CN109437307A - A kind of method of efficient preparation high quality molybdenum disulfide nano line - Google Patents
A kind of method of efficient preparation high quality molybdenum disulfide nano line Download PDFInfo
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- CN109437307A CN109437307A CN201811559699.XA CN201811559699A CN109437307A CN 109437307 A CN109437307 A CN 109437307A CN 201811559699 A CN201811559699 A CN 201811559699A CN 109437307 A CN109437307 A CN 109437307A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
A kind of method of efficient preparation high quality molybdenum disulfide nano line, comprising the following steps: firstly, preparing suitable surfactant solution, suitable structure directing agent is then added thereto again and is stirred mixing, obtains solution A；Secondly, weighing suitable ammonium molybdate and thioacetamide is respectively molybdenum source and sulphur source, it is stirred in deionized water solution uniformly, obtains solution B；Again, solution A is slowly added dropwise into B solution, ibid, then suitable reducing agent hydrazine hydrate is added thereto；Finally, for adjustment oil bath pot temperature to 100-120 DEG C, reaction time 10-24h, the mixing speed of shuttle shape magneton is 20-60rpm after hydrazine hydrate is added completely into, after reaction, reaction product is repeatedly centrifuged and deionization washs.
Description
Technical field
The present invention relates to technical field of nano material, and in particular to a kind of efficiently to prepare high quality molybdenum disulfide nano line
Method.
Background technique
Molybdenum disulfide is a kind of two-dimentional transition-metal sulphides, with the layer structure similar to graphene by pass
Note.Due to its unique electricity, acoustics, optically and mechanically performance, so that it is in lithium ion battery negative material, photocatalysis material
The application fields such as material, energy storage material and electrochemical sensor have extensive research.
In its crystal structure, it is similar to graphene, interlayer atom is combined in the form of covalent bond, and between layers
It is combined with Van der Waals force, the interplanar distance of (002) crystal face is 0.61nm, this size is significantly greater than lithium ion, and it is theoretical
Capacity is up to 1290mAh/g, significantly larger than graphene.Therefore, the research for being applied to new energy battery has huge dive
Power.
Currently, according to the inventors knowledge, the main method for preparing molybdenum disulfide has mechanical stripping method, hydrothermal synthesis method, ultrasound
Stripping method (the research article of such as Coleman et al.), chemical vapour deposition technique.Although there are many methods to prepare curing
Molybdenum, but the molybdenum disulfide of these methods preparation is all rendered as laminated structure substantially, and these laminated structures are in the synthesis process,
It is easy to reunite, to lose the high-specific surface area of two-dimensional material and the feature of high activity.In addition, different application scene needs not
Material with pattern meets actual needs to greatest extent, is such as applied to molybdenum disulfide to prepare lithium ion battery negative material
When, if nanometer sheet stacks serious, this electrolyte be difficult to enter material internal to carry out ion exchange, while ion be also difficult into
Enter interlayer and carries out intercalation.These all illustrate, for molybdenum disulfide, studying it also has very wide space.
And in the prior art, it is found after being retrieved according to inventor, molybdenum disulfide is all concentrated substantially for the research of molybdenum disulfide
In the preparation of nanometer sheet, the report of other nanostructures is seldom related to.Only discovery Chinese patent CN104071846A is disclosed
A kind of preparation method of molybdenum disulfide nano line is raw material using sulphur powder and molybdenum oxide, two has been obtained after solid phase calcination
Molybdenum sulfide nano wire, and as can be seen that prepared molybdenum disulfide nano line mass is very poor from its attached drawing, containing more miscellaneous
Matter is only the preparation for realizing molybdenum disulfide nano.
Therefore, in order to expand the range of choice of molybdenum disulfide nano structure, realize that molybdenum disulfide nano material is answered in difference
It is showed with the optimal performance of occasion.The purpose of the present invention is to provide a kind of sides for preparing high quality molybdenum disulfide nano structure
Method is specifically to provide a kind of method of efficiently preparation high quality molybdenum disulfide nano line.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing high quality molybdenum disulfide nano structure, specifically, providing
A kind of method of efficient preparation high quality molybdenum disulfide nano line.
A kind of method of efficient preparation high quality molybdenum disulfide nano line, comprising the following steps:
Firstly, prepare suitable surfactant solution, be then added thereto again suitable structure directing agent be stirred it is mixed
It closes, obtains solution A；
Secondly, weighing suitable ammonium molybdate and thioacetamide is respectively molybdenum source and sulphur source, stirred in deionized water solution
It mixes uniformly, obtains solution B；
Again, solution A is slowly added dropwise into B solution, ibid, then suitable reducing agent hydrazine hydrate is added thereto；
Finally, after hydrazine hydrate is added completely into, adjustment oil bath pot temperature is to 100-120 DEG C, reaction time 10-24h, shuttle shape magnetic
The mixing speed of son is 20-60rpm, after reaction, is repeatedly centrifuged to reaction product and deionization washs.
Preferably, the surfactant refers to cetyl trimethylammonium bromide, Cetyltrimethylammonium bromide, ten
One or more of six alkyl trimethyl ammonium chlorides or dodecyl trimethyl ammonium bromide.
Preferably, the structure directing agent refers to amine substance, preferably ethylenediamine.
Preferably, the molar ratio of the molybdenum source and sulphur source is (0.01-0.05): (0.1-0.2).
Compared with prior art, the beneficial effect that the present invention obtains is:
The direction of growth, which is adjusted, using surfactant combination ethylenediamine has quickly generated two sulphur under the reduction of hydrazine hydrate
Change molybdenum nano wire, rather than general molybdenum disulfide nano sheet, this method is simple, and the molybdenum disulfide nano line of preparation has preferable
Dispersibility and higher quality, be a kind of novel preparation method, the range of choice of widened molybdenum disulfide nano structure is
Realize that the molybdenum disulfide performance application of different occasions is laid a good foundation.
Detailed description of the invention
Molybdenum disulfide nano line TEM photo prepared by Fig. 1 embodiment of the present invention 1；
Molybdenum disulfide nano line TEM photo prepared by Fig. 2 embodiment of the present invention 2；
Molybdenum disulfide nano line XRD spectra prepared by Fig. 3 embodiment of the present invention 1.
Specific embodiment
All reagents used in the present invention are all bought from Sinopharm Chemical Reagent Co., Ltd., and analysis is pure, are not needed
Additional purification directly uses.
A kind of method of efficient preparation high quality molybdenum disulfide nano line, comprising the following steps:
Firstly, prepare suitable surfactant solution, be then added thereto again suitable structure directing agent be stirred it is mixed
It closes, obtains solution A；
Secondly, weighing suitable ammonium molybdate and thioacetamide is respectively molybdenum source and sulphur source, stirred in deionized water solution
It mixes uniformly, obtains solution B；
Again, solution A is slowly added dropwise into B solution, ibid, then suitable reducing agent hydrazine hydrate is added thereto；
Finally, after hydrazine hydrate is added completely into, adjustment oil bath pot temperature is to 100-120 DEG C, reaction time 10-24h, shuttle shape magnetic
The mixing speed of son is 20-60rpm, after reaction, is repeatedly centrifuged to reaction product and deionization washs.
In order to make those skilled in the art that the contents of the present invention be more clearly understood, combined with specific embodiments below to this hair
It is bright to be described in detail.
Embodiment 1
By concentration to be added in the cetyl trimethylammonium bromide aqueous solution of 50mL in the ethylenediamine solution of 0.03mg/mL,
Magnetic agitation is carried out, solution A is obtained；Ammonium molybdate and thioacetamide stirring are weighed for the ratio of 0.01:0.1 in molar ratio again
It is scattered in deionized water, obtains solution B；After mixing by solution A and B, liquid-transfering gun is reused to delay into mixed solution
The slow hydrazine hydrate that 0.5mL is added dropwise, continues to stir (having to open logical draught cupboard herein), increases oil bath pot temperature later to 100
DEG C and react 12h, meanwhile, adjustment shuttle shape magneton revolving speed be 50rpm.After reaction, band reaction solution is cooled to room temperature, to production
Object is centrifuged, is washed.
Embodiment 2
By concentration to be added in the cetyl trimethylammonium bromide aqueous solution of 50mL in the ethylenediamine solution of 0.03mg/mL,
Magnetic agitation is carried out, solution A is obtained；Ammonium molybdate and thioacetamide stirring are weighed for the ratio of 0.05:0.2 in molar ratio again
It is scattered in deionized water, obtains solution B；After mixing by solution A and B, liquid-transfering gun is reused to delay into mixed solution
The slow hydrazine hydrate that 0.5mL is added dropwise, continues to stir (having to open logical draught cupboard herein), increases oil bath pot temperature later to 100
DEG C and react 20h, meanwhile, adjustment shuttle shape magneton revolving speed be 50rpm.After reaction, band reaction solution is cooled to room temperature, to production
Object is centrifuged, is washed.
Embodiment 3
By concentration to be added in the Cetyltrimethylammonium bromide aqueous solution of 50mL in the ethylenediamine solution of 0.03mg/mL,
Magnetic agitation is carried out, solution A is obtained；Ammonium molybdate and thioacetamide stirring are weighed for the ratio of 0.01:0.1 in molar ratio again
It is scattered in deionized water, obtains solution B；After mixing by solution A and B, liquid-transfering gun is reused to delay into mixed solution
The slow hydrazine hydrate that 0.5mL is added dropwise, continues to stir (having to open logical draught cupboard herein), increases oil bath pot temperature later to 100
DEG C and react 12h, meanwhile, adjustment shuttle shape magneton revolving speed be 50rpm.After reaction, band reaction solution is cooled to room temperature, to production
Object is centrifuged, is washed.
Embodiment 4
By concentration to be added in the cetyl trimethylammonium bromide aqueous solution of 50mL in the ethylenediamine solution of 0.03mg/mL,
Magnetic agitation is carried out, solution A is obtained；Ammonium molybdate and thioacetamide stirring are weighed for the ratio of 0.03:0.12 in molar ratio again
It is scattered in deionized water, obtains solution B；After mixing by solution A and B, liquid-transfering gun is reused to delay into mixed solution
The slow hydrazine hydrate that 0.5mL is added dropwise, continues to stir (having to open logical draught cupboard herein), increases oil bath pot temperature later to 110
DEG C and react 12h, meanwhile, adjustment shuttle shape magneton revolving speed be 50rpm.After reaction, band reaction solution is cooled to room temperature, to production
Object is centrifuged, is washed.
Embodiment 5
By concentration to be added in the cetyl trimethylammonium bromide aqueous solution of 50mL in the ethylenediamine solution of 0.03mg/mL,
Magnetic agitation is carried out, solution A is obtained；Ammonium molybdate and thioacetamide stirring are weighed for the ratio of 0.01:0.1 in molar ratio again
It is scattered in deionized water, obtains solution B；After mixing by solution A and B, liquid-transfering gun is reused to delay into mixed solution
The slow hydrazine hydrate that 0.5mL is added dropwise, continues to stir (having to open logical draught cupboard herein), increases oil bath pot temperature later to 100
DEG C and react 12h, meanwhile, adjustment shuttle shape magneton revolving speed be 30rpm.After reaction, band reaction solution is cooled to room temperature, to production
Object is centrifuged, is washed.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (5)
1. a kind of method of efficiently preparation high quality molybdenum disulfide nano line, it is characterised in that: the following steps are included:
Firstly, prepare suitable surfactant solution, be then added thereto again suitable structure directing agent be stirred it is mixed
It closes, obtains solution A；
Secondly, weighing suitable ammonium molybdate and thioacetamide is respectively molybdenum source and sulphur source, stirred in deionized water solution
It mixes uniformly, obtains solution B；
Again, solution A is slowly added dropwise into B solution, ibid, then suitable reducing agent hydrazine hydrate is added thereto；
Finally, after hydrazine hydrate is added completely into, adjustment oil bath pot temperature is to 100-120 DEG C, reaction time 10-24h, shuttle shape magnetic
The mixing speed of son is 20-60rpm, after reaction, is repeatedly centrifuged to reaction product and deionization washs.
2. a kind of method of efficiently preparation high quality molybdenum disulfide nano line according to claim 1, it is characterised in that: institute
It states surfactant and refers to cetyl trimethylammonium bromide, Cetyltrimethylammonium bromide, cetyl trimethyl chlorination
One or more of ammonium or dodecyl trimethyl ammonium bromide.
3. a kind of method of efficiently preparation high quality molybdenum disulfide nano line according to claim 1, it is characterised in that: institute
It states structure directing agent and refers to amine substance, preferably ethylenediamine.
4. a kind of method of efficiently preparation high quality molybdenum disulfide nano line according to claim 1, it is characterised in that: institute
The molar ratio for stating molybdenum source and sulphur source is (0.01-0.05): (0.1-0.2).
5. molybdenum disulfide nano line according to claim 1, it is characterised in that: the diameter of nano wire is 20-50nm, length
It is 0.5-1.5 μm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109850947A (en) * | 2019-03-22 | 2019-06-07 | 合肥学院 | A kind of method that 12 hetropoly acid ammonium prepares molybdenum disulfide particle |
| CN111501061A (en) * | 2020-04-24 | 2020-08-07 | 唐友莲 | Nano Ni2P-MoS2Electrocatalytic hydrogen production material modified with graphene and preparation method thereof |
| CN114573027A (en) * | 2022-03-09 | 2022-06-03 | 北方民族大学 | Vanadium pentoxide nanobelt and preparation method thereof |
| CN116216780A (en) * | 2023-03-01 | 2023-06-06 | 淮北师范大学 | Broken shell-shaped MoS 2 Nanosphere material and preparation method and application thereof |
-
2018
- 2018-12-19 CN CN201811559699.XA patent/CN109437307A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109850947A (en) * | 2019-03-22 | 2019-06-07 | 合肥学院 | A kind of method that 12 hetropoly acid ammonium prepares molybdenum disulfide particle |
| CN109850947B (en) * | 2019-03-22 | 2021-09-21 | 合肥学院 | Method for preparing molybdenum disulfide particles from ammonium dodecamolybdenum phosphapolyate |
| CN111501061A (en) * | 2020-04-24 | 2020-08-07 | 唐友莲 | Nano Ni2P-MoS2Electrocatalytic hydrogen production material modified with graphene and preparation method thereof |
| CN114573027A (en) * | 2022-03-09 | 2022-06-03 | 北方民族大学 | Vanadium pentoxide nanobelt and preparation method thereof |
| CN114573027B (en) * | 2022-03-09 | 2023-08-18 | 北方民族大学 | Vanadium pentoxide nanobelt and preparation method thereof |
| CN116216780A (en) * | 2023-03-01 | 2023-06-06 | 淮北师范大学 | Broken shell-shaped MoS 2 Nanosphere material and preparation method and application thereof |
| CN116216780B (en) * | 2023-03-01 | 2024-04-26 | 淮北师范大学 | Broken shell-shaped MoS2Nanosphere material and preparation method and application thereof |
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Application publication date: 20190308 |