CN115465895A - Hydrothermal method for preparing pure-phase 1T-MoS 2 Method (2) - Google Patents
Hydrothermal method for preparing pure-phase 1T-MoS 2 Method (2) Download PDFInfo
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- CN115465895A CN115465895A CN202211157292.0A CN202211157292A CN115465895A CN 115465895 A CN115465895 A CN 115465895A CN 202211157292 A CN202211157292 A CN 202211157292A CN 115465895 A CN115465895 A CN 115465895A
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Abstract
The invention discloses a hydrothermal method for preparing pure-phase 1T-MoS 2 The method comprises the following steps: s1: 0.235g of Na was taken 2 MoO 4 ·2H 2 O, 3.12g of CH 4 N 2 S and 0.1g of PEG600-PEG10000 are dissolved by 60mL of deionized water; s2: standing for 100 minutes, and magnetically stirring for 30 minutes to obtain a mixed solution; s3: heating the mixed solution to 160-200 ℃ in a reaction kettle, maintaining the temperature 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. The invention has mild reaction conditions: the reaction is stable at 160-200 ℃, the reaction time is within 24h, and the conditions are mild; the requirement on equipment is low: the ordinary air-blast drying oven is the preparation equipment of the test. Simple and low-cost: the hydrothermal method is adopted to prepare stable 1T-MoS in the experiment 2 Without taking more experimental constraints, thereforeSimple and low 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 The method of (1).
Background
Transition metal sulfide MoS 2 As a typical graphene-like laminated two-dimensional material, the graphene-like laminated two-dimensional material has a very wide application prospect in the fields of photoelectrons, photonics, catalysts, energy conversion, storage and the like.
MoS 2 Exhibits unique physicochemical properties, based on the difference in the coordination and stacking manner of S-Mo-S among the single layers, moS 2 Different phases exist and are out of phaseMoS 2 The electrochemical performance showed a significant difference between them.
In nature, moS 2 In the 2H phase, the monolayer consists of three layers of S-Mo-S atoms, two of which are arranged symmetrically, and the Mo atom is centered in the triangular prism formed by the S atoms and coordinated to the surrounding six S atoms.
Unlike the conventional semiconductor phase MoS 2 ，1T-MoS 2 Exhibits a metal-like conductivity and is therefore also referred to as metal phase MoS 2 The monolayer thereof is composed of three S-Mo-S atoms, with Mo sandwiched between the two 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 obtained by rotating one layer of S atoms by 60 ° around the center of the top surface on the basis of the triangular prism structure in the 2H phase.
Thus, in 1T-MoS 2 The central Mo atom is octahedral coordinated with six surrounding S atoms. Because of the special coordination structure between Mo and S, 1T-MoS 2 Having a difference from 2H-MoS 2 The electrochemical performance of (2). 1T-MoS 2 The 1T-MoS is enabled by the fact that the basal surface has considerable catalytic activity, excellent conductivity and more abundant active sites 2 Becomes compared with 2H-MoS 2 More ideal catalytic materials.
Although 1T-MoS 2 The special properties of (A) make it show obvious advantages in the field of electrocatalysis, but because of the special coordination structure and energy band structure, the free energy of the catalyst is obviously higher than that of 2H-MoS 2 Therefore, the stability is poor, and the method belongs to a metastable phase. External factors such as temperature induce a change in the coordination structure of Mo-S, thereby converting the 1T phase into the 2H phase. Thus 1T-MoS 2 Does not exist in 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 adopts hydrothermal method to prepare 2H-MoS 2 Nanosheets, and then subjecting the multilayer 2H-MoS to ultrasonic-assisted lithium ion intercalation 2 Stripping the nano sheet to obtain the porous single-layer 1T-MoS 2 Nanosheets. CN112316959A molybdate and potassium carbonate were supported by impregnationOn silicon-based materials, in H 2 /H 2 Vulcanizing in S mixed atmosphere to obtain K insertion type 1T-MoS 2 。
Wang et al (NH) 4 )6Mo 7 O 24 ·4H 2 O is molybdenum source and NH 2 CSNH 2 Hydrothermal synthesis of 1T-MoS in 9T magnetic field as sulfur source 2 Nanosheets. Synthesis of MoS by direct hydrothermal method 2 There have been many attempts, but in most cases, 2H-MoS was obtained 2 @1T-MoS 2 A hetero-phase material.
MoS 2 There are many crystal forms of the metal 1T and the semiconductors 2H and 3R. This is due to the different possible arrangements of the S and Mo atoms in their crystal structures. This feature allows molybdenum disulfide to have adjustable structural and electronic properties, and 2H-MoS of semiconductors 2 Different, 1T phase MoS 2 (1T-MoS 2 ) Has metallic property, and the electronic conductivity is 105 times higher. In addition, the 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 many difficulties in the preparation and application of the compound:
(1) Conventional preparation of 1T-MoS 2 The method requires extremely harsh synthesis conditions;
(2)1T-MoS 2 poor phase stability and easy generation of 2H-MoS 2 The transformation of (3);
therefore, a hydrothermal method is provided 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 hydrothermal method for preparing pure-phase 1T-MoS 2 To solve the problems set forth in the background art described above.
In order to achieve the purpose, the invention provides the following technical scheme: hydrothermal method for preparing pure-phase 1T-MoS 2 The method comprises the following steps:
s1: 0.235g of Na was taken 2 MoO 4 ·2H 2 O, 3.12g CH 4 N 2 S and 0.1g of PEG600-PEG10000 are dissolved by 60mL of deionized water;
Na 2 MoO 4 ·2H 2 O、CH 4 N 2 s and PEG600-PEG10000 are sequentially added into a dissolving bottle, and then 60mL of deionized water is poured along the bottle wall of the dissolving bottle;
s2: standing for 100 minutes, and magnetically stirring for 30 minutes to obtain a mixed solution;
s3: heating the mixed solution to 160-200 ℃ in a reaction kettle, maintaining the temperature for 24 hours, and precipitating and filtering to obtain 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.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a hydrothermal method for preparing pure-phase 1T-MoS 2 The method has mild reaction conditions: the reaction is stable at 160-200 ℃, the reaction time is within 24h, and the conditions are mild; the requirement on equipment is low: the ordinary air-blast drying oven is the preparation equipment of the test. Simple and low-cost: the hydrothermal method is adopted to prepare stable 1T-MoS in the experiment 2 And more test limiting conditions are not needed, so that the method is simple and low in cost.
Drawings
FIG. 1 is a schematic Raman spectrum of the present invention;
FIG. 2 shows an unstripped 2H-MoS 2 Nanosheets and exfoliated porous 1T-MoS 2 A Raman spectrogram schematic diagram of the nanosheet;
figure 3 is XRD characterization information for the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1: the invention provides a hydrothermal method for preparing pure phase 1T-MoS as shown in figures 1-3 2 The method comprises the following steps:
s1: 0.235g of Na was taken 2 MoO 4 ·2H 2 O, 3.12g of CH 4 N 2 S and 0.1g of PEG600-PEG10000 are dissolved by 60mL of deionized water;
s2: standing for 100 minutes, and magnetically stirring for 30 minutes to obtain a mixed solution;
s3: heating the mixed solution to 160-200 ℃ in a reaction kettle, maintaining the temperature 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 60 ℃ forced air drying cabinet for 12h.
In the step S1, na 2 MoO 4 ·2H 2 O、CH 4 N 2 S and PEG600-PEG10000 are sequentially added into a dissolving bottle, and then 60mL of deionized water is poured along the bottle wall of the dissolving bottle.
The heating temperature in the step S3 is 180 ℃.
In the step S3, after the heating is completed, a black powder sample is obtained by precipitation and filtration.
In conclusion, compared with the prior art, the reaction conditions of the invention are mild: the reaction is stable at 160-200 ℃, the reaction time is within 24h, and the conditions are mild; the requirement on equipment is low: the ordinary air-blast drying oven is the preparation equipment of the test. Simple and low-cost: the hydrothermal method is adopted in the experiment to prepare stable 1T-MoS 2 And more test limiting conditions are not needed, so that the method is simple and low in cost.
Finally, it should be noted that: 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 or portions thereof without departing from the spirit and scope of the invention.
Claims (4)
1. Hydrothermal method for preparing pure-phase 1T-MoS 2 The method of (2), characterized by: the method comprises the following steps:
s1: 0.235g of Na was taken 2 MoO 4 ·2H 2 O, 3.12g of CH 4 N 2 S and 0.1g of PEG600-PEG10000 are dissolved by 60mL of deionized water;
s2: standing for 100 minutes, and magnetically stirring for 30 minutes to obtain a mixed solution;
s3: heating the mixed solution to 160-200 ℃ in a reaction kettle, maintaining the temperature 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. The hydrothermal process of claim 1, wherein the hydrothermal process produces phase-pure 1T-MoS 2 The method is characterized in that: in the step S1, na 2 MoO 4 ·2H 2 O、CH 4 N 2 S and PEG600-PEG10000 are sequentially put into a dissolving bottle, and then 60mL of deionized water is poured along the bottle wall of the dissolving bottle.
3. The hydrothermal process of claim 1, wherein the hydrothermal process produces pure-phase 1T-MoS 2 The method of (2), characterized by: the heating temperature in the step S3 is 180 ℃.
4. The hydrothermal process of claim 1, wherein the hydrothermal process produces phase-pure 1T-MoS 2 The method of (2), characterized by: in the step S3, after the heating is completed, a black powder sample is obtained by precipitation and filtration.
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| CN202211157292.0A CN115465895B (en) | 2022-09-22 | 2022-09-22 | Preparation of pure phase 1T-MoS by hydrothermal method 2 Is a method of (2) |
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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 |
|---|
| WANG SHIQUAN ET AL.: "Hydrothermal Synthesis of Molybdenum Disulfide for Lithium Ion Battery Applications", CHINESE JOURNAL OF CHEMICAL ENGINEERING * |
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