CN104495935B - A kind of strip preparation method of molybdenum disulfide nano sheet layer - Google Patents
A kind of strip preparation method of molybdenum disulfide nano sheet layer Download PDFInfo
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- CN104495935B CN104495935B CN201410717991.5A CN201410717991A CN104495935B CN 104495935 B CN104495935 B CN 104495935B CN 201410717991 A CN201410717991 A CN 201410717991A CN 104495935 B CN104495935 B CN 104495935B
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- 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
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- 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
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- 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 kind of molybdenum bisuphide（MoS2）The strip preparation method of nanoscale twins.By the stirring or ultrasonically treated in the mixed solvent containing oxidant, raw material molybdenum bisuphide is stripped and forms molybdenum disulfide nano sheet.The method uses cheap reagent, operates at room temperature, and energy consumption is low, pollution-free, efficiency high, and the molybdenum disulfide nano sheet layer of preparation can be widely applied to the field such as energy storage and conversion, catalysis, lubrication and various composites.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, a kind of individual layer or few layer are in particular, provided and containing defective
Or the strip preparation method of the molybdenum disulfide nano sheet layer of hole.
Background technology
Molybdenum bisuphide can easily be extracted from natural molybdenite and prepared, in lubrication, catalysis, energy storage and various composite woods
It is widely used in material.Single molybdenum bisuphide lamella wraps a sandwich structure group for molybdenum atom layer by upper and lower two S atoms layer
Into about 0.8 ~ 1.0 nanometer of thickness.Molybdenum bisuphide lamella has good mechanical property（The TPa of Young's modulus 0.33, fracture are strong
Spend 23 GPa）, in face electron mobility up to 200 ~ 500 cm2/ V.s, high current on/off ratio 108, thus in flexible electrical
Son, energy stores（Lithium ion battery, ultracapacitor, fuel cell）, the numerous areas such as Industrial Catalysis have extensively using preceding
Scape.Therefore, many research work have also been attracted to be devoted to developing inexpensive, efficient molybdenum bisuphide stripping technology of preparing.
Molybdenum bisuphide bulk material can directly using adhesive tape mechanics stripping means or in appropriate organic solvent（Such as
1-METHYLPYRROLIDONE, NMP）Middle ultrasound is realized peeling off and prepared.Research provides high quality monolayer or few layer is received based on the former
Rice lamella sample, but be not suitable for plant-scale application；The current charge stripping efficiency of the latter still has much room for improvement, though with curing
In the good solvent NMP that molybdenum surface can be close carry out that ultrasonic stripping is repeated several times, its yield is still below 20%.At present, improved stripping
Technology is mostly to weaken the interaction between molybdenum bisuphide lamella using alkali metal compound intercalation, then real by ultrasound again
Existing high yield is peeled off.Such technology path can reach more than 90% individual layer charge stripping efficiency, but still come with some shortcomings, such as alkali
Metal intercalation overlong time（More than 2 days）, intercalation temperature it is higher（More than 100 DEG C）, the energy consumption of preparation process is larger, cycle mistake
Grow, and molybdenum bisuphide prepared by lithium intercalation also needs to recover the 2H lattice structures of its semi-conductor type by high annealing.For optimization is made
Standby process, electrochemical method is also suggested the preparation process for accelerating molybdenum disulfide hybrid compound, its preparation time can contract
It is as short as 5-6 hours.But raw material molybdenum bisuphide need to be combined composition and be made electrochemistry electricity by the technology by binding agent, conductive agent etc.
Pole, preparation process is significantly restricted in electrode size（Limit yield）The not good electrical conductivity with electrochemical electrode.Additionally, conductive agent
Addition have also been introduced external pollutant, cause that subsequent treatment is difficult, increase preparation cost.
Chinese patent（201310704356.0）Disclose carries out pre-treatment, so to molybdenum bisuphide using a kind of using liquid nitrogen
The method that ultrasound is peeled off to improve nanoscale twins charge stripping efficiency in NMP afterwards.Chinese patent（201410086208.x）It is open
It is a kind of by molybdenum bisuphide in intercalation processing under HTHP, the method peeled off then is realized by ultrasound again.Chinese patent
（201110347902.9）Disclose a kind of stripping of use jet flow cavitation technique realization to molybdenum disulfide nano sheet layer.
The stripping technology of preparing of existing molybdenum disulfide nano sheet layer is summarized, still suffer from that the preparation process cycle is long, energy consumption is big,
The problems such as charge stripping efficiency is remained to be further improved.
The content of the invention
It is an object of the invention to propose one kind can at ambient conditions, realize molybdenum bisuphide low cost, low energy consumption, height
The strip preparation method of efficiency, environment-friendly molybdenum disulfide nano sheet layer.
To achieve the above object, the technical solution adopted by the present invention is as follows：
Raw material molybdenum disulfide powder is added in the organic solvent containing oxidant, at stirring or ultrasound treatment patterns
Reason 10 minutes ~ 20 hours, controlling reaction temperature is 0 ~ 100 DEG C, and it is curing to be stripped into raw material molybdenum disulfide powder
Molybdenum nanometer sheet；Filter, dry, obtain dry molybdenum disulfide nano sheet；Wherein：Organic solvent quality is raw material molybdenum bisuphide
10 ~ 5000 times, oxidant quality is 0.001 ~ 0.1 times of organic solvent quality.
In the present invention, the stirring or sonication treatment time are 20 minutes ~ 10 hours.
In the present invention, described ultrasonically treated for Probe Ultrasonic Searching or water bath sonicator, its power is 100 ~ 2000 W.
In the present invention, described oxidant refers to that the material of redox reaction can occur with molybdenum bisuphide, wherein wrapping
Include hydrogen peroxide（H2O2）, potassium permanganate, potassium bichromate, ammonium persulfate, oleum, in perchloric acid or concentrated nitric acid more than one.
In the present invention, described molybdenum bisuphide directly buys the molybdenum bisuphide commonly used from business without by special
Pretreatment.
In the present invention, described organic solvent is the solvent that can have good affinity with molybdenum bisuphide surface, including N- first
Base -2-Pyrrolidone（NMP）, N,N-dimethylformamide（DMF）, DMAC N,N' dimethyl acetamide, gamma-butyrolacton and can lead to
Overregulating solvent composition control surface energy, realization has the mixed solvent of good affinity with molybdenum bisuphide（Surface can be about 70
mJ/mol）, such as ethanol-water mixed solvent.
In the present invention, when stirring or be ultrasonically treated, controlling reaction temperature is 10 ~ 50 DEG C.
In the present invention, described organic solvent quality is 50-1000 times of raw material molybdenum bisuphide, and oxidant quality is organic
0.005-0.05 times of solvent quality.
In the present invention, the yield of the molybdenum disulfide nano sheet of gained is more than 60 wt%.
The beneficial effects of the present invention are：The method uses cheap reagent, operates at room temperature, and energy consumption is low, pollution-free, effect
Rate is high, and the molybdenum disulfide nano sheet layer of preparation can be widely applied to energy storage with conversion, catalysis, lubrication and various composite woods
The fields such as material.
Brief description of the drawings
The SEM SEM image of the unstripped molybdenum disulfide particles of Fig. 1.
Fig. 2 H2O2-NMP（Mass ratio 1：19）The molybdenum disulfide nano sheet layer AFM peeled off in mixed solvent
（AFM）Image.
Fig. 3 H2O2-NMP（Mass ratio 1：19）The molybdenum disulfide nano sheet layer transmission electron microscope peeled off in mixed solvent
（TEM）Image.
Specific embodiment
Technical scheme is illustrated below by instantiation.It should be understood that the present invention mention one or more
Step is not repelled before and after the combination step also and is existed between other method and steps, or these specifically mentioned steps also
May be inserted into other method and steps.It should also be understood that these examples are merely to illustrate the present invention rather than limit of the invention
Scope.Unless otherwise indicated, the numbering of various method steps is only the purpose for differentiating various method steps, rather than to limit each method
Ordering or limit practical range of the invention, its relativeness is altered or modified, without substantial technological content alteration
Under conditions of, when being also considered as enforceable category of the invention.
For the various problems that prior art is present, the present inventor is by long-term research and practice, it is proposed that the present invention
Technical scheme, the program can realize the system of high efficiency, low cost, the individual layer of scale or few layer molybdenum disulfide nano sheet layer
It is standby.Especially the technology path of spontaneous stripping avoids prolonged high temperature intercalation operation, reduces the energy consumption of production process.Together
When, the present invention is it is also proposed that when ultrasound peels off molybdenum bisuphide, addition oxidant can greatly improve the product that ultrasound peels off molybdenum bisuphide
Rate, shows good practical prospect.
Embodiment 1
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONE mixed solvents containing hydrogen peroxide
（NMP：30% H2O2The mass ratio of the aqueous solution is 10：1）, in being stirred 10 hours at 35 DEG C, it is subsequently cooled to room temperature.In 5000 turns/
Centrifugation is collected upper liquid and simultaneously filters, dries for 10 minutes to remove unstripped powder under point rotating speed.Final molybdenum bisuphide of peeling off is received
The yield of rice lamella is about 60 wt%（Relative to material powder）.The scanning electron microscopy of molybdenum bisuphide material powder before stripping
Mirror image is as shown in figure 1, the atomic force microscopy and transmission electron microscope image of nanoscale twins after peeling off are respectively such as Fig. 2 and Fig. 3
Shown, wherein atomic force microscopy confirms that the height of lamella is 0.95 nm, meets typical individual layer molybdenum disulfide nano sheet
Height.
Embodiment 2
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONE mixed solvents containing hydrogen peroxide
（NMP：30% H2O2The mass ratio of the aqueous solution is 100：1）, in being stirred 10 hours at 35 DEG C, it is subsequently cooled to room temperature.In 5000
Centrifugation is collected upper liquid and simultaneously filters, dries for 10 minutes to remove unstripped powder under rev/min rotating speed.It is final to peel off molybdenum bisuphide
The yield of nanoscale twins is more than 60 wt%（Relative to material powder）.
Embodiment 3
100 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONE mixed solvents containing hydrogen peroxide
In（NMP：30% H2O2The mass ratio of the aqueous solution is 10：1）, in being stirred 10 hours at 35 DEG C, it is subsequently cooled to room temperature.In 5000
Centrifugation is collected upper liquid and simultaneously filters, dries for 10 minutes to remove unstripped powder under rev/min rotating speed.It is final to peel off molybdenum bisuphide
The yield of nanoscale twins is more than 30 wt%（Relative to material powder）.
Embodiment 4
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONE mixed solvents containing hydrogen peroxide
（NMP：30% H2O2The mass ratio of the aqueous solution is 10：1）, in being stirred 2 hours at 35 DEG C, it is subsequently cooled to room temperature.In 5000 turns/
Centrifugation is collected upper liquid and simultaneously filters, dries for 10 minutes to remove unstripped powder under point rotating speed.Final molybdenum bisuphide of peeling off is received
The yield of rice lamella is more than 60 wt%（Relative to material powder）.
Embodiment 5
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONE mixed solvents containing hydrogen peroxide
（NMP：30% H2O2The mass ratio of the aqueous solution is 10：1）, use power to be carried out for 500 W Probe Ultrasonic Searchings wave producers ultrasonically treated
Room temperature is cooled to after 1 hour.In 10 minutes are centrifuged under 5000 revs/min of rotating speeds to remove unstripped powder, upper liquid and mistake are collected
Filter, dry.The final yield for peeling off molybdenum disulfide nano sheet layer is more than 60 wt%（Relative to material powder）.
Embodiment 6
1 gram of molybdenum bisuphide powder is scattered in 100 milliliters of METHYLPYRROLIDONE mixed solvents containing hydrogen peroxide
（NMP：30% H2O2The mass ratio of the aqueous solution is 10：1）, use power to be carried out for 500 W Probe Ultrasonic Searchings wave producers ultrasonically treated
Room temperature is cooled to after 1 hour.In 10 minutes are centrifuged under 5000 revs/min of rotating speeds to remove unstripped powder, upper liquid and mistake are collected
Filter, dry.The final yield for peeling off molybdenum disulfide nano sheet layer is more than 50 wt%（Relative to material powder）.
Embodiment 7
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONE mixed solvents containing hydrogen peroxide
（NMP：30% H2O2The mass ratio of the aqueous solution is 100：1）, in being stirred 10 hours at 15 DEG C, it is subsequently cooled to room temperature.In 5000
Centrifugation is collected upper liquid and simultaneously filters, dries for 10 minutes to remove unstripped powder under rev/min rotating speed.It is final to peel off molybdenum bisuphide
The yield of nanoscale twins is more than 40 wt%（Relative to material powder）.
Embodiment 8
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONE mixed solvents containing hydrogen peroxide
（NMP：30% H2O2The mass ratio of the aqueous solution is 10：1）, use power to be carried out for 200 W Probe Ultrasonic Searchings wave producers ultrasonically treated
Room temperature is cooled to after 1 hour.In 10 minutes are centrifuged under 5000 revs/min of rotating speeds to remove unstripped powder, upper liquid and mistake are collected
Filter, dry.The final yield for peeling off molybdenum disulfide nano sheet layer is more than 60 wt%（Relative to material powder）.
Embodiment 9
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONE mixed solvents containing hydrogen peroxide
（NMP：30% H2O2The mass ratio of the aqueous solution is 10：1）, it is 200 W water bath sonicators treatment 2 to use power（1 hour or 2 small
When）Room temperature is cooled to after hour.In 10 minutes are centrifuged under 5000 revs/min of rotating speeds to remove unstripped powder, upper liquid is collected
And filter, dry.The final yield for peeling off molybdenum disulfide nano sheet layer is in 60 wt%（Relative to material powder）.
Embodiment 10
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of dimethylformamides containing hydrogen peroxide（DMF：30% H2O2Water
The mass ratio of solution is 10：1）, in being stirred 10 hours at 35 DEG C, it is subsequently cooled to room temperature.In centrifugation under 5000 revs/min of rotating speeds
To remove unstripped powder, collect upper liquid and filter, dry within 10 minutes.The final yield for peeling off molybdenum disulfide nano sheet layer
More than 60 wt%（Relative to material powder）.
Embodiment 11
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONE mixed solvents containing potassium permanganate
In（NMP：Potassium permanganate mass ratio is 10：1）, in being stirred 10 hours at 35 DEG C, it is subsequently cooled to room temperature.Turn in 5000 revs/min
The lower centrifugation of speed is collected upper liquid and filters, dries for 10 minutes to remove unstripped powder.It is final to peel off molybdenum disulfide nano sheet
The yield of layer is about 60 wt%（Relative to material powder）.The scanning electron microscope diagram of molybdenum bisuphide material powder before stripping
As shown in figure 1, peel off after nanoscale twins atomic force microscopy and transmission electron microscope image respectively as shown in Figures 2 and 3.
Embodiment 12
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of DMF solutions containing potassium permanganate（DMF：Potassium permanganate quality
Than being 10：1）, in being stirred 10 hours at 35 DEG C, it is subsequently cooled to room temperature.In 10 minutes are centrifuged under 5000 revs/min of rotating speeds removing
Unstripped powder is removed, upper liquid is collected and is filtered, dries.The final yield for peeling off molybdenum disulfide nano sheet layer is about 60 wt%
（Relative to material powder）.After the scanning electron microscope image of molybdenum bisuphide material powder is as shown in figure 1, peel off before stripping
Nanoscale twins atomic force microscopy and transmission electron microscope image respectively as shown in Figures 2 and 3.
Comparative example 1
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONEs, it is small in stirring 10 at 35 DEG C
When, it is subsequently cooled to room temperature.In 10 minutes are centrifuged under 5000 revs/min of rotating speeds to remove unstripped powder, upper liquid and mistake are collected
Filter, dry.The final yield for peeling off molybdenum disulfide nano sheet layer is less than 10 wt%（Relative to material powder）.
Comparative example 2
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONE mixed solvents containing hydrogen peroxide
（NMP：30% H2O2The mass ratio of the aqueous solution is 5000：1）, in being stirred 10 hours at 35 DEG C, it is subsequently cooled to room temperature.In 5000
Centrifugation is collected upper liquid and simultaneously filters, dries for 10 minutes to remove unstripped powder under rev/min rotating speed.It is final to peel off molybdenum bisuphide
The yield of nanoscale twins is less than 10 wt%（Relative to material powder）.
Comparative example 3
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of METHYLPYRROLIDONE mixed solvents containing hydrogen peroxide
（NMP：30% H2O2The mass ratio of the aqueous solution is 10：1）, in being stirred 10 hours at 100 DEG C, it is subsequently cooled to room temperature.In 5000
Centrifugation is collected upper liquid and simultaneously filters, dries for 10 minutes to remove unstripped powder under rev/min rotating speed.It is final to peel off molybdenum bisuphide
The yield of nanoscale twins is less than 10 wt%（Relative to material powder）.
Comparative example 4
20 milligrams of molybdenum bisuphide powders are scattered in 20 milliliters of dichloromethane mixed solvents containing hydrogen peroxide（Dichloromethane
Alkane：30% H2O2The mass ratio of the aqueous solution is 10：1）, in being stirred 10 hours at 35 DEG C, it is subsequently cooled to room temperature.In 5000 revs/min
10 minutes are centrifuged under rotating speed to remove unstripped powder, collect upper liquid and filters, dries.It is final to peel off molybdenum disulfide nano
The yield of lamella is less than 10 wt%（Relative to material powder）.
Claims (6)
1. the strip preparation method of a kind of molybdenum disulfide nano sheet layer, it is characterised in that comprise the following steps that：By raw material curing
Molybdenum powder is added in the organic solvent containing oxidant, is processed 10 minutes~20 hours using stirring or ultrasound treatment patterns, control
Reaction temperature processed is 10~50 DEG C, and it is molybdenum disulfide nano sheet to be stripped into raw material molybdenum disulfide powder；Filter, dry, obtain
To dry molybdenum disulfide nano sheet；Wherein：Organic solvent quality is 10~5000 times of raw material molybdenum bisuphide, oxidant quality
It is 0.01~0.1 times of organic solvent quality；The oxidant include hydrogen peroxide, potassium permanganate, potassium bichromate, ammonium persulfate,
In oleum, perchloric acid or concentrated nitric acid more than one；The organic solvent includes METHYLPYRROLIDONE, N, N- diformazans
In base formamide or DMAC N,N' dimethyl acetamide any one.
2. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, it is characterised in that described to stir
Mix or sonication treatment time is 20 minutes~10 hours.
3. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, it is characterised in that described
It is ultrasonically treated for Probe Ultrasonic Searching or water bath sonicator, its power is 100~2000W.
4. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, it is characterised in that described
Molybdenum bisuphide directly buys the molybdenum bisuphide commonly used from business without by special pretreatment.
5. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, it is characterised in that described
Organic solvent quality is 50-1000 times of raw material molybdenum bisuphide, and oxidant quality is 0.01-0.05 times of organic solvent quality.
6. the strip preparation method of a kind of molybdenum disulfide nano sheet layer according to claim 1, it is characterised in that gained
The yield of molybdenum disulfide nano sheet is more than 60wt%.
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| 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 |
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| 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 |
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