CN115465895B - Preparation of pure phase 1T-MoS by hydrothermal method 2 Is a method of (2) - Google Patents
Preparation of pure phase 1T-MoS by hydrothermal method 2 Is a method of (2) Download PDFInfo
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- CN115465895B CN115465895B CN202211157292.0A CN202211157292A CN115465895B CN 115465895 B CN115465895 B CN 115465895B CN 202211157292 A CN202211157292 A CN 202211157292A CN 115465895 B CN115465895 B CN 115465895B
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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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- 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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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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Abstract
The invention discloses a hydrothermal method for preparing pure phase 1T-MoS 2 Comprises the following steps: s1: 0.235g of Na is taken 2 MoO 4 ·2H 2 O, 3.12g of CH 4 N 2 S and 0.1g of PEG600-PEG10000, dissolving with 60mL deionized water; s2: standing for 100 minutes, and magnetically stirring for 30 minutes to obtain a mixed solution; s3: placing the mixed solution into a reaction kettle, heating to 160-200 ℃, maintaining for 24 hours, and obtaining a black powder sample after heating is completed; s4: the black powder samples were washed several times with ethanol and deionized water and then dried in a forced air oven at 60 ℃ for 12h. The reaction condition of the invention is mild: the reaction is stable at 160-200 ℃, the reaction time is within 24 hours, and the conditions are mild; the requirements on equipment are low: the common blast drying box is the preparation equipment for the test. Simple low cost: the test adopts a hydrothermal method to prepare stable 1T-MoS 2 No more test limiting conditions need to be adopted, so the method is simple and low in cost.
Description
Technical Field
The invention belongs to 1T-MoS 2 The technical field of materials, in particular to a hydrothermal method for preparing pure phase 1T-MoS 2 Is a method of (2).
Background
Transition metal sulfide MoS 2 As a typical graphene-like layered two-dimensional material, the material has very broad application prospects in the fields of photoelectrons, photonics, catalysts, energy conversion, storage and the like.
MoS 2 Exhibits unique physicochemical properties based on different S-Mo-S coordination and stacking modes between single layers, moS 2 Different phases exist and MoS of different phases 2 The electrochemical properties showed a significant difference between them.
In nature, moS 2 In the presence of 2H phase, the monolayer is composed of three layers of S-Mo-S atoms, wherein two layers of S atoms are symmetrically arranged, and Mo atoms are positioned in the center of a triangular prism formed by the S atoms and coordinate with six surrounding S atoms.
Unlike the common semiconductor phase MoS 2 ，1T-MoS 2 Exhibits conductivity similar to metals, and is therefore also known as metal phase MoS 2 The monolayer is composed of three layers of S-Mo-S atoms, with Mo sandwiched between the two layers of S atoms. However, unlike the 2H phase, in the 1T phase, two layers of S atoms are asymmetrically arranged, and the structure thereof can be described as being based on a triangular prism structure in the 2H phase, in which one layer of S atoms is rotated by 60 ° with the center of the top surface as the rotation center.
Thus, in 1T-MoS 2 The Mo atom and the surrounding six S atoms are in octahedral coordination. Because of the special coordination structure between Mo and S, 1T-MoS 2 With a difference from 2H-MoS 2 Is used for the electrochemical performance of the battery. 1T-MoS 2 The basal plane has considerable catalytic activity, excellent electric conduction capability and richer active sites, so that 1T-MoS 2 Becomes compared with 2H-MoS 2 More ideal catalytic material.
Although 1T-MoS 2 The special properties of (C) lead the catalyst to show obvious advantages in the field of electrocatalysis, but the free energy is obviously higher than that of 2H-MoS due to the special coordination structure and energy band structure 2 Therefore, the stability is poor, and the metastable phase is included. External factors such as temperature induce a change in coordination structure between Mo and S, thereby converting the 1T phase to the 2H phase. Thus 1T-MoS 2 Is not existed in the nature and needs to be prepared manually.
Reported 1T-MoS 2 The preparation method of the nano-sheet comprises the following steps: (1) chemical stripping; (2) magnetic field hydrothermal method. CN106311282B preparation of 2H-MoS by hydrothermal method 2 Nano sheet, then using ultrasonic auxiliary lithium ion intercalation method to make multi-layer 2H-MoS 2 Stripping the nano sheet to obtain a porous single-layer 1T-MoS 2 A nano-sheet. CN112316959A is prepared by loading molybdate and potassium carbonate on silicon-based material by impregnation method, and adding hydrogen sulfide 2 /H 2 Vulcanizing under S mixed atmosphere to obtain K insertion type 1T-MoS 2 。
X.Wang et al (NH) 4 )6Mo 7 O 24 ·4H 2 O is a molybdenum source, NH 2 CSNH 2 Hydrothermal synthesis of 1T-MoS as sulfur source in 9T magnetic field 2 A nano-sheet. Synthesis of MoS by direct hydrothermal method 2 In many cases, 2H-MoS is obtained 2 @1T-MoS 2 And (3) a heterogeneous material.
MoS 2 There are multiple crystalline forms of metal 1T and semiconductors 2H and 3R. This is due to the possible arrangement of S and Mo atoms in their crystal structure. This feature allows for adjustable structural and electronic characteristics of molybdenum disulfide, in combination with semiconductor 2H-MoS 2 Different from1T phase MoS 2 (1T-MoS 2 ) Has metallic property and electronic conductivity higher than 105 times. In addition, distorted octahedral coordination increases the interlayer spacing of the 1T phase, resulting in a decrease in the sodium ion diffusion barrier. However, 1T-MoS 2 There are a number of difficulties in the preparation and use of (a):
(1) Traditional preparation of 1T-MoS 2 The method requires extremely severe synthesis conditions;
(2)1T-MoS 2 poor phase stability and easy occurrence of 2H-MoS 2 Is transformed by (a);
for this reason, we propose a hydrothermal method for preparing pure phase 1T-MoS 2 To solve the problems mentioned in the background art.
Disclosure of Invention
The invention aims to provide a method for preparing pure-phase 1T-MoS by a hydrothermal method 2 To solve the problems set forth in the background art.
In order to achieve the above purpose, the present invention provides the following technical solutions: preparation of pure phase 1T-MoS by hydrothermal method 2 Comprises the following steps:
s1: 0.235g of Na is taken 2 MoO 4 ·2H 2 O, 3.12g of CH 4 N 2 S and 0.1g of PEG600-PEG10000, dissolving with 60mL deionized water;
Na 2 MoO 4 ·2H 2 O、CH 4 N 2 s and PEG600-PEG10000 are firstly sequentially put into a dissolving bottle, and then 60mL of deionized water is poured along the wall of the dissolving bottle;
s2: standing for 100 minutes, and magnetically stirring for 30 minutes to obtain a mixed solution;
s3: placing the mixed solution into a reaction kettle, heating to 160-200 ℃, maintaining for 24 hours, and obtaining a black powder sample after the heating is completed and precipitation and filtration are carried out;
s4: the black powder samples were washed several times with ethanol and deionized water and then dried in a forced air oven at 60 ℃ for 12h.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a method for preparing pure phase 1T-MoS by a hydrothermal method 2 The reaction condition of the method is mild: the reaction is stable at 160-200 ℃, the reaction time is within 24 hours, and the conditions are mild; the requirements on equipment are low: the common blast drying box is the preparation equipment for the test. Simple low cost: the test adopts a hydrothermal method to prepare stable 1T-MoS 2 No more test limiting conditions need to be adopted, so the method is simple and low in cost.
Drawings
FIG. 1 is a schematic diagram of a Raman spectrum of the present invention;
FIG. 2 is an unpeeled 2H-MoS 2 Nanoplatelets and peeled porous 1T-MoS 2 A schematic of raman spectra of the nanoplatelets;
figure 3 is XRD characterization information of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1: the invention provides a hydrothermal method for preparing pure phase 1T-MoS as shown in figures 1-3 2 Comprises the following steps:
s1: 0.235g of Na is taken 2 MoO 4 ·2H 2 O, 3.12g of CH 4 N 2 S and 0.1g of PEG600-PEG10000, dissolving with 60mL deionized water;
s2: standing for 100 minutes, and magnetically stirring for 30 minutes to obtain a mixed solution;
s3: placing the mixed solution into a reaction kettle, heating to 160-200 ℃, maintaining for 24 hours, and obtaining a black powder sample after heating is completed;
s4: the black powder samples were washed several times with ethanol and deionized water and then dried in a forced air oven at 60 ℃ for 12h.
In the step S1, na 2 MoO 4 ·2H 2 O、CH 4 N 2 S andPEG600-PEG10000 was added sequentially to the dissolution bottle and then 60mL of deionized water was poured along the wall of the dissolution bottle.
The heating temperature in the step S3 is 180 ℃.
In the step S3, after heating, a black powder sample is obtained by precipitation and filtration.
In conclusion, compared with the prior art, the method has the advantages that the reaction conditions are mild: the reaction is stable at 160-200 ℃, the reaction time is within 24 hours, and the conditions are mild; the requirements on equipment are low: the common blast drying box is the preparation equipment for the test. Simple low cost: the test adopts a hydrothermal method to prepare stable 1T-MoS 2 No more test limiting conditions need to be adopted, so the method is simple and low in cost.
Finally, it should be noted that: the foregoing description is only illustrative of the preferred embodiments of the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements or changes may be made without departing from the spirit and principles of the present invention.
Claims (4)
1. Preparation of pure phase 1T-MoS by hydrothermal method 2 Is characterized in that: the method comprises the following steps:
s1: 0.235g of Na is taken 2 MoO 4 ·2H 2 O, 3.12g of CH 4 N 2 S and 0.1g of PEG10000, dissolving with 60mL deionized water;
s2: standing for 100 minutes, and magnetically stirring for 30 minutes to obtain a mixed solution;
s3: placing the mixed solution into a reaction kettle, heating to 160-180 ℃, maintaining for 24 hours, and obtaining a black powder sample after heating;
s4: the black powder samples were washed several times with ethanol and deionized water and then dried in a forced air oven at 60 ℃ for 12h.
2. A method for preparing pure phase 1T-MoS by hydrothermal method according to claim 1 2 Is characterized in that: in the step S1, na 2 MoO 4 ·2H 2 O、CH 4 N 2 S and PEG10000 are firstly put into a dissolving bottle in sequence, and then 60mL of deionized water is poured along the wall of the dissolving bottle.
3. A method for preparing pure phase 1T-MoS by hydrothermal method according to claim 1 2 Is characterized in that: the heating temperature in the step S3 is 180 ℃.
4. A method for preparing pure phase 1T-MoS by hydrothermal method according to claim 1 2 Is characterized in that: in the step S3, after heating, a black powder sample is obtained by precipitation and filtration.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241878A (en) * | 2016-08-22 | 2016-12-21 | 河南师范大学 | A kind of preparation method of 1T phase monolayer molybdenum disulfide nano sheet |
| CN106311282A (en) * | 2016-08-09 | 2017-01-11 | 河南工程学院 | Preparing method of porous monocrystal IT MoS2 nanosheet and application thereof |
| CN106477631A (en) * | 2016-10-11 | 2017-03-08 | 郑州大学 | A kind of method realizing molybdenum bisuphide 2H to 1T phase in version |
| CN112225252A (en) * | 2020-10-23 | 2021-01-15 | 青岛大学 | Multi-morphology micro-nano MoS2Preparation method of (1) |
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- 2022-09-22 CN CN202211157292.0A patent/CN115465895B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106311282A (en) * | 2016-08-09 | 2017-01-11 | 河南工程学院 | Preparing method of porous monocrystal IT MoS2 nanosheet and application thereof |
| CN106241878A (en) * | 2016-08-22 | 2016-12-21 | 河南师范大学 | A kind of preparation method of 1T phase monolayer molybdenum disulfide nano sheet |
| CN106477631A (en) * | 2016-10-11 | 2017-03-08 | 郑州大学 | A kind of method realizing molybdenum bisuphide 2H to 1T phase in version |
| CN112225252A (en) * | 2020-10-23 | 2021-01-15 | 青岛大学 | Multi-morphology micro-nano MoS2Preparation method of (1) |
Non-Patent Citations (1)
| Title |
|---|
| Hydrothermal Synthesis of Molybdenum Disulfide for Lithium Ion Battery Applications;WANG Shiquan et al.;Chinese Journal of Chemical Engineering * |
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