CN104495935A - Preparation method of molybdenum disulfide nanosheet in stripping manner - Google Patents
Preparation method of molybdenum disulfide nanosheet in stripping manner Download PDFInfo
- Publication number
- CN104495935A CN104495935A CN201410717991.5A CN201410717991A CN104495935A CN 104495935 A CN104495935 A CN 104495935A CN 201410717991 A CN201410717991 A CN 201410717991A CN 104495935 A CN104495935 A CN 104495935A
- Authority
- CN
- China
- Prior art keywords
- molybdenum disulfide
- nano sheet
- disulfide nano
- molybdenumdisulphide
- sheet layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a preparation method of a molybdenum disulfide nanosheet in a stripping manner. Stirring or ultrasonic treatment is carried out in a mixed solvent containing an oxidizing agent, and a raw material, namely molybdenum disulfide, is stripped, so that the molybdenum disulfide nanosheet is formed. The preparation method of the molybdenum disulfide nanosheet has the advantages that a cheap reagent is adopted, operation is carried out at room temperature, energy consumption is low, no pollution is caused, efficiency is high, and the prepared molybdenum disulfide nanosheet can be widely applied to the fields of energy storage and conversion, catalysis, lubrication, various composite materials and the like.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, in particular, provide a kind of individual layer or few layer and the strip preparation method of molybdenum disulfide nano sheet layer containing defectiveness or hole.
Background technology
Molybdenumdisulphide can extract preparation easily from natural molybdenum glance, is widely used in lubrication, catalysis, energy storage and various matrix material.The sandwich structure that single molybdenumdisulphide lamella wraps a molybdenum atom layer by upper and lower two S atomic shells forms, thickness about 0.8 ~ 1.0 nanometer.Molybdenumdisulphide lamella has electronic mobility in good mechanical property (Young's modulus 0.33 TPa, breaking tenacity 23 GPa), face can reach 200 ~ 500 cm
2/ V.s, high current on/off ratio 10
8, thus at numerous areas such as flexible electronic, stored energy (lithium ion battery, ultracapacitor, fuel cell), Industrial Catalysis, there is wide application prospect.Therefore, many research work have also been attracted to be devoted to development low cost, high efficiency molybdenumdisulphide stripping technology of preparing.
Molybdenumdisulphide bulk material directly can adopt sealing tape mechanics stripping means or preparation is peeled off in ultrasonic realization in suitable organic solvent (as N-Methyl pyrrolidone, NMP).Based on the former, research provides high quality monolayer or few layer nanoscale twins sample, but is not suitable for plant-scale application; The current charge stripping efficiency of the latter still has much room for improvement, even if repeatedly repeat ultrasonic stripping in the good solvent NMP close with molybdenumdisulphide surface energy, its productive rate is still lower than 20%.At present, mostly the lift-off technology of improvement is that employing alkali metal compound intercalation weakens the interaction between molybdenumdisulphide lamella, and then is peeled off by the ultrasonic high yield that realizes.Such technological line can reach the individual layer charge stripping efficiency of more than 90%, but still come with some shortcomings, as basic metal intercalation overlong time (more than 2 days), intercalation temperature higher (more than 100 DEG C), the energy consumption of preparation process is larger, excessive cycle, and molybdenumdisulphide prepared by lithium intercalation also needs the 2H crystalline network being recovered its semi-conductor type by high temperature annealing.For optimized fabrication process, electrochemical method is also suggested the preparation process accelerating molybdenum disulfide hybrid compound, its preparation time can be foreshortened to 5-6 hour.But raw material molybdenumdisulphide need be made electrochemical electrode by the composition that combines such as binding agent, conductive agent by this technology, preparation process is significantly limited to electrode size (limiting output) and the not good specific conductivity of electrochemical electrode.In addition, the interpolation of conductive agent have also been introduced external pollutent, causes subsequent disposal difficulty, increases preparation cost.
Chinese patent (201310704356.0) disclose adopt a kind of adopt liquid nitrogen to carry out pre-treatment to molybdenumdisulphide and then in NMP ultrasonic stripping to improve the method for nanoscale twins charge stripping efficiency.Chinese patent (201410086208.x) discloses a kind of by molybdenumdisulphide intercalation processing under High Temperature High Pressure, then again by the ultrasonic method realizing peeling off.Chinese patent (201110347902.9) discloses a kind of jet flow cavitation technique that adopts and realizes stripping to molybdenum disulfide nano sheet layer.
Sum up the stripping technology of preparing of existing molybdenum disulfide nano sheet layer, still there is the problems such as the preparation process cycle is grown, energy consumption is large, charge stripping efficiency remains to be further improved.
Summary of the invention
The object of the invention is to propose a kind of can at ambient conditions, realize the strip preparation method of molybdenumdisulphide low cost, less energy-consumption, high-level efficiency, eco-friendly molybdenum disulfide nano sheet layer.
For achieving the above object, the technical solution used in the present invention is as follows:
Joined by raw material molybdenum disulfide powder in the organic solvent containing oxygenant, adopt and stir or ultrasound treatment patterns process 10 minutes ~ 20 hours, controlling temperature of reaction is 0 ~ 100 DEG C, makes raw material molybdenum disulfide powder be stripped into as molybdenum disulfide nano sheet; Filtration, drying, obtain dry molybdenum disulfide nano sheet; Wherein: organic solvent quality is 10 ~ 5000 times of raw material molybdenumdisulphide, oxygenant quality is 0.001 ~ 0.1 times of organic solvent quality.
In the present invention, described stirring or sonication treatment time are 20 minutes ~ 10 hours.
In the present invention, described supersound process is Probe Ultrasonic Searching or water bath sonicator, and its power is 100 ~ 2000 W.
In the present invention, described oxygenant refer to can with the material of molybdenumdisulphide generation redox reaction, comprising in hydrogen peroxide (H2O2), potassium permanganate, potassium bichromate, ammonium persulphate, oleum, perchloric acid or concentrated nitric acid more than one.
In the present invention, described molybdenumdisulphide directly to buy in business conventional molybdenumdisulphide and not through special pre-treatment.
In the present invention, described organic solvent is can have the solvent of good affinity with molybdenumdisulphide surface, comprise METHYLPYRROLIDONE (NMP), N, dinethylformamide (DMF), N, N-N,N-DIMETHYLACETAMIDE, gamma-butyrolactone and the mixed solvent (surface energy is about 70 mJ/mol) by regulating solvent composition control surface energy, realization and molybdenumdisulphide to have good affinity, as ethanol-water mixed solvent.
In the present invention, when stirring or supersound process, controlling temperature of reaction is 10 ~ 50 DEG C.
In the present invention, described organic solvent quality is 50-1000 times of raw material molybdenumdisulphide, and oxygenant quality is 0.005-0.05 times of organic solvent quality.
In the present invention, the productive rate of the molybdenum disulfide nano sheet of gained is greater than 60 wt%.
Beneficial effect of the present invention is: the method adopts cheap reagent, operate under room temperature, energy consumption is low, pollution-free, efficiency is high, and the molybdenum disulfide nano sheet layer of preparation can be widely used in the field such as energy storage and conversion, catalysis, lubrication and various matrix materials.
Accompanying drawing explanation
The scanning electronic microscope SEM image of the unstripped molybdenum disulfide particles of Fig. 1.
Fig. 2 H
2o
2-NMP(mass ratio 1:19) molybdenum disulfide nano sheet layer atomic force microscope (AFM) image peeled off in mixed solvent.
Fig. 3 H
2o
2-NMP(mass ratio 1:19) molybdenum disulfide nano sheet layer transmission electron microscope (TEM) image peeled off in mixed solvent.
Embodiment
Below by specific examples, technical scheme of the present invention is described.Should be appreciated that, one or more steps that the present invention mentions are not repelled also there is other method and step before and after described combination step, or can also insert other method and step between these specifically mentioned steps.Should also be understood that these examples are only not used in for illustration of the present invention to limit the scope of the invention.Except as otherwise noted, the numbering of various method steps is only the object differentiating various method steps, but not for restriction each method ordering or limit practical range of the present invention, the change of its relativeness or adjustment, under the condition without substantial technological content alteration, when being also considered as the enforceable category of the present invention.
For the various problems that prior art exists, the present inventor, through long-term Researching and practicing, proposes technical scheme of the present invention, and the program can realize high-level efficiency, low cost, the individual layer of mass-producing or the preparation of few layer molybdenum disulfide nano sheet layer.The technological line of especially spontaneous stripping avoids the operation of long high temperature intercalation, reduces the energy consumption of production process.Meanwhile, the present invention also proposes when ultrasonic stripping molybdenumdisulphide, adds the productive rate that oxygenant significantly can improve ultrasonic stripping molybdenumdisulphide, demonstrates good practical prospect.
Embodiment 1
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing (NMP:30% H in the METHYLPYRROLIDONE mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 10:1), stir 10 hours at 35 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is about 60 wt%(relative to material powder).Before stripping, the scanning electron microscope image of molybdenumdisulphide raw material powder as shown in Figure 1, the atomic force microscopy of the nanoscale twins after stripping and transmission electron microscope image are respectively as shown in Figures 2 and 3, wherein atomic force microscopy confirms that the height of lamella is 0.95 nm, meets the height of typical individual layer molybdenum disulfide nano sheet.
Embodiment 2
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing (NMP:30% H in the METHYLPYRROLIDONE mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 100:1), stir 10 hours at 35 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is greater than 60 wt%(relative to material powder).
Embodiment 3
100 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing (NMP:30% H in the METHYLPYRROLIDONE mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 10:1), stir 10 hours at 35 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is greater than 30 wt%(relative to material powder).
Embodiment 4
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing (NMP:30% H in the METHYLPYRROLIDONE mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 10:1), stir 2 hours at 35 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is greater than 60 wt%(relative to material powder).
Embodiment 5
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing (NMP:30% H in the METHYLPYRROLIDONE mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 10:1), adopt power to be that 500 W Probe Ultrasonic Searching wave producers carry out supersound process and are cooled to room temperature after 1 hour.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is greater than 60 wt%(relative to material powder).
Embodiment 6
1 gram of molybdenumdisulphide powder is scattered in 100 milliliters containing (NMP:30% H in the METHYLPYRROLIDONE mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 10:1), adopt power to be that 500 W Probe Ultrasonic Searching wave producers carry out supersound process and are cooled to room temperature after 1 hour.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is greater than 50 wt%(relative to material powder).
Embodiment 7
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing (NMP:30% H in the METHYLPYRROLIDONE mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 100:1), stir 10 hours at 15 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is greater than 40 wt%(relative to material powder).
Embodiment 8
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing (NMP:30% H in the METHYLPYRROLIDONE mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 10:1), adopt power to be that 200 W Probe Ultrasonic Searching wave producers carry out supersound process and are cooled to room temperature after 1 hour.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is greater than 60 wt%(relative to material powder).
Embodiment 9
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing (NMP:30% H in the METHYLPYRROLIDONE mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 10:1), adopt power to be 200 W water bath sonicator process 2(1 hour still 2 hours?) hour after be cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is relative to material powder in 60 wt%().
Embodiment 10
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters of dimethyl formamide (DMF:30% H containing hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 10:1), stir 10 hours at 35 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is greater than 60 wt%(relative to material powder).
Embodiment 11
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing in the METHYLPYRROLIDONE mixed solvent of potassium permanganate (NMP: potassium permanganate mass ratio is 10:1), stir 10 hours at 35 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is about 60 wt%(relative to material powder).Before stripping, the scanning electron microscope image of molybdenumdisulphide raw material powder as shown in Figure 1, and the atomic force microscopy of the nanoscale twins after stripping and transmission electron microscope image are respectively as shown in Figures 2 and 3.
Embodiment 12
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters of DMF solution (DMF: potassium permanganate mass ratio is 10:1) containing potassium permanganate, stir 10 hours at 35 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is about 60 wt%(relative to material powder).Before stripping, the scanning electron microscope image of molybdenumdisulphide raw material powder as shown in Figure 1, and the atomic force microscopy of the nanoscale twins after stripping and transmission electron microscope image are respectively as shown in Figures 2 and 3.
Comparative example 1
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters of METHYLPYRROLIDONEs, stir 10 hours at 35 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is less than 10 wt%(relative to material powder).
Comparative example 2
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing (NMP:30% H in the METHYLPYRROLIDONE mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 5000:1), stir 10 hours at 35 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is less than 10 wt%(relative to material powder).
Comparative example 3
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing (NMP:30% H in the METHYLPYRROLIDONE mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 10:1), stir 10 hours at 100 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is less than 10 wt%(relative to material powder).
Comparative example 4
20 milligrams of molybdenumdisulphide powders are scattered in 20 milliliters containing (methylene dichloride: 30% H in the methylene dichloride mixed solvent of hydrogen peroxide
2o
2the mass ratio of the aqueous solution is 10:1), stir 10 hours at 35 DEG C, be then cooled to room temperature.Under 5000 revs/min of rotating speeds centrifugal 10 minutes to remove unstripped powder, collect upper liquid and filter, dry.The productive rate of final stripping molybdenum disulfide nano sheet layer is less than 10 wt%(relative to material powder).
Claims (9)
1. the strip preparation method of a molybdenum disulfide nano sheet layer, it is characterized in that concrete steps are as follows: joined by raw material molybdenum disulfide powder in the organic solvent containing oxygenant, adopt and stir or ultrasound treatment patterns process 10 minutes ~ 20 hours, controlling temperature of reaction is 0 ~ 100 DEG C, makes raw material molybdenum disulfide powder be stripped into as molybdenum disulfide nano sheet; Filtration, drying, obtain dry molybdenum disulfide nano sheet; Wherein: organic solvent quality is 10 ~ 5000 times of raw material molybdenumdisulphide, oxygenant quality is 0.001 ~ 0.1 times of organic solvent quality.
2. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, is characterized in that described stirring or sonication treatment time are 20 minutes ~ 10 hours.
3. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, it is characterized in that described supersound process is Probe Ultrasonic Searching or water bath sonicator, its power is 100 ~ 2000 W.
4. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, it is characterized in that described oxygenant refer to can with the material of molybdenumdisulphide generation redox reaction, to be specially in hydrogen peroxide, potassium permanganate, potassium bichromate, ammonium persulphate, oleum, perchloric acid or concentrated nitric acid more than one.
5. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, is characterized in that described molybdenumdisulphide directly to buy in business conventional molybdenumdisulphide and not through special pre-treatment.
6. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, it is characterized in that described organic solvent is can have the solvent of good affinity with molybdenumdisulphide surface, be specially METHYLPYRROLIDONE, N, dinethylformamide, N, in N-N,N-DIMETHYLACETAMIDE or gamma-butyrolactone, any one, or be ethanol-water mixed solvent.
7. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, when it is characterized in that stirring or supersound process, controlling temperature of reaction is 10 ~ 50 DEG C.
8. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, it is characterized in that described organic solvent quality is 50-1000 times of raw material molybdenumdisulphide, oxygenant quality is 0.005-0.05 times of organic solvent quality.
9. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, is characterized in that the productive rate of the molybdenum disulfide nano sheet of gained is greater than 60 wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410717991.5A CN104495935B (en) | 2014-12-03 | 2014-12-03 | A kind of strip preparation method of molybdenum disulfide nano sheet layer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410717991.5A CN104495935B (en) | 2014-12-03 | 2014-12-03 | A kind of strip preparation method of molybdenum disulfide nano sheet layer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104495935A true CN104495935A (en) | 2015-04-08 |
| CN104495935B CN104495935B (en) | 2017-06-16 |
Family
ID=52937415
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410717991.5A Active CN104495935B (en) | 2014-12-03 | 2014-12-03 | A kind of strip preparation method of molybdenum disulfide nano sheet layer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104495935B (en) |
Cited By (28)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104986802A (en) * | 2015-07-08 | 2015-10-21 | 华东师范大学 | Platy nanometer material and preparation method thereof |
| CN105056977A (en) * | 2015-07-28 | 2015-11-18 | 复旦大学 | Hydrogen evolution reaction catalyst and preparation method thereof |
| CN105316084A (en) * | 2015-11-24 | 2016-02-10 | 苏州盖德精细材料有限公司 | Gear lubricating oil nanometer additives and preparation method thereof |
| CN105668631A (en) * | 2016-03-14 | 2016-06-15 | 西安建筑科技大学 | Preparing method of single-layer or few-layer molybdenum disulfide nanometer material |
| CN105776349A (en) * | 2016-03-14 | 2016-07-20 | 金堆城钼业股份有限公司 | Preparation method of layered MoS2-Fe3O4 nanocomposite |
| CN105858727A (en) * | 2016-05-26 | 2016-08-17 | 金堆城钼业股份有限公司 | Preparing method for 2H-MoS2 nanosheets |
| CN106064833A (en) * | 2016-05-26 | 2016-11-02 | 金堆城钼业股份有限公司 | One is prepared 2H MoS by molybdenum concntrate2the method of nanometer sheet |
| CN106099053A (en) * | 2016-06-03 | 2016-11-09 | 东华大学 | A kind of molybdenum sulfide/selenizing molybdenum composite material and preparation thereof and application |
| CN106379940A (en) * | 2016-11-24 | 2017-02-08 | 厦门理工学院 | Two-dimensional nano-molybdenum disulfide and preparation method thereof |
| CN106564954A (en) * | 2016-11-04 | 2017-04-19 | 西安建筑科技大学 | Method for preparing graphene-like molybdenum disulfide through low-temperature reduction |
| CN106564953A (en) * | 2016-11-04 | 2017-04-19 | 西安建筑科技大学 | Method for reducing preparation of graphene-like molybdenum disulfide through carbohydrate organic carbon |
| CN106564952A (en) * | 2016-11-04 | 2017-04-19 | 西安建筑科技大学 | Method for preparing graphene-like molybdenum disulfide-graphene composite material by reducing carbohydrate organic carbon |
| CN106582720A (en) * | 2016-11-04 | 2017-04-26 | 西安建筑科技大学 | Method for preparing graphene-like molybdenum disulfide-bismuth molybdate composite material through saccharide organic carbon reduction |
| CN106596651A (en) * | 2016-12-05 | 2017-04-26 | 黑龙江大学 | Molybdenum disulfide/magnesium hydroxide nano composite material as well as preparation method and application thereof |
| CN106622297A (en) * | 2016-11-04 | 2017-05-10 | 西安建筑科技大学 | A method of preparing a graphene-like molybdenum disulfide-graphene composite material through protein substance reduction |
| CN106629851A (en) * | 2016-11-04 | 2017-05-10 | 西安建筑科技大学 | Method for reducing preparation of graphene-like molybdenum disulfide from protein substance |
| CN106732667A (en) * | 2016-11-04 | 2017-05-31 | 西安建筑科技大学 | A kind of protein matter reduction prepares the preparation method of class Graphene molybdenum bisuphide bismuth molybdate composite |
| CN106876731A (en) * | 2017-01-23 | 2017-06-20 | 吉林大学 | A kind of molybdenum disulfide nano superstructure material and its application |
| CN108039459A (en) * | 2017-11-20 | 2018-05-15 | 复旦大学 | A kind of preparation method of yolk-shell structures molybdenum disulfide@carbon electrode materials |
| CN108529570A (en) * | 2018-05-21 | 2018-09-14 | 西北师范大学 | The method for preparing transient metal sulfide nanometer sheet using the coupling ultrasonic wave microfacies stripping of biliquid system |
| CN108987746A (en) * | 2018-07-03 | 2018-12-11 | 陕西科技大学 | A kind of fixed three-dimensional porous nano reticular structure MoS of extra granular2Composite granule and its preparation method and application |
| CN109095502A (en) * | 2018-10-16 | 2018-12-28 | 大连理工大学 | A kind of microemulsion removing prepares the method that single layer lacks layer molybdenum disulfide |
| CN109665563A (en) * | 2019-01-31 | 2019-04-23 | 内蒙古大学 | A method of it removing natural molybdenite and prepares two-dimentional molybdenum disulfide nano material |
| CN110642295A (en) * | 2019-10-25 | 2020-01-03 | 四川大学 | Molybdenum disulfide nanosheet layer stripping preparation method based on solid-phase mechanochemical reactor |
| CN110697781A (en) * | 2019-11-08 | 2020-01-17 | 上海理工大学 | Preparation method of two-dimensional material of graphene quantum dot adhesion lamellar molybdenum disulfide |
| CN114314529A (en) * | 2022-01-09 | 2022-04-12 | 西北大学 | Preparation method for obtaining gallium selenide nanosheet through potassium dichromate auxiliary stripping |
| CN114956178A (en) * | 2022-04-08 | 2022-08-30 | 湖南大学 | Electrochemical stripping method of two-dimensional layered material |
| CN115072676A (en) * | 2022-06-22 | 2022-09-20 | 佛山(华南)新材料研究院 | Method for preparing two-dimensional material by mechanical stripping assisted by chemical method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102398920A (en) * | 2011-11-07 | 2012-04-04 | 北京航空航天大学 | Method for preparing two-dimensional nano molybdenum disulfide by jet cavitation technology |
| CN102583547A (en) * | 2012-03-07 | 2012-07-18 | 长安大学 | Preparation method of monolayer MoS2 nano-sheet solution |
| CN103641171A (en) * | 2013-11-19 | 2014-03-19 | 江苏大学 | Method used for regulating synthesis of MoS2 ultrathin nano sheets using Zn<2+> |
| CN103641172A (en) * | 2013-12-19 | 2014-03-19 | 中国科学院上海硅酸盐研究所 | Method for preparing nanometer layered molybdenum disulfide |
| CN103771517A (en) * | 2014-01-17 | 2014-05-07 | 哈尔滨工业大学 | Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets |
| CN103787417A (en) * | 2014-03-07 | 2014-05-14 | 深圳先进技术研究院 | Preparation method of magnetic layered molybdenum disulfide nanosheets |
-
2014
- 2014-12-03 CN CN201410717991.5A patent/CN104495935B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102398920A (en) * | 2011-11-07 | 2012-04-04 | 北京航空航天大学 | Method for preparing two-dimensional nano molybdenum disulfide by jet cavitation technology |
| CN102583547A (en) * | 2012-03-07 | 2012-07-18 | 长安大学 | Preparation method of monolayer MoS2 nano-sheet solution |
| CN103641171A (en) * | 2013-11-19 | 2014-03-19 | 江苏大学 | Method used for regulating synthesis of MoS2 ultrathin nano sheets using Zn<2+> |
| CN103641172A (en) * | 2013-12-19 | 2014-03-19 | 中国科学院上海硅酸盐研究所 | Method for preparing nanometer layered molybdenum disulfide |
| CN103771517A (en) * | 2014-01-17 | 2014-05-07 | 哈尔滨工业大学 | Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets |
| CN103787417A (en) * | 2014-03-07 | 2014-05-14 | 深圳先进技术研究院 | Preparation method of magnetic layered molybdenum disulfide nanosheets |
Cited By (39)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104986802A (en) * | 2015-07-08 | 2015-10-21 | 华东师范大学 | Platy nanometer material and preparation method thereof |
| CN105056977A (en) * | 2015-07-28 | 2015-11-18 | 复旦大学 | Hydrogen evolution reaction catalyst and preparation method thereof |
| CN105316084A (en) * | 2015-11-24 | 2016-02-10 | 苏州盖德精细材料有限公司 | Gear lubricating oil nanometer additives and preparation method thereof |
| CN105776349B (en) * | 2016-03-14 | 2017-06-13 | 金堆城钼业股份有限公司 | A kind of stratiform MoS2‑Fe3O4The preparation method of nano composite material |
| CN105668631A (en) * | 2016-03-14 | 2016-06-15 | 西安建筑科技大学 | Preparing method of single-layer or few-layer molybdenum disulfide nanometer material |
| CN105776349A (en) * | 2016-03-14 | 2016-07-20 | 金堆城钼业股份有限公司 | Preparation method of layered MoS2-Fe3O4 nanocomposite |
| CN105858727A (en) * | 2016-05-26 | 2016-08-17 | 金堆城钼业股份有限公司 | Preparing method for 2H-MoS2 nanosheets |
| CN106064833A (en) * | 2016-05-26 | 2016-11-02 | 金堆城钼业股份有限公司 | One is prepared 2H MoS by molybdenum concntrate2the method of nanometer sheet |
| CN106099053A (en) * | 2016-06-03 | 2016-11-09 | 东华大学 | A kind of molybdenum sulfide/selenizing molybdenum composite material and preparation thereof and application |
| CN106622297B (en) * | 2016-11-04 | 2018-12-14 | 西安建筑科技大学 | A kind of protein matter reduction preparation class graphene molybdenum disulfide-graphene composite material method |
| CN106564952B (en) * | 2016-11-04 | 2018-06-29 | 西安建筑科技大学 | A kind of method that carbohydrate organic carbon reduction prepares class graphene molybdenum disulfide-graphene composite material |
| CN106564952A (en) * | 2016-11-04 | 2017-04-19 | 西安建筑科技大学 | Method for preparing graphene-like molybdenum disulfide-graphene composite material by reducing carbohydrate organic carbon |
| CN106582720A (en) * | 2016-11-04 | 2017-04-26 | 西安建筑科技大学 | Method for preparing graphene-like molybdenum disulfide-bismuth molybdate composite material through saccharide organic carbon reduction |
| CN106732667B (en) * | 2016-11-04 | 2018-12-14 | 西安建筑科技大学 | A kind of protein matter reduction preparation class graphene molybdenum disulfide-bismuth molybdate composite material preparation method |
| CN106622297A (en) * | 2016-11-04 | 2017-05-10 | 西安建筑科技大学 | A method of preparing a graphene-like molybdenum disulfide-graphene composite material through protein substance reduction |
| CN106629851A (en) * | 2016-11-04 | 2017-05-10 | 西安建筑科技大学 | Method for reducing preparation of graphene-like molybdenum disulfide from protein substance |
| CN106732667A (en) * | 2016-11-04 | 2017-05-31 | 西安建筑科技大学 | A kind of protein matter reduction prepares the preparation method of class Graphene molybdenum bisuphide bismuth molybdate composite |
| CN106564954A (en) * | 2016-11-04 | 2017-04-19 | 西安建筑科技大学 | Method for preparing graphene-like molybdenum disulfide through low-temperature reduction |
| CN106582720B (en) * | 2016-11-04 | 2018-12-07 | 西安建筑科技大学 | A kind of carbohydrate organic carbon reduction preparation class graphene molybdenum disulfide-bismuth molybdate composite material method |
| CN106629851B (en) * | 2016-11-04 | 2018-04-24 | 西安建筑科技大学 | A kind of method that protein matter reduction prepares class graphene molybdenum disulfide |
| CN106564954B (en) * | 2016-11-04 | 2018-04-24 | 西安建筑科技大学 | A kind of method that low-temperature reduction prepares class graphene molybdenum disulfide |
| CN106564953A (en) * | 2016-11-04 | 2017-04-19 | 西安建筑科技大学 | Method for reducing preparation of graphene-like molybdenum disulfide through carbohydrate organic carbon |
| CN106379940B (en) * | 2016-11-24 | 2018-05-29 | 厦门理工学院 | A kind of two-dimensional nano molybdenum disulfide and preparation method thereof |
| CN106379940A (en) * | 2016-11-24 | 2017-02-08 | 厦门理工学院 | Two-dimensional nano-molybdenum disulfide and preparation method thereof |
| CN106596651A (en) * | 2016-12-05 | 2017-04-26 | 黑龙江大学 | Molybdenum disulfide/magnesium hydroxide nano composite material as well as preparation method and application thereof |
| CN106876731A (en) * | 2017-01-23 | 2017-06-20 | 吉林大学 | A kind of molybdenum disulfide nano superstructure material and its application |
| CN108039459A (en) * | 2017-11-20 | 2018-05-15 | 复旦大学 | A kind of preparation method of yolk-shell structures molybdenum disulfide@carbon electrode materials |
| CN108529570A (en) * | 2018-05-21 | 2018-09-14 | 西北师范大学 | The method for preparing transient metal sulfide nanometer sheet using the coupling ultrasonic wave microfacies stripping of biliquid system |
| CN108987746A (en) * | 2018-07-03 | 2018-12-11 | 陕西科技大学 | A kind of fixed three-dimensional porous nano reticular structure MoS of extra granular2Composite granule and its preparation method and application |
| CN108987746B (en) * | 2018-07-03 | 2021-04-30 | 陕西科技大学 | Three-dimensional porous nano-network structure MoS fixed by ultra-small particles2Composite powder and preparation method and application thereof |
| CN109095502A (en) * | 2018-10-16 | 2018-12-28 | 大连理工大学 | A kind of microemulsion removing prepares the method that single layer lacks layer molybdenum disulfide |
| CN109665563A (en) * | 2019-01-31 | 2019-04-23 | 内蒙古大学 | A method of it removing natural molybdenite and prepares two-dimentional molybdenum disulfide nano material |
| CN110642295A (en) * | 2019-10-25 | 2020-01-03 | 四川大学 | Molybdenum disulfide nanosheet layer stripping preparation method based on solid-phase mechanochemical reactor |
| CN110642295B (en) * | 2019-10-25 | 2021-08-03 | 四川大学 | Molybdenum disulfide nanosheet layer stripping preparation method based on solid-phase mechanochemical reactor |
| CN110697781A (en) * | 2019-11-08 | 2020-01-17 | 上海理工大学 | Preparation method of two-dimensional material of graphene quantum dot adhesion lamellar molybdenum disulfide |
| CN114314529A (en) * | 2022-01-09 | 2022-04-12 | 西北大学 | Preparation method for obtaining gallium selenide nanosheet through potassium dichromate auxiliary stripping |
| CN114956178A (en) * | 2022-04-08 | 2022-08-30 | 湖南大学 | Electrochemical stripping method of two-dimensional layered material |
| CN114956178B (en) * | 2022-04-08 | 2023-08-08 | 湖南大学 | Electrochemical stripping method for two-dimensional layered material |
| CN115072676A (en) * | 2022-06-22 | 2022-09-20 | 佛山(华南)新材料研究院 | Method for preparing two-dimensional material by mechanical stripping assisted by chemical method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104495935B (en) | 2017-06-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104495935A (en) | Preparation method of molybdenum disulfide nanosheet in stripping manner | |
| Liang et al. | A chronicle review of nonsilicon (Sn, Sb, Ge)‐based lithium/sodium‐ion battery alloying anodes | |
| Rahman et al. | Nanostructured silicon anodes for high‐performance lithium‐ion batteries | |
| CN109235024B (en) | Carbon cloth loaded nickel sulfide-molybdenum sulfide heterogeneous nanosheet array structure and preparation method thereof | |
| Chang et al. | Recent developments in advanced anode materials for lithium-ion batteries | |
| JP2019530190A (en) | Composite, its preparation method and use in lithium ion secondary battery | |
| Xiao et al. | Recent developments of two-dimensional anode materials and their composites in lithium-ion batteries | |
| Mukherjee et al. | Exfoliated transition metal dichalcogenide nanosheets for supercapacitor and sodium ion battery applications | |
| Bashir et al. | A review of the energy storage aspects of chemical elements for lithium-ion based batteries | |
| CN102307807A (en) | Method for manufacturing a SnO2 composite material and carbon nanotubes and/or carbon nanofibres, material obtained by the method, and lithium battery electrode comprising said material | |
| CN101937985A (en) | Graphene/titanium dioxide lithium ion battery cathode material and preparation method | |
| CN109546139A (en) | A kind of metal sulfide/carbon composite, preparation method and its application in cell negative electrode material | |
| Narsimulu et al. | Designed lamination of binder-free flexible iron oxide/carbon cloth as high capacity and stable anode material for lithium-ion batteries | |
| Tao et al. | Rational designing of MoSe2 nanosheets in carbon framework for high-performance potassium-ion batteries | |
| Lu et al. | Engineering metal selenides for sodium-and potassium-ion batteries | |
| CN105366662A (en) | Preparing method for sulfur-doped graphene | |
| CN111769272A (en) | Bi @ C hollow nanosphere composite material and preparation method and application thereof | |
| CN112707386A (en) | Preparation method and application of waste biomass derived graphene material | |
| CN103482674A (en) | Preparation method of copper oxide nanowires and application of copper oxide nanowires in negative electrode of lithium ion battery | |
| Zia et al. | MXene, silicene and germanene: preparation and energy storage applications | |
| CN107634193B (en) | Porous ferrous sulfide nanowire and nitrogen-doped carbon composite material as well as preparation method and application thereof | |
| Wang et al. | N-doped carbon coated CoO nanowire arrays derived from zeolitic imidazolate framework-67 as binder-free anodes for high-performance lithium storage | |
| Li et al. | Research progress of SiOx-based anode materials for lithium-ion batteries | |
| CN105161690A (en) | Method for improving charge-discharge cycling capacity of molybdenum disulfide by doping graphene and titanium dioxide | |
| CN112331845B (en) | Preparation method of cobaltosic oxide nanowire array negative electrode material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant |