CN103693693A - Preparation method for synthesizing molybdenum sulfide nanospheres by microwave-assisted liquid phase deposition - Google Patents
Preparation method for synthesizing molybdenum sulfide nanospheres by microwave-assisted liquid phase deposition Download PDFInfo
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Abstract
The invention discloses a preparation method for synthesizing molybdenum sulfide nanospheres by microwave-assisted liquid phase deposition, and belongs to the technical field of inorganic micro-nano materials. The method comprises the following steps: dissolving a certain amount of ammonium thiomolybdate in de-ionized water while stirring to form a clear solution, adding a reducer-hydrazine while stirring, stirring until the reducer is completely dissolved, transferring a reaction system to a glass round-bottom flask, performing microwave heating in a microwave furnace for a certain time under reflux conditions, naturally cooling to room temperature, rinsing obtained deposits by the de-ionized water and absolute ethanol respectively, performing centrifugal separation, and drying in a drying box to obtain amorphous molybdenum sulfide nanospheres. The synthetic method has the advantages of simple process, low cost, quickness, high efficiency, uniform product shape and size, high synthetic amount and high yield; the molybdenum sulfide nanospheres synthesized by the method are uniform in size, have the average diameter of 100 nm to 270 nm, and are expected to be widely applied in the fields of lithium ion battery electrode materials, photoelectric catalysts, solid lubricants and the like.
Description
Technical field
The present invention relates to a kind of preparation of micro Nano material, relate in particular to the preparation method of the synthetic moly-sulfide nanometer ball of a kind of microwave-assisted liquid phase, belong to inorganic technical field of micro nano material preparation.
Background technology
Molybdenumdisulphide (MoS
2) be typical stratiform transient metal sulfide, because its widespread use in fields such as hydrogenation catalyst, photoelectrocatalysis hydrogen production by water decomposition, solid lubricant and lithium ion batteries receives much concern.While MoS
2or a kind of diamagnetism and there is the compound of semiconductor property, its energy gap is 1.78eV, visible light absorbing, thereby be widely used aspect photoelectric material.The nano level MoS of different-shape
2demonstrate some unique performances, therefore there is the MoS of special appearance
2preparation receive investigator's very big concern.At present, nano level MoS
2the chemical preparation process of material has many kinds, is mainly divided into solid phase method and liquid phase method.Wherein solid phase method comprises thermal decomposition method (O. C. Monteiro, Materials Research Bulletin, 2004, 357), chemical Vapor deposition process (X. L. Li, Chemistry A European Journal, 2004, 6163), template (C. M. Zelenski, Journal of The American Chemical Society, 1998, 734), induced with laser synthesis method (E. Borsella, Journal of Materials Science Letters, 2001. 187) and Microwave Induced Plasma vapour deposition process (D. J. Brooks, Nanotechnolgy, 2006, 1245) etc., and liquid phase method comprises the hot method of hydrothermal/solvent (X. L. Li, The Journal of Physical Chemistry B, 2004,13893, S. J. Ding, Nanoscale, 2012,95, N. Berntsen, Chemistry of Materials, 2003,4498), sonochemical method (I. Uzcanga, Chemistry of Materials, 2005,2575), electrochemical process (Q. Li, The Journal of Physical Chemistry B, 2005,3169), sol-gel method (N. Li, Materials Letters, 2012,112) etc.Its pattern is mainly the richness of zero-dimension structural and strangles rare nanostructure (N. Sano, Chemical Physics Letters, 2003,331), nanometer ball (Y. M. Tian, Materials Letters, 2006,527; S. K. Park, CrystEngComm, 2012,8323); The nanotube of one-dimentional structure (J. Chen; Journal of The American Chemical Society; 2001,11813), nano wire (Q. Li, The Journal of Physical Chemistry B; 2005; 31694,45, nanometer rod (X. W. Zheng, Ultrasonics Sonochemistry; 2004,83); Nanometer plate (C. F. Castro-Guerrero, Catalysis Science & Technology, 2011 of the structure of two dimension, 1024), nano flake (X. L. Li, The Journal of Physical Chemistry B, 2004,13893); And the multi-level nano-structure (S. J. Ding, Nanoscale, 2012,95 that by nanometer sheet, are formed three-dimensional structure; L. N. Ye, Chemistry of Materials, 2007,6331).
But in above preparation method otherwise need higher temperature of reaction and longer reaction times (as hydro-thermal or solvent thermal temperature more than 180 ℃, general 24 hours of reaction times; As thermolysis or chemical vapour deposition need more than 800 ℃, approximately several hours reaction times).As a kind of quick, even, energy-conservation and heating means that efficiency is high, carry out microwave radiation heating technology is widely applied in synthetic in organic chemical synthesis and material.Microwave heating technique has been successfully used to the synthetic of the nano materials such as metal nano material, metal oxide nano-material and metallic sulfide.But up to the present, by the method for the amorphous sulfuration molybdenum nanometer ball of the synthetic pattern of the quick liquid phase of carry out microwave radiation heating technology and size uniform, yet there are no open report.
Summary of the invention
The object of the present invention is to provide the preparation method of the synthetic moly-sulfide nanometer ball of a kind of microwave-assisted liquid phase, the method can be under lower temperature condition, adopt raw material and simple process cheap and easy to get, the synthetic pattern of rapid, high volume and the comparatively uniform amorphous sulfuration molybdenum nanometer ball of size.
The preparation method of the synthetic moly-sulfide nanometer ball of a kind of microwave-assisted liquid phase provided by the invention, the method is carried out as follows:
1) ammonium thiomolybdate is under agitation dissolved in deionized water and forms settled solution, the volumetric molar concentration of ammonium thiomolybdate is 0.01～0.05mol/L;
2) under agitation add hydrazine (having another name called hydrazine hydrate) (as reductive agent), the consumption of hydrazine is 7.0～10.0ml hydrazine/every 1mmol ammonium thiomolybdate;
3) reaction system step 2 being obtained is transferred in glass round-bottomed flask, under reflux conditions microwave heating 15～45 minutes in microwave oven, then naturally cooling, fully washs rear collection and dryly obtains amorphous sulfuration molybdenum nanometer ball with centrifugation and deionized water.
In preparation process of the present invention, adopting ammonium thiomolybdate is He Liu source, molybdenum source; Adopt hydrazine as reductive agent.
The present invention regulates the size of amorphous sulfuration molybdenum nanometer ball by changing ammonium thiomolybdate concentration or microwave heating time.
Beneficial effect of the present invention is:
1. have that preparation technology is simple, with low cost, product pattern and size uniform, can synthesize in a large number and advantage that product yield is high;
2. the amorphous sulfuration molybdenum nanometer ball mean diameter of preparing is between 100nm～270nm;
3. this product is expected to obtain in fields such as lithium ion battery electrode material, photoelectrocatalysis agent and solid lubricants application widely.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of the amorphous sulfuration molybdenum nanometer ball that makes of present method;
Fig. 2 is scanning electron microscope (a) and the transmission electron microscope picture (b) of the amorphous sulfuration molybdenum nanometer ball that makes of present method;
Fig. 3 is the scanning electron microscope (SEM) photograph of the amorphous sulfuration molybdenum nanometer ball that makes of present method.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail, these embodiment are only used for illustrating the present invention, do not limit the scope of the invention.
Embodiment 1
1.5mmol ammonium thiomolybdate is under agitation dissolved in deionized water and forms settled solution, and the volumetric molar concentration of ammonium thiomolybdate is 0.025mol/L; Under agitation add 10ml hydrazine as reductive agent, this reaction system is transferred in 100ml glass round-bottomed flask, under reflux conditions in microwave oven with 80% peak power microwave heating 30 minutes, then naturally cooling, fully washs rear collection and dryly obtains amorphous sulfuration molybdenum nanometer ball with centrifugation and deionized water.The X-ray diffractogram of moly-sulfide product is shown in Fig. 1, only occurs (002) and (100) diffraction peak in figure, therefore can find out that moly-sulfide is amorphous products.Its scanning electron microscope (SEM) photograph and transmission electron microscope picture are shown in respectively Fig. 2 a and 2b, show that moly-sulfide product is size pattern nanometer ball comparatively uniformly, mean diameter 161nm.
Embodiment 2
1.5mmol ammonium thiomolybdate is under agitation dissolved in deionized water and forms settled solution, and the volumetric molar concentration of ammonium thiomolybdate is 0.025mol/L; Under agitation add 10ml hydrazine as reductive agent, this reaction system is transferred in 100ml glass round-bottomed flask, under reflux conditions in microwave oven with 80% peak power microwave heating 45 minutes, then naturally cooling, fully washs rear collection and dryly obtains amorphous sulfuration molybdenum nanometer ball with centrifugation and deionized water.The scanning electron microscope (SEM) photograph of moly-sulfide product is shown in Fig. 3, shows that moly-sulfide product is size pattern nanometer ball comparatively uniformly, mean diameter 193nm.
Embodiment 3
0.6mmol ammonium thiomolybdate is under agitation dissolved in deionized water and forms settled solution, and the volumetric molar concentration of ammonium thiomolybdate is 0.01mol/L; Under agitation add 5ml hydrazine as reductive agent, this reaction system is transferred in 100ml glass round-bottomed flask, under reflux conditions in microwave oven with 80% peak power microwave heating 30 minutes, then naturally cooling, fully washs rear collection and dryly obtains amorphous sulfuration molybdenum nanometer ball with centrifugation and deionized water.The mean diameter 118nm of moly-sulfide product.
Embodiment 4
3mmol ammonium thiomolybdate is under agitation dissolved in deionized water and forms settled solution, and the volumetric molar concentration of ammonium thiomolybdate is 0.05mol/L; Under agitation add 15ml hydrazine as reductive agent, this reaction system is transferred in 100ml glass round-bottomed flask, under reflux conditions in microwave oven with 80% peak power microwave heating 30 minutes, then naturally cooling, fully washs rear collection and dryly obtains amorphous sulfuration molybdenum nanometer ball with centrifugation and deionized water.The mean diameter 247nm of moly-sulfide product.
Claims (4)
1. a preparation method for the synthetic moly-sulfide nanometer ball of microwave-assisted liquid phase, is characterized in that: the method comprises the steps:
1) ammonium thiomolybdate is under agitation dissolved in deionized water and forms settled solution, the volumetric molar concentration of ammonium thiomolybdate is 0.01～0.05mol/L;
2) under agitation add hydrazine, have another name called hydrazine hydrate, the consumption of hydrazine is 7.0～10.0ml hydrazine/every 1mmol ammonium thiomolybdate;
3) reaction system step 2 being obtained is transferred in glass round-bottomed flask, under reflux conditions microwave heating 15～45 minutes in microwave oven, then naturally cooling, fully washs rear collection and dryly obtains amorphous sulfuration molybdenum nanometer ball with centrifugation and deionized water.
2. the preparation method that a kind of microwave-assisted synthesizes moly-sulfide nanometer ball according to claim 1, is characterized in that: the method adopts carry out microwave radiation heating technology fast.
3. the preparation method that a kind of microwave-assisted synthesizes moly-sulfide nanometer ball according to claim 1, is characterized in that: in carry out microwave radiation heating, be equipped with reflux.
4. the preparation method that a kind of microwave-assisted synthesizes moly-sulfide nanometer ball according to claim 1, is characterized in that: it is molybdenum source that the method is used ammonium thiomolybdate, take hydrazine as reductive agent.
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| CN104953119A (en) * | 2015-06-08 | 2015-09-30 | 陕西科技大学 | Preparation method for two-dimensional matrix rod-like WS2 anode material |
| CN105399060A (en) * | 2015-09-28 | 2016-03-16 | 中国科学院重庆绿色智能技术研究院 | Method for rapid synthesis of two-dimensional layered nanometer material |
| CN105489387A (en) * | 2016-01-13 | 2016-04-13 | 宿州学院 | Nitrogen-doped carbon microsphere load MoS2 composite, preparing method and application thereof |
| CN106803589A (en) * | 2017-02-26 | 2017-06-06 | 桂林理工大学 | A kind of single dispersing class flower ball-shaped MoS2Raw powder's production technology |
| CN106986387A (en) * | 2017-06-02 | 2017-07-28 | 岭南师范学院 | A kind of three-dimensional molybdenum disulfide bouquet and preparation method thereof |
| CN112028121A (en) * | 2020-09-28 | 2020-12-04 | 四川大学 | Preparation method of amorphous molybdenum disulfide nano material based on photocatalytic synthesis |
| CN114887631A (en) * | 2022-05-05 | 2022-08-12 | 中国石油大学(华东) | Solvothermal method for preparing mixed morphology 1T-2H MoS 2 Preparation method and application of |
| CN116062793A (en) * | 2023-02-08 | 2023-05-05 | 南京邮电大学 | Amorphous MoS x Nano-disk and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104953119A (en) * | 2015-06-08 | 2015-09-30 | 陕西科技大学 | Preparation method for two-dimensional matrix rod-like WS2 anode material |
| CN105399060A (en) * | 2015-09-28 | 2016-03-16 | 中国科学院重庆绿色智能技术研究院 | Method for rapid synthesis of two-dimensional layered nanometer material |
| CN105489387A (en) * | 2016-01-13 | 2016-04-13 | 宿州学院 | Nitrogen-doped carbon microsphere load MoS2 composite, preparing method and application thereof |
| CN105489387B (en) * | 2016-01-13 | 2018-07-17 | 宿州学院 | A kind of nitrating carbosphere load MoS2Compound, preparation method and application |
| CN106803589A (en) * | 2017-02-26 | 2017-06-06 | 桂林理工大学 | A kind of single dispersing class flower ball-shaped MoS2Raw powder's production technology |
| CN106803589B (en) * | 2017-02-26 | 2019-08-09 | 桂林理工大学 | A kind of monodisperse class flower ball-shaped MoS2Raw powder's production technology |
| CN106986387A (en) * | 2017-06-02 | 2017-07-28 | 岭南师范学院 | A kind of three-dimensional molybdenum disulfide bouquet and preparation method thereof |
| CN112028121A (en) * | 2020-09-28 | 2020-12-04 | 四川大学 | Preparation method of amorphous molybdenum disulfide nano material based on photocatalytic synthesis |
| CN112028121B (en) * | 2020-09-28 | 2021-08-03 | 四川大学 | Preparation method of amorphous molybdenum disulfide nano material based on photocatalytic synthesis |
| CN114887631A (en) * | 2022-05-05 | 2022-08-12 | 中国石油大学(华东) | Solvothermal method for preparing mixed morphology 1T-2H MoS 2 Preparation method and application of |
| CN114887631B (en) * | 2022-05-05 | 2023-08-18 | 中国石油大学(华东) | Solvothermal method for preparing mixed morphology 1T-2H MoS 2 Preparation method and application of (C) |
| CN116062793A (en) * | 2023-02-08 | 2023-05-05 | 南京邮电大学 | Amorphous MoS x Nano-disk and preparation method and application thereof |
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Application publication date: 20140402 |