate figure under embodiment 5 different ultrasonic power；
Figure 17 be embodiment 6 sand mill rotating speed be the ultraviolet-visible light of gained molybdenum disulfide nano sheet suspension under 1800 rpm
Absorption spectrum；
Figure 18 is stripping productivity and the detachment rate figure of gained molybdenum disulfide nano sheet under the different sand mill rotating speed of embodiment 6；
Figure 19 is embodiment 7 PVP monomer and MoS2The ultraviolet-visible of gained molybdenum disulfide nano sheet suspension when mol ratio is 1
Optical absorption spectra；
Figure 20 is stripping productivity and the detachment rate figure of gained molybdenum disulfide nano sheet under the different PVP content of embodiment 7；
Figure 21 is that the single field of force of effect experimental one is (left: the most ultrasonic；Right: ultrasonic sand milling is peeled off step by step) effect lower difference stripping
The uv-visible absorption spectroscopy of time gained molybdenum disulfide nano sheet suspension；
Figure 22 is the single field of force (the most ultrasonic and ultrasonic sand milling substep peel off) of effect experimental one and many field of forces couple (super
Sound-sand milling) the stripping productivity of the lower molybdenum disulfide nano sheet of effect and detachment rate figure；
Figure 23 is the chemical property figure that gained molybdenum disulfide nano sheet is peeled off in ultrasonic-sand milling coupling.
Detailed description of the invention
Sand milling-ultrasound couple device disclosed in following example is to realize a kind of device of the present invention, and other have similar functions
Device can be applied equally to the present invention.
Embodiment 1
Preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in ultrasonic-sand milling coupling, and step is as follows:
11.25 g molybdenite micropowders are scattered in 250 mL NMP(N-methyl pyrrolidones, C5H9NO) suspension is formed in；2)
Add 3.9 g PVP(polyvinylpyrrolidones, (C therewith6H9NO) n), ultrasonic 20 min make it fully dispersed；3) transfer after
Enter sand mill (rotating speed 2250 rpm) reaction cavity, then under high-energy ultrasonic effect (ultrasonic power is 280 W), sand milling-
Ultrasonic coupling peels off 6 h；4) the molybdenum disulfide nano sheet suspension peeled off is stood about 24 h, centrifugal classification, classification from
Heart rotating speed is respectively 1500 rpm, 8000 rpm, 10000 rpm, and centrifugation time is respectively 45 min.To be centrifuged at 1500 rpm
The molybdenum disulfide nano sheet solid content of the upper strata suspension after 45 min peels off the evaluation criterion of productivity as evaluating: use purple
The relative concentration of molybdenum disulfide nano sheet in outward-visible absorption spectra the real time measure suspension, and use sucking filtration measuring to hang
The absolute concentration of solid phase molybdenum disulfide nano sheet in supernatant liquid, makes working curve, unit of account time molybdenum disulfide nano sheet
Peel off productivity, thus calculate detachment rate.Finally can be further by the precipitate distilled water wash number of centrifugal classification gained
Secondary, lyophilization i.e. obtains few layer molybdenum disulfide nano sheet.
In this embodiment, mol ratio: PVP(repetitive)/MoS2=0.5。
Fig. 1 is the installation drawing of sand milling-ultrasonic coupling stripping system, i.e. uses ultrasonic cell disintegration machine and sand mill phase mutual coupling
The method closed, sand mill used configures ceramic-lined and cooling water system, a diameter of 2-5 mm of abrading-ball, is placed in by ultrasonic probe
In the cavity of sand mill, it is simultaneously introduced ultrasonic cavitation in sand milling shear action, improves the charge stripping efficiency of molybdenite.
Fig. 2 is that sand milling-ultrasonic coupling peels off schematic diagram.The abrading-ball run up in sand mill clashes into molybdenite microgranule,
Make its interlayer and layer edge crack or defect, under ultrasonic cavitation, promote solvent molecule, peel off the entrance layers such as auxiliary agent
Between, it is achieved the efficient stripping of molybdenite.
Fig. 3 be peel off after the digital photograph of gained molybdenum disulfide nano sheet suspension, through the standing of 42 days, bottom did not had
Precipitation, green suspension darkly, can keep stable for a long time.
Fig. 4 is the transmission electricity of gained molybdenum disulfide nano sheet suspension products therefrom after 10000 rpm are centrifuged 45 min
Sub-microphotograph.Obtained by peeling off, molybdenum disulfide nano sheet presents good single crystal forms, and lamella is relatively thin.
Fig. 5 is the AFM Analysis result of gained molybdenum disulfide nano sheet；Can be seen that obtained MoS2Nanometer
The thickness of sheet is about 1 nm, for monolayer.
Fig. 6 is that the scanning electron that gained molybdenum disulfide nano sheet suspension is centrifuged 45 min products therefroms through 8000 rpm shows
Micro mirror photo, it can be seen that molybdenum disulfide nano sheet defines thin and translucent thin film owing to being stacked with.
Fig. 7 is that gained molybdenum disulfide nano sheet suspension is centrifuged the XRD figure spectrum of 45 min products therefroms through 10000 rpm,
Its thing is 2H-MoS mutually2, in (002), crystallographic plane diffraction peak has widthization phenomenon, illustrates that the thickness of molybdenum disulfide nano sheet is the least.
Fig. 8 is gained molybdenum disulfide nano sheet N2Adsorption-desorption isothermal, is centrifuged 45 min gained through 10000 rpm and produces
The BET surface area of thing is up to 926 m2 /g。
Fig. 9 is the uv-visible absorption spectroscopy of gained molybdenum disulfide nano sheet under different splitting time.Find out from figure,
Along with the prolongation of splitting time, the ultraviolet-visible absorption spectroscopy of centrifuged suspension absorbance at 660 nm is gradually increased, root
According to Beer law, prolongation over time being described, the amount peeling off gained molybdenum disulfide nano sheet steps up.
Figure 10 is that molybdenum disulfide nano sheet peels off productivity and detachment rate figure, it can be seen that increase over time, stripping
Productivity is increasing, and speed variation tendency is little.
Embodiment 2
Preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in ultrasonic-sand milling coupling, and step is as follows:
11.25 g molybdenite micropowders are scattered in 250 mL ethanol solution (48%wt ethanol, C2H5OH) suspension is formed in；2)
Add 3.9 g PVP(polyvinylpyrrolidones, (C therewith6H9NO) n), ultrasonic 20 min make it fully dispersed；3) transfer after
Enter sand mill (rotating speed 2250 rpm) reaction cavity, then intercouple under ultrasonication (ultrasonic power is 280 W) into
Row peels off 4 h；4) suspension peeled off is stood about 2 h, centrifugal classification, respectively 1500 rpm, 5000 rpm,
Centrifugal 45 min under 8000 rpm.Subsequent treatment is with embodiment 1.
Figure 11 is that molybdenum disulfide nano sheet peels off productivity and detachment rate figure, prolongation over time, peels off productivity gradually
Increase, using ethanol solution as solvent, peel off productivity and the linear change of splitting time.
Embodiment 3
Preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in ultrasonic-sand milling coupling, and step is as follows:
6.25 g molybdenite micropowders are scattered in 250 mL NMP(N-methyl pyrrolidones, C5H9NO) suspension is formed in；2)
Add 2.17 g PVP(polyvinylpyrrolidones, (C therewith6H9NO) n), ultrasonic 20 min make it fully dispersed, are simultaneously introduced salt
(0.57gNaCl) or alkali (0.39gNaOH) peel off auxiliary agent；3) sand mill (rotating speed 2250 rpm) reaction chamber is transitioned into after
Body, then intercouples under ultrasonication (ultrasonic power is 280 W) and carries out peeling off 4 h；4) by quiet for the suspension peeled off
Put about 24 h, centrifugal classification, respectively centrifugal 45 min under 1500 rpm, 8000 rpm, 10000 rpm.Subsequent treatment is same
Embodiment 1.
Figure 12 is that molybdenum disulfide nano sheet peels off productivity and rate analysis figure, NMP for peeling off solvent, add salt (NaCl) and
Alkali (NaOH) peels off auxiliary agent to peeling off productivity and the impact of efficiency.Add both of which as can be seen from Fig. to charge stripping efficiency and productivity
Increasing, and addition NaOH compares NaCl and improves more, productivity reaches 28.24%.
Embodiment 4
Different original solids content is on peeling off productivity and the impact of efficiency
Experimentation is with embodiment 1.
The initial content changing molybdenite micropowder in this embodiment is respectively 3.75,6.25,8.75,11.25,13.75 g,
Corresponding solid content is respectively 15,25,35,45,55 g/L.
Figure 13 be original solids content be the ultraviolet of gained molybdenum disulfide nano sheet suspension under 35 g/L, different time-can
See spectrum；Find out from figure, along with the prolongation of splitting time, the suction at 660 nm of the ultraviolet-visible absorption spectroscopy of centrifuged suspension
Luminosity is gradually increased, and according to Beer law, splitting time is the longest, and charge stripping efficiency is the highest.
Figure 14 is to peel off gained molybdenum disulfide nano sheet suspension under difference initial molybdenite solid content to peel off in difference
In time, gained molybdenum disulfide nano sheet obtains solid content and peels off productivity rate diagram.Found out by figure, along with the increasing of original solids content
Adding, detachment rate and productivity all have rising；When solid content is 15 g/L, the efficiency of stripping is maximum；Along with original solids content
Increase, peel off productivity when 45 g/L and 55 g/L and be more or less the same.
Embodiment 5
Different ultrasonic powers is on peeling off productivity and the impact of efficiency
Experimentation is with embodiment 1.
This embodiment, with embodiment 1, only changes embodiment 1 step 3 ultrasonic power, peels off ultrasonic power used and is respectively
200、240、280、320、350 W；
Figure 15 is when ultrasonic power is 320 W, the ultraviolet-visible of different splitting time gained molybdenum disulfide nano sheet suspension
Absorption spectrum；Finding out from figure, along with the prolongation of splitting time, the ultraviolet-visible absorption spectroscopy of centrifuged suspension is at 660 nm
Absorbance is gradually increased, and illustrates that charge stripping efficiency gradually steps up.
Figure 16 is the solid content of gained molybdenum disulfide nano sheet suspension under different ultrasonic power, under different splitting time
And peel off productivity, rate diagram.Along with the increase of ultrasonic stripping power, stripping productivity first increases and reduces afterwards, reaches when 280 W
Greatly.
Embodiment 6
Different sand mill rotating speeds is on peeling off productivity and the impact of efficiency
The experimentation of this embodiment, with embodiment 1, only changes the rotating speed of sand mill, respectively 1500,1800,2250 rpm.
Figure 17 be sand mill rotating speed be 1800 rpm, the purple of different splitting time gained molybdenum disulfide nano sheet suspension
Outward-visible absorption spectra.Finding out from figure, along with the prolongation of splitting time, charge stripping efficiency gradually steps up.
Figure 18 is to peel off gained molybdenum disulfide nano sheet suspension under sand mill different rotating speeds in different splitting times
Solid content and stripping productivity, rate diagram.It can be seen that gained molybdenum disulfide nano sheet productivity under three different rotating speeds of sand mill,
Detachment rate is more or less the same.
Embodiment 7
Different PVP content is on peeling off productivity and the impact of efficiency
The experimentation of this embodiment, with embodiment 1, only changes mol ratio: PVP/MoS2=0、0.25、0.5、1。
Figure 19 is PVP/MoS2When=1 under different splitting times the ultraviolet-visible of gained molybdenum disulfide nano sheet suspension
Absorption spectrum.Finding out from figure, splitting time is the longest, and the absorbance of suspension uv-visible absorption spectra at 660 nm is more
Greatly, according to Beer law, illustrate that splitting time is the longest, peel off productivity the highest.
Figure 20 is to peel off gained molybdenum disulfide nano sheet suspension consolidating in different splitting times under different PVP content to contain
Amount and stripping productivity, rate diagram.Along with the increase of PVP content, productivity and the speed of stripping all increase.
Effect test one
Sand milling the most ultrasonic, ultrasonic substep is peeled off and is coupled stripping contrast with " ultrasonic-sand milling ":
(1) independent ultrasonic stripping: 11.25 g molybdenite micropowders are scattered in 250 mL NMP formation suspension, add therewith
3.9 g PVP, ultrasonic 20 min make it fully dispersed, be placed on ultrasonic stripping in wide mouthed bottle, power is 280 W, and the time is
4 h, peel off post-treatment condition with embodiment 1.
(2) ultrasonic sand milling substep is peeled off: 11.25 g molybdenite micropowders are scattered in 250 mL NMP formation suspension,
Adding 3.9 g PVP therewith, ultrasonic 20 min make fully dispersed, be placed in sand milling chamber and carry out sand milling stripping, sand mill turns
Speed is 2250 rpm, and the time is 4 h, peels off post-treatment condition with embodiment 1.
(3) ultrasonic-sand milling coupling is peeled off: coupling splitting time is 4 h, and other are with embodiment 1.
Figure 21 is (left: the most ultrasonic；Right: ultrasonic, sand milling substep is peeled off) it is that sand milling the most ultrasonic, ultrasonic substep is peeled off
The uv-visible absorption spectra of different time gained molybdenum disulfide nano sheet.Along with the prolongation of splitting time, absorbance gradually increases
Add, Beer law illustrate that peeling off productivity gradually steps up.
Figure 22 is that sand milling the most ultrasonic, ultrasonic substep stripping couples gained under three kinds of modes such as stripping with " ultrasonic-sand milling "
Molybdenum disulfide nano sheet suspension stripping productivity in different splitting times, rate diagram.Can be seen that three kinds of different strippings
Under mode, coupling release effect can give full play to shock shear action and the synergy of ultrasonic cavitation of sand milling, from
And improve stripping productivity.
Effect test two
The stripping process of molybdenum disulfide nano sheet is with implementing 1；The chemical property of test gained molybdenum disulfide nano sheet.Will be super
Sound-sand milling coupling stripping suspension, in 8000-10000 rpm interval centrifugation, prepares few layer MoS2Nanometer sheet.Take 4 mg institutes
Obtain few layer MoS2Nanometer sheet is scattered in 950 ml DMF (N-N dimethylformamide) and 50 ml and draws in luxuriant and rich with fragrance solution and ultrasonic point
Dissipate, then take 4 ml and be coated on glass-carbon electrode, make working electrode.Then with saturated calomel electrode as reference electrode, platinum electricity
Extremely to electrode, carry out electrochemical property test.The sweep speed of the Linear Circulation volt-ampere of electrocatalytic hydrogen evolution performance is 2 mV/s.
Figure 23 is gained widow layer MoS2The electrocatalysis characteristic of nanometer sheet.Being found out by figure, high rotating speed is centrifuged gained widow layer MoS2Receive
Rice sheet is centrifuged gained sample than molybdenite micropowder and the slow-speed of revolution, has less OCP and bigger electric current density, and
Less Ta Feier slope.High rotating speed is centrifuged gained MoS2Nanometer sheet sample is thinner, and surface activity site is increased, and is more beneficial for
Liberation of hydrogen catalytic reaction.
Claims (5)
- The method that preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in the most ultrasonic-sand milling coupling, it is characterised in that include following step Rapid: 1) molybdenite micropowder is scattered in stripping solvent and forms suspension；2) dispersant, stripping auxiliary agent are dissolved in ultrasonic disperse in the suspension of step 1)；3) step 2) suspension after ultrasonic disperse peels off continuously under ultrasonic, sand milling coupling simultaneously and obtains molybdenum bisuphide and receive Rice sheet.
- The method that preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in the most ultrasonic-sand milling coupling, its feature Being, peeling off solvent is N-methyl pyrrole network alkanone, and dispersant is polyvinylpyrrolidone, and peeling off auxiliary agent is NaOH or NaCl.
- The method that preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in the most ultrasonic-sand milling coupling, its Being characterised by, the granularity of molybdenite micropowder is 5-50 micron, and the content of molybdenum bisuphide is more than 99.8%.
- The method that preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in the most ultrasonic-sand milling coupling, its Being characterised by, in step 1) suspension, the solid content of molybdenite micropowder is 10-60 g/L；Step 2) in dispersant micro-with molybdenite The mol ratio of powder is 0.1-1, and the mol ratio peeling off auxiliary agent and molybdenite micropowder is 0-1.
- The method that preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in the most ultrasonic-sand milling coupling, its Being characterised by, power ultrasonic in step 3) is 200-350 W, and rotating speed during sand milling is 1500-2250 rpm, coupling Time is 0.5-6 h.
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| CN114212781A (en) * | 2021-12-23 | 2022-03-22 | 江苏杉元科技有限公司 | Low-foam high-conductivity graphene aqueous slurry and preparation method thereof |
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