CN108190960A - It is a kind of that the method that lithium stripping prepares individual layer molybdenum disulfide is inserted based on electrolyte solvent heat - Google Patents
It is a kind of that the method that lithium stripping prepares individual layer molybdenum disulfide is inserted based on electrolyte solvent heat Download PDFInfo
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Abstract
The method that lithium stripping prepares individual layer molybdenum disulfide is inserted based on electrolyte solvent heat the invention discloses a kind of, using solvent-thermal method, in a kettle, with MoS2Powder is presoma, and electrolyte is solvent, and under the protection of high-purity argon gas, lithium ion in electrolyte is embedded into MoS2Between layer, unreacted MoS is removed by centrifuging process2, obtain the individual layer MoS of embedding lithium2Nano material, then by adding in acetone eccentric cleaning several times, the MoS of the single layer structure of high-purity has been prepared finally by deionized water supersound process2Nano material.Preparation method of the present invention is novel, and low manufacture cost, preparation process is simple, and lithium ion is made full use of to be embedded in MoS2Nano material, so as to effectively improve the yield of individual layer molybdenum sulfide.
Description
Technical field
The invention belongs to semiconductor nano materials and devices field, and in particular to a kind of to insert lithium stripping based on electrolyte solvent heat
From the method for preparing individual layer molybdenum disulfide.
Background technology
Semi-conductor industry has developed one of industry the most quick since being 21st century, development speed is considerably beyond with vapour
Turner industry and the traditional processing manufacturing industry that steel and iron industry is representative.Due to the presence of Moore's Law, i.e. " IC chip unit
The core number of area often spends 18 months and just increases one times ", the size of semiconductor still reduces at a terrific speed.Meanwhile it rubs
Your second law shows that the processing cost of chip while chip size reduces can exponentially increase.So consider technology hair
Exhibition and the factor of product cost input, the service life of germanium silicon semiconductor are walked to be at the end at last.With the arrival in " rear mole of epoch ", hair
The demand for opening up germanium silicon semiconductor alternative materials is extremely urgent.It is excellent with its by the two-dimensional layered-structure material of representative of graphene
Physicochemical property have been a great concern.Intrinsic band gap however, as graphene is zero so that being made of graphene film
FET current on/off ratios it is very low.With deepening continuously for research, it has been found that transition-metal sulphides（TMDCs）Have
The very much like two-dimensional layered structure with graphene.As the Typical Representative of TMDCs, molybdenum disulfide is due to its unique atom
Structure, adjustable band gap performance and higher current on/off ratio so that molybdenum disulfide can be good at being applied to low-power consumption
Device, in the application of electronic device have great potentiality.The nanoscale layer structure that molybdenum disulfide has so that size
The higher semiconductor chip of smaller, efficiency is manufactured as possibility, so molybdenum disulfide is in micro-nano magnitude logic circuit and crystalline substance
There is great application value in the preparation of body pipe.Although MoS2With very huge application prospect, but large scale, height
Quality monolayer MoS2Preparation be still a challenge subject.
In recent years, in order to obtain the large-sized individual layer MoS of large area2, people, which are widely applied liquid and remove, carrys out peeling layer
Shape molybdenum sulfide, intercalation cause spacing between layers to increase, and interlaminar action power reduces, and sonication is not changing chemical knot
Further auxiliary breaks Van der Waals force between layers to prepare individual layer two-dimension nano materials under the premise of structure, this is obtains big face
Product, large scale, high quality molybdenum sulfide open another new research direction and may.
Invention content
The purpose of the present invention is to solve the shortcomings of the prior art and defect, one kind is provided, lithium is inserted based on electrolyte solvent heat
The method that stripping prepares individual layer molybdenum disulfide.The preparation method of the present invention is novel, and low manufacture cost, preparation process is simple, fully
MoS is embedded in using lithium ion2Nano material becomes the individual layer MoS for preparing large area, large scale, high quality2Most effectual way.
To achieve the above object, the present invention adopts the following technical scheme that realization：
It is a kind of that the method that lithium stripping prepares individual layer molybdenum disulfide is inserted based on electrolyte solvent heat, specifically include following steps：
Step S1：Reaction vessel of the autoclave as solvent heat is chosen, the autoclave includes stainless steel autoclave body
And polytetrafluoroethylliner liner；
Step S2：Prepare LiPF6Electrolyte, the LiPF that will be obtained6Electrolyte is as Li+The presoma in source;
Step S3：Prepare MoS2, the MoS that will obtain2Presoma as solvent thermal reaction；
Step S4：Prepare the individual layer MoS of lithium insertion2Nano material；
Step S5：Individual layer MoS is prepared by eccentric cleaning, ultrasonic technique2。
Further, LiPF is prepared in the step S26The specific method of electrolyte is：In glove box, utilization is high-purity
The protection of Ar gas, by a certain amount of LiPF6Be dissolved in certain volume than diethyl carbonate and dimethyl carbonate in the mixed solvent,
Obtain certain density LiPF6Electrolyte.
Preferably, the diethyl carbonate and the volume ratio of dimethyl carbonate are 1:1, LiPF6Electrolyte it is a concentration of
1mol/l。
Further, MoS in the step S32Preparation method specifically include following steps：
Step S31：Prepare molybdenum trioxide：It will（30wt%）The hydrogen peroxide solution of concentration is poured into beaker, under condition of ice bath, is delayed
Slowly molybdenum powder is added in the hydrogen peroxide solution, and constantly stirred, after the reaction was complete after it, deionized water is added to this
In solution, continue to stir to get uniform orange solution, then the solution is placed in reaction kettle pass sequentially through hydro-thermal reaction,
Natural cooling, obtains reaction product 2-3 time at suction filtration using deionized water high speed centrifugation cleaning treatment repeatedly, finally will it is described instead
Product drying is answered to can obtain molybdenum trioxide.
Step S32：Prepare molybdenum disulfide：Thiocarbamide and molybdenum trioxide are added in deionized water, then stirred, then will
It, which is transferred in reaction kettle, passes sequentially through hydro-thermal reaction, natural cooling, filters separation, repeatedly clear using deionized water high speed centrifugation
It washes processing and obtains reaction product, reaction product drying finally be can obtain into crystal of molybdenum disulfide.
Further, in the step S31, mixing time 25min-45min；The hydrothermal reaction kettle volume is
75ml-150ml；The hydrothermal temperature is 150 DEG C -250 DEG C, hydrothermal conditions 30h-40h；The high speed centrifugation
Technological parameter be：Centrifuge RPMs are 6000-8000rpm, centrifugation time 10min-20min；The drying temperature is 60
DEG C -100 DEG C, drying time 10h-15h.
Further, in the step S32, mixing time 25min-45min；The hydrothermal reaction kettle volume is
25ml-75ml；The hydrothermal temperature is 200 DEG C -250 DEG C, hydrothermal conditions 20h-30h；The high speed centrifugation
Technological parameter be：Centrifuge RPMs are 6000-8000rpm, centrifugation time 10min-20min；The drying temperature is 60
DEG C -100 DEG C, drying time 10h-15h.
Further, the individual layer MoS of lithium insertion is prepared in the step S42The specific method of nanometer sheet material is：In hand
In casing, using the protection of high-purity Ar gas, the LiPF that will be prepared in the step S26It is prepared in electrolyte and the step S3
MoS2Mixing, which is placed in reaction kettle, to be sealed, and the reaction kettle being sealed is placed in air dry oven and is obtained by solvent thermal reaction
To MoS2Suspension after it has reacted natural cooling, then carries out low-speed centrifugal, and collection takes supernatant liquor, obtains the list of lithium insertion
Layer MoS2Nano material.
Preferably, the hydrothermal reaction kettle volume is 25ml-50ml；Solvent thermal reaction temperature is 100 DEG C -250 DEG C, molten
Agent heat treatment time is 36h-60h；The technological parameter of the low-speed centrifugal is：Centrifuge RPMs are 500-2000rpm, centrifugation time
For 15min-30min.
Further, the specific method of the step S5 is：Supernatant liquor in the step S4 is added in into acetone at a high speed
Eccentric cleaning 2-3 times, by the MoS of gained2Precipitation adds in deionized water and obtains the individual layer MoS of high-purity by being ultrasonically treated2Nanometer
Material.
Preferably, the ultracentrifugal technological parameter is：Centrifuge RPMs are 6000-8000rpm, and centrifugation time is
30min-45min；The ultrasonic time is 2h-4h.
Compared with prior art, the present invention is using solvent-thermal method, in a kettle, with MoS2Powder is presoma, electrolysis
Liquid is solvent, and under the protection of high-purity argon gas, lithium ion in electrolyte is embedded into MoS2Between layer, removed by centrifuging process
Unreacted MoS2, obtain the individual layer MoS of embedding lithium2Nano material, then by adding in acetone eccentric cleaning several times, finally by
Deionized water supersound process has prepared the MoS of the single layer structure of high-purity2Nano material.Preparation method of the present invention is novel, system
Make at low cost, preparation process is simple, and lithium ion is made full use of to be embedded in MoS2Nano material becomes and prepares large area, large scale, height
The individual layer MoS of quality2Most effectual way.
Description of the drawings
Fig. 1 is blocky molybdenum disulfide structure diagram；
Fig. 2 is the individual layer MoS of lithium insertion2Nanometer material structure schematic diagram；
Fig. 3 is the individual layer MoS of high-purity2Nanometer material structure schematic diagram；
Fig. 4 is individual layer molybdenum sulfide nanometer sheet Atomic Arrangement structure diagram；
Label declaration：1 is individual layer molybdenum disulfide nano sheet, and 2 be lithium ion, and 3 be S atom, and 4 be Mo atoms.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and embodiments.
Embodiment 1
（1）In glove box, using the protection of high-purity Ar gas, the LiPF of 1.519g is weighed6It is placed in the reagent bottle of 15ml, then
It measures 5ml diethyl carbonates and 5ml dimethyl carbonates is placed in 15ml reagent bottles, make it completely dissolved to form clear solution, i.e.,
LiPF for a concentration of 1mol/l6Electrolyte；
（2）Molybdenum powder 0.8g is weighed, then measures 5ml（30%）In the hydrogen peroxide solution merging 10ml beakers of concentration, in condition of ice bath
Under, slowly load weighted molybdenum powder is added in the hydrogen peroxide solution, and constantly stirs, after the reaction was complete after it, is measured
50ml deionized waters are added in the solution, are diluted to 0.15mol/L, continue to stir 25min, obtain uniform orange
Color solution is transferred it in 75ml reaction kettles, the hydro-thermal 30h at 150 DEG C, after its natural cooling, the breast that will obtain
Then white suspension cleans 2 times, centrifugation rate 6000rpm, centrifugation time by filtering with deionized water high speed centrifugation
Reaction product after cleaning is finally placed in drying 10h in 60 DEG C of air dry oven and can obtain molybdenum trioxide by 10min；
（3）Molybdenum trioxide 0.08g, thiocarbamide 0.32g are weighed, 10ml deionized waters is then measured and pours into the beaker of 20ml, will claim
Measured sample and thiocarbamide are added in the 10ml deionized waters, then stir 25min, are then transferred into 25ml reaction kettles
In, the hydro-thermal 20h at 200 DEG C after its natural cooling, obtained black solid by filtering is detached, then uses deionization
Water high speed centrifugation cleans 2 times, centrifugation rate 6000rpm, centrifugation time 10min and the reaction product after cleaning finally is placed in 60
DEG C air dry oven in drying 10h can obtain molybdenum disulfide, Fig. 1 is blocky molybdenum disulfide structure diagram, wherein 1 is single
Layer molybdenum disulfide nano sheet；
（4）Molybdenum disulfide 0.05g is weighed, in glove box, using the protection of high-purity Ar gas, measures the LiPF of 10ml6Electrolyte
It pours into the reaction kettle of 25ml, load weighted molybdenum disulfide is placed in the electrolyte, the reaction kettle being sealed is placed in air blast
In drying box, 36h is heat-treated under 100 DEG C of temperature conditions, after it has reacted natural cooling, then carries out low-speed centrifugal removal not
The molybdenum sulfide of reaction, centrifugation rate 500rpm, centrifugation time 15min, collection take supernatant liquor to obtain the individual layer MoS that lithium is embedded in2
Nano material, Fig. 2 are the individual layer MoS of lithium insertion2Nanometer material structure schematic diagram, wherein 1 is individual layer molybdenum sulfide nanometer sheet, 2 are
Lithium ion；
（5）The individual layer MoS that will be embedded in containing lithium2The supernatant liquor of nano material adds in 200ml acetone high speed centrifugation and cleans 2 times,
Centrifugation rate is 6000rpm, centrifugation time 30min, and the molybdenum sulfide precipitation of gained is added in deionized water passes through 600W power
Lower supersound process 2h obtains the individual layer MoS of high-purity2Nano material, Fig. 3 are the individual layer MoS of high-purity2Nanometer material structure is illustrated
Figure, wherein 1 is individual layer molybdenum disulfide nano sheet；Fig. 4 is individual layer molybdenum disulfide nano sheet Atomic Arrangement structure diagram, wherein 3
It is Mo atoms for S atom, 4.
Embodiment 2
（1）In glove box, using the protection of high-purity Ar gas, the LiPF of 3.038g is weighed6It is placed in the reagent bottle of 30ml, then
It measures 10ml diethyl carbonates and 10ml dimethyl carbonates is placed in reagent bottle, make it completely dissolved to form clear solution, as
The LiPF of a concentration of 1mol/l6Electrolyte；
（2）Molybdenum powder 1.2g is weighed, then measures 10ml（30%）In the hydrogen peroxide solution merging 15ml beakers of concentration, in ice bath item
Under part, slowly load weighted molybdenum powder is added in the hydrogen peroxide solution, and constantly stirs, after after it, the reaction was complete, amount
50ml deionized waters are taken, is added in the solution, is diluted to 0.2mol/L, continue to stir 35min, are obtained uniform orange
Color solution is transferred it in 100ml reaction kettles, the hydro-thermal 36h at 200 DEG C, after its natural cooling, the breast that will obtain
Then white suspension cleans 2 times, centrifugation rate 7000rpm, centrifugation time by filtering with deionized water high speed centrifugation
Reaction product after cleaning is finally placed in drying 13h in 80 DEG C of air dry oven and can obtain molybdenum trioxide by 15min；
（3）Molybdenum trioxide 0.12g, thiocarbamide 0.48g are weighed, 30ml deionized waters is then measured and pours into the beaker of 50ml, will claim
Measured sample and thiocarbamide are added in the 30ml deionized waters, then stir 35min, are then transferred into 50ml reaction kettles
In, the hydro-thermal 25h at 230 DEG C after its natural cooling, obtained black solid by filtering is detached, then uses deionization
Water high speed centrifugation cleans 2 times, centrifugation rate 7000rpm, centrifugation time 15min and the reaction product after cleaning finally is placed in 80
DEG C air dry oven in drying 13h can obtain molybdenum disulfide, Fig. 1 is blocky molybdenum disulfide structure diagram, wherein 1 is single
Layer molybdenum disulfide nano sheet；
（4）Molybdenum disulfide 0.1g is weighed, in glove box, using the protection of high-purity Ar gas, measures the LiPF of 20ml6Electrolyte falls
In the reaction kettle for entering 30ml, load weighted molybdenum disulfide is placed in the electrolyte, the reaction kettle being sealed is placed in air blast does
In dry case, 48h is heat-treated under 200 DEG C of temperature conditions, after it has reacted natural cooling, then carry out low-speed centrifugal removal it is not anti-
The molybdenum sulfide answered, centrifugation rate 1000rpm, centrifugation time 24min, collection take supernatant liquor to obtain the individual layer MoS that lithium is embedded in2It receives
Rice material, Fig. 2 are the individual layer MoS2 nanometer material structure schematic diagrames of lithium insertion, wherein 1 is individual layer molybdenum sulfide nanometer sheet, 2 be lithium
Ion；
（5）The individual layer MoS that will be embedded in containing lithium2The supernatant liquor of nano material adds in 200ml acetone high speed centrifugation and cleans 2 times,
Centrifugation rate is 7000rpm, centrifugation time 40min, and the molybdenum sulfide precipitation of gained is added in deionized water passes through 600W power
Lower supersound process 3h obtains the individual layer MoS of high-purity2Nano material, Fig. 3 are the individual layer MoS of high-purity2Nanometer material structure is illustrated
Figure, wherein 1 is individual layer molybdenum disulfide nano sheet；Fig. 4 is individual layer molybdenum disulfide nano sheet Atomic Arrangement structure diagram, wherein 3
It is Mo atoms for S atom, 4.
Embodiment 3
（1）In glove box, using the protection of high-purity Ar gas, the LiPF of 4.557g is weighed6It is placed in the reagent bottle of 50ml, then
It measures 15ml diethyl carbonates and 15ml dimethyl carbonates is placed in reagent bottle, make it completely dissolved to form clear solution, as
The LiPF6 electrolyte of a concentration of 1mol/l；
（2）Molybdenum powder 2g is weighed, then measures 20ml（30%）In the hydrogen peroxide solution merging 30ml beakers of concentration, in condition of ice bath
Under, slowly load weighted molybdenum powder is added in the hydrogen peroxide solution, and constantly stirs, after the reaction was complete after it, is measured
50ml deionized waters are added in the solution, are diluted to 0.25mol/L, continue to stir 45min, obtain uniform orange
Color solution is transferred it in 150ml reaction kettles, the hydro-thermal 40h at 250 DEG C, after its natural cooling, the breast that will obtain
Then white suspension cleans 3 times, centrifugation rate 8000rpm, centrifugation time by filtering with deionized water high speed centrifugation
Reaction product after cleaning is finally placed in drying 15h in 100 DEG C of air dry oven and can obtain molybdenum trioxide by 20min；
（3）Molybdenum trioxide 0.2g, thiocarbamide 0.8g are weighed, 50ml deionized waters is then measured and pours into the beaker of 100ml, will weigh
Good sample and thiocarbamide is added in the 50ml deionized waters, is then stirred 45min, is then transferred into 75ml reaction kettles
In, the hydro-thermal 30h at 250 DEG C after its natural cooling, obtained black solid by filtering is detached, then uses deionization
Water high speed centrifugation cleans 3 times, centrifugation rate 8000rpm, centrifugation time 20min and the reaction product after cleaning finally is placed in 100
DEG C air dry oven in drying 15h can obtain molybdenum disulfide, Fig. 1 is blocky molybdenum disulfide structure diagram, wherein 1 is single
Layer molybdenum disulfide nano sheet；
（4）Molybdenum disulfide 0.15g is weighed, in glove box, using the protection of high-purity Ar gas, measures the LiPF of 30ml6Electrolyte
It pours into the reaction kettle of 50ml, load weighted molybdenum disulfide is placed in the electrolyte, the reaction kettle being sealed is placed in air blast
In drying box, 60h is heat-treated under 250 DEG C of temperature conditions, after it has reacted natural cooling, then carries out low-speed centrifugal removal not
The molybdenum sulfide of reaction, centrifugation rate 2000rpm, centrifugation time 30min, collection take supernatant liquor to obtain the individual layer MoS that lithium is embedded in2
Nano material, Fig. 2 are the individual layer MoS of lithium insertion2Nanometer material structure schematic diagram, wherein 1 be individual layer molybdenum disulfide nano sheet, 2
For lithium ion；
（5）The individual layer MoS that will be embedded in containing lithium2The supernatant liquor of nano material adds in 200ml acetone high speed centrifugation and cleans 3 times,
Centrifugation rate is 8000rpm, centrifugation time 45min, and the molybdenum sulfide precipitation of gained is added in deionized water passes through 600W power
Lower supersound process 4h obtains the individual layer MoS of high-purity2Nano material, Fig. 3 are the individual layer MoS of high-purity2Nanometer material structure is illustrated
Figure, wherein 1 is individual layer molybdenum disulfide nano sheet；Fig. 4 is individual layer molybdenum disulfide nano sheet Atomic Arrangement structure diagram, wherein 3
It is Mo atoms for S atom, 4.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (9)
1. a kind of insert the method that lithium stripping prepares individual layer molybdenum disulfide based on electrolyte solvent heat, it is characterised in that：
Step S1：Choose reaction vessel of the autoclave as solvent heat；
Step S2：Prepare LiPF6Electrolyte, the LiPF that will be obtained6Electrolyte is as Li+The presoma in source;
Step S3：Prepare MoS2, the MoS that will obtain2Presoma as solvent thermal reaction；
Step S4：Prepare the individual layer MoS of lithium insertion2Nano material, specific method are：In glove box, the guarantor of high-purity Ar gas is utilized
Shield, the LiPF that will be prepared in the step S26The MoS prepared in electrolyte and the step S32Mixing is placed on close in reaction kettle
It seals, the reaction kettle being sealed is placed in air dry oven, MoS is obtained by solvent thermal reaction2Suspension treats that it has been reacted
It after natural cooling, then is centrifuged, collection takes supernatant liquor, obtains the individual layer MoS of lithium insertion2Nano material；
Step S5：The supernatant liquor obtained in the step S4 is prepared into individual layer MoS by eccentric cleaning, ultrasonic technique2Nanometer
Material.
2. it is according to claim 1 it is a kind of the method that lithium stripping prepares individual layer molybdenum disulfide is inserted based on electrolyte solvent heat,
It is characterized in that：LiPF is prepared in the step S26The specific method of electrolyte is：In glove box, high-purity Ar gas is utilized
Protection, by LiPF6Diethyl carbonate and dimethyl carbonate in the mixed solvent are dissolved in, obtains LiPF6Electrolyte.
3. it is according to claim 2 it is a kind of the method that lithium stripping prepares individual layer molybdenum disulfide is inserted based on electrolyte solvent heat,
It is characterized in that：The diethyl carbonate and the volume ratio of dimethyl carbonate are 1:1, LiPF6A concentration of 1mol/ of electrolyte
l。
4. it is according to claim 1 it is a kind of the method that lithium stripping prepares individual layer molybdenum disulfide is inserted based on electrolyte solvent heat,
It is characterized in that：MoS in the step S32Preparation method specifically include following steps：
Step S31：Prepare molybdenum trioxide：The hydrogen peroxide solution of 30wt% is poured into beaker, under condition of ice bath, slowly by molybdenum
Powder is added in the hydrogen peroxide solution, and is constantly stirred, and after the reaction was complete after it, deionized water is added to the solution
In, continue to stir to get uniform orange solution, then the solution is placed in reaction kettle and passes sequentially through hydro-thermal reaction, nature
Cooling is filtered and is handled 2-3 times using deionized water eccentric cleaning repeatedly, reaction product is obtained, finally by the reaction product
Drying obtains molybdenum trioxide；
Step S32：Prepare molybdenum disulfide：Thiocarbamide and molybdenum trioxide are added in deionized water, then stirred, then by its turn
It moves on in reaction kettle and passes sequentially through hydro-thermal reaction, natural cooling and filter separation, reacted repeatedly using deionized water eccentric cleaning
The reaction product finally is dried to obtain crystal of molybdenum disulfide by product.
5. it is according to claim 4 it is a kind of based on electrolyte solvent heat insert lithium stripping prepare individual layer vulcanize two molybdenums method,
It is characterized in that：In the step S31, mixing time 25min-45min；The reaction kettle volume is 75ml-150ml；
The hydrothermal temperature is 150 DEG C -250 DEG C, hydrothermal conditions 30h-40h；The technological parameter of the centrifugation is：From
Heart revolution is 6000-8000rpm, centrifugation time 10min-20min；The drying temperature is 60 DEG C -100 DEG C, during drying
Between 10h-15h.
6. it is according to claim 4 it is a kind of the method that lithium stripping prepares individual layer molybdenum disulfide is inserted based on electrolyte solvent heat,
It is characterized in that：In the step S32, mixing time 25min-45min；The reaction kettle volume is 25ml-75ml；Institute
The hydrothermal temperature stated is 200 DEG C -250 DEG C, hydrothermal conditions 20h-30h；The technological parameter of the centrifugation is：Centrifugation
Revolution is 6000-8000rpm, centrifugation time 10min-20min；The drying temperature is 60 DEG C -100 DEG C, drying time
10h-15h。
7. it is according to claim 1 it is a kind of the method that lithium stripping prepares individual layer molybdenum disulfide is inserted based on electrolyte solvent heat,
It is characterized in that：In the step S4, reaction kettle volume is 25ml-50ml；Solvent thermal reaction temperature is 100 DEG C -250 DEG C, molten
Agent heat treatment time is 36h-60h；The technological parameter of the centrifugation is：Centrifuge RPMs are 1000-3000rpm, and centrifugation time is
15min-30min。
8. it is according to claim 1 it is a kind of the method that lithium stripping prepares individual layer molybdenum disulfide is inserted based on electrolyte solvent heat,
It is characterized in that：The specific method of the step S5 is：Supernatant liquor in the step S4 is added in into acetone eccentric cleaning 2-3
It is secondary, the precipitation of gained is added in into deionized water and obtains individual layer MoS by being ultrasonically treated2Nano material.
9. it is according to claim 8 it is a kind of the method that lithium stripping prepares individual layer molybdenum disulfide is inserted based on electrolyte solvent heat,
It is characterized in that：The technological parameter of the centrifugation is：Centrifuge RPMs are 6000-8000rpm, centrifugation time 30min-45min；
The sonication treatment time is 2h-4h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108865131A (en) * | 2018-07-04 | 2018-11-23 | 青岛大学 | A kind of method that bi-polar electrochemical method prepares molybdenum disulfide quantum dot and radio-radar absorber simultaneously |
| CN109666946A (en) * | 2019-01-29 | 2019-04-23 | 东北大学 | A kind of melten salt electriochemistry graft process prepares two-dimensional layer MoS2The method of material |
| CN110776006A (en) * | 2018-07-27 | 2020-02-11 | 香港科技大学 | Preparation method of ultrathin antimony sulfide nanosheet used as negative electrode material of lithium/sodium ion battery |
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| CN108865131B (en) * | 2018-07-04 | 2021-02-09 | 青岛大学 | Method for simultaneously preparing molybdenum disulfide quantum dots and electromagnetic wave absorbent by bipolar electrochemical method |
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| CN110776006B (en) * | 2018-07-27 | 2023-07-21 | 香港科技大学 | Preparation method of ultrathin antimony sulfide nanosheets serving as lithium/sodium ion battery anode materials |
| CN109666946A (en) * | 2019-01-29 | 2019-04-23 | 东北大学 | A kind of melten salt electriochemistry graft process prepares two-dimensional layer MoS2The method of material |
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