CN109453791A - A kind of sulfur-bearing vacancy MoS2Nanometer sheet and preparation method thereof - Google Patents
A kind of sulfur-bearing vacancy MoS2Nanometer sheet and preparation method thereof Download PDFInfo
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- CN109453791A CN109453791A CN201811375638.8A CN201811375638A CN109453791A CN 109453791 A CN109453791 A CN 109453791A CN 201811375638 A CN201811375638 A CN 201811375638A CN 109453791 A CN109453791 A CN 109453791A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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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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Abstract
The present invention provides a kind of sulfur-bearing vacancy MoS2The preparation method of nanometer sheet, comprising the following steps: step 1:MoS2The synthesis of nanometer sheet presoma；Step 2: the presoma is subjected to nanosecond laser irradiation using laser liquid phase ablation；Step 3: the product of nanosecond laser irradiation is finally obtained into the sulphur vacancy MoS after freeze-drying2Nanometer sheet.Utilize the MoS in the method for the present invention Laser synthesizing sulfur-bearing vacancy2The method cleaning of nanometer sheet, quick, efficient, the advantage for having conventional method incomparable.
Description
Technical field
The present invention relates to technical field of image processing more particularly to a kind of sulfur-bearing vacancy MoS2Nanometer sheet and its preparation side
Method.
Background technique
Since fossil energy reserves are limited and its burning bring environmental pollution, cleaning, green Hydrogen Energy are considered as most
The substitute of ideal fossil energy.Have using the method for this green of electrolysis aquatic products hydrogen (HER), efficient conversion Hydrogen Energy non-
The application prospect of Chang Chong great.At present in the catalyst of HER, noble metal platinum based catalyst is had excellent catalytic properties, but by
In its application with high costs for limiting it in the industrial production.So non-precious metal catalyst especially molybdenum disulfide due to
In acidic electrolysis bath have preferable catalytic stability, earth's surface rich reserves and have received widespread attention.But curing at present
The problems such as molybdenum is low since there are catalytic activity, poorly conductive, HER performance is also difficult to compare favourably with noble metal catalyst.Therefore,
The catalytic performance for how promoting molybdenum disulfide becomes the hot spot of people's research.
Currently, introducing vacancy in the catalyst has become a kind of important method for improving catalyst performance.Have
Many work prove that after introducing vacancy, the adsorption energy of proton hydrogen can be effectively reduced in catalyst surface, while can increase substantially material
The electric conductivity of itself is expected, to effectively promote the catalytic capability of catalyst.However the existing side for introducing vacancy in the catalyst
Method depends on hydrogen reduction and active metal restoring method under high temperature and pressure mostly, considerably increase energy consumption in synthesis process and
Risk.In today that environment and energy problem are got worse, green, quick, height are increasingly tended to the synthetic method of catalyst
Effect, cleaning.Laser liquid phase ablation (LAL) is a kind of method of novel nano materials, has many advantages: (1) this
It is a kind of green, quickly synthesis nanostructure method, by-product is few, and presoma is simple, without using additional catalyst；
(2) it can be synthesized in room temperature condition, method is mild, greatly reduces risk and energy consumption in synthesis process；(3) due to swashing
Light can ablation material it is numerous, can be widely applied to synthesize a variety of nano materials.Laser can be in moment at ablator surface
High temperature and high pressure environment is formed, is then quenched to room temperature, this process is conducive to the synthesis and reservation in the vacancy of material surface.Therefore
Develop this green, efficient, controllable molybdenum chalcogenide of the method synthesis rich in vacancy of laser liquid phase ablation as efficient
HER catalyst have highly important Research Prospects and industrial application value.
Summary of the invention
It is an object of the invention to solve the problems of the above-mentioned prior art, a kind of sulfur-bearing vacancy MoS is provided2Nanometer sheet
And preparation method thereof.
A kind of sulfur-bearing vacancy MoS2The preparation method of nanometer sheet, comprising the following steps:
Step 1:MoS2The synthesis of nanometer sheet presoma；
Step 2: the presoma is subjected to nanosecond laser irradiation using laser liquid phase ablation；
Step 3: the product of nanosecond laser irradiation is finally obtained into the sulphur vacancy MoS after freeze-drying2Nanometer sheet.
Further, sulfur-bearing vacancy MoS as described above2The preparation method of nanometer sheet, the step 1 include:
Ammonium molybdate and thiocarbamide dissolution are stirred continuously in deionized water to formation homogeneous solution；
Then solution is transferred in reaction kettle and reacts 4h at 260 DEG C；
It is then cooled to room temperature, product be lyophilized after repeatedly washing obtains MoS for 24 hours2Nanometer sheet presoma.
Further, sulfur-bearing vacancy MoS as described above2The preparation method of nanometer sheet, the step 2 include:
Take 1mg presoma MoS2Nanometer sheet is dispersed in 3ml ethyl alcohol, irradiates 10min using nanosecond laser room temperature.
Further, sulfur-bearing vacancy MoS as described above2The preparation method of nanometer sheet, the nanosecond laser pulsewidth are
7ns, power density 1.8*106W cm-2。
The sulfur-bearing vacancy MoS being prepared according to either method as above2Nanometer sheet.
The utility model has the advantages that
Utilize the MoS in the method for the present invention Laser synthesizing sulfur-bearing vacancy2The method of nanometer sheet cleans, quickly, efficiently, has and passes
The incomparable advantage of system method.
Detailed description of the invention
Fig. 1 is MoS2The sulfur-bearing vacancy MoS of nanometer sheet presoma and laser preparation2The X-ray diffraction result of nanometer sheet；
Fig. 2 is sulfur-bearing vacancy MoS2The low power transmission electron microscope picture of nanometer sheet；Illustration is selective electron diffraction style；
Fig. 3 is sulfur-bearing vacancy MoS2The high power transmission electron microscope picture of nanometer sheet；Dashed region is sulphur vacancy.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the technical solution below in the present invention carries out clear
Chu is fully described by, it is clear that described embodiments are some of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment:
Sulfur-bearing vacancy MoS2Nanometer sheet the preparation method is as follows:
Laser prepares the MoS in sulfur-bearing vacancy2Nanometer sheet first has to synthesis presoma MoS2Nanometer sheet, by 50mg ammonium molybdate and
100mg thiocarbamide, which is dissolved in 30ml deionized water, to be stirred continuously to formation homogeneous solution.Subsequent solution is transferred to the reaction of 50ml
4h is reacted at 260 DEG C in kettle.It is then cooled to room temperature, product be lyophilized after repeatedly washing acquisition presoma MoS for 24 hours2It receives
Rice piece.The MoS in sulfur-bearing vacancy2Nanometer sheet is obtained by laser liquid phase ablation.Use ps pulsed laser and ns pulsed laser Dawa-350, pulsewidth
For 7ns, power density 1.8*106W cm-2.Take 1mg presoma MoS2Nanometer sheet is dispersed in 3ml ethyl alcohol, is swashed using nanosecond
Light room temperature irradiates 10min.The product of acquisition be lyophilized after repeatedly washing the MoS for obtaining sulfur-bearing vacancy for 24 hours2Nanometer sheet.Object phase
Characterization is as shown in Figure 1-3, it is existing for can be seen that by 1-3 using the object phase and sulphur vacancy of the method for the present invention products therefrom.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (5)
1. a kind of sulfur-bearing vacancy MoS2The preparation method of nanometer sheet, which comprises the following steps:
Step 1:MoS2The synthesis of nanometer sheet presoma；
Step 2: the presoma is subjected to nanosecond laser irradiation using laser liquid phase ablation；
Step 3: the product of nanosecond laser irradiation is finally obtained into the sulphur vacancy MoS after freeze-drying2Nanometer sheet.
2. sulfur-bearing vacancy MoS according to claim 12The preparation method of nanometer sheet, which is characterized in that step 1 packet
It includes:
Ammonium molybdate and thiocarbamide dissolution are stirred continuously in deionized water to formation homogeneous solution；
Then solution is transferred in reaction kettle and reacts 4h at 260 DEG C；
It is then cooled to room temperature, product be lyophilized after repeatedly washing obtains MoS for 24 hours2Nanometer sheet presoma.
3. sulfur-bearing vacancy MoS according to claim 22The preparation method of nanometer sheet, which is characterized in that step 2 packet
It includes:
Take 1mg presoma MoS2Nanometer sheet is dispersed in 3ml ethyl alcohol, irradiates 10min using nanosecond laser room temperature.
4. sulfur-bearing vacancy MoS according to claim 32The preparation method of nanometer sheet, which is characterized in that the nanosecond laser
Pulsewidth is 7ns, power density 1.8*106W cm-2。
5. the sulfur-bearing vacancy MoS that -4 either method are prepared according to claim 12Nanometer sheet.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811375638.8A CN109453791A (en) | 2018-11-19 | 2018-11-19 | A kind of sulfur-bearing vacancy MoS2Nanometer sheet and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110787816A (en) * | 2019-11-23 | 2020-02-14 | 台州学院 | Quadruple-modified molybdenum disulfide electrocatalyst and preparation method thereof |
| CN112479257A (en) * | 2020-11-25 | 2021-03-12 | 华中科技大学 | Laser-induced chemical synthesis of micro-nano-scale MoS at normal atmospheric temperature2Method and application of |
| CN114349053A (en) * | 2021-12-02 | 2022-04-15 | 安庆师范大学 | Preparation method and application of molybdenum sulfide nanosheet with controllable sulfur vacancy concentration |
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| US20110303555A1 (en) * | 2010-06-14 | 2011-12-15 | Mohammed Ashraf Gondal | Method for detection of cyanide in water |
| CN106905966A (en) * | 2017-01-12 | 2017-06-30 | 北京理工大学 | A kind of method that individual layer molybdenum bisuphide quantum dot is prepared based on dynamic control |
| CN107185530A (en) * | 2017-04-24 | 2017-09-22 | 天津大学 | The method of silver nano-grain of the Laser synthesizing rich in crystal defect |
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| US20110303555A1 (en) * | 2010-06-14 | 2011-12-15 | Mohammed Ashraf Gondal | Method for detection of cyanide in water |
| CN106905966A (en) * | 2017-01-12 | 2017-06-30 | 北京理工大学 | A kind of method that individual layer molybdenum bisuphide quantum dot is prepared based on dynamic control |
| CN107185530A (en) * | 2017-04-24 | 2017-09-22 | 天津大学 | The method of silver nano-grain of the Laser synthesizing rich in crystal defect |
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| 周玥: "激光合成富含结构缺陷的过渡金属化合物及其能源应用研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110787816A (en) * | 2019-11-23 | 2020-02-14 | 台州学院 | Quadruple-modified molybdenum disulfide electrocatalyst and preparation method thereof |
| CN110787816B (en) * | 2019-11-23 | 2022-06-21 | 台州学院 | Quadruple-modified molybdenum disulfide electrocatalyst and preparation method thereof |
| CN112479257A (en) * | 2020-11-25 | 2021-03-12 | 华中科技大学 | Laser-induced chemical synthesis of micro-nano-scale MoS at normal atmospheric temperature2Method and application of |
| CN114349053A (en) * | 2021-12-02 | 2022-04-15 | 安庆师范大学 | Preparation method and application of molybdenum sulfide nanosheet with controllable sulfur vacancy concentration |
| CN114349053B (en) * | 2021-12-02 | 2023-11-10 | 安庆师范大学 | Preparation method and application of molybdenum sulfide nanosheets with controllable sulfur vacancy concentration |
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