CN107961799A - A kind of pyramid molybdenum disulfide nano sheet and its preparation method and application - Google Patents
A kind of pyramid molybdenum disulfide nano sheet and its preparation method and application Download PDFInfo
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- CN107961799A CN107961799A CN201711157497.8A CN201711157497A CN107961799A CN 107961799 A CN107961799 A CN 107961799A CN 201711157497 A CN201711157497 A CN 201711157497A CN 107961799 A CN107961799 A CN 107961799A
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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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Abstract
The present invention relates to a kind of pyramid molybdenum disulfide nano sheet and its preparation method and application, the method is as follows：S1：3~5min of immersion in hydrofluoric acid is placed in using glass slide as substrate, then cleaning removes surface silicates reaction generation product, drying, spare；S2：With chemical vapour deposition technique, using sublimed sulfur and molybdenum trioxide, molybdenum chloride or four thio ammonium molybdate as sulphur source and molybdenum source, molybdenum disulfide is grown in substrate with three-temperature-zone tube furnace.Pyramid molybdenum disulfide nano sheet size uniform provided by the invention, there is higher density boundary, has excellent conductive performance and catalytic performance.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular, to a kind of pyramid molybdenum disulfide nano sheet
And its preparation method and application.
Background technology
Energy and environment are the topics closely bound up with us, and the growing energy consumption of people and are therefore brought
Contradiction between environmental pollution is becoming increasingly acute.The development and utilization of the recyclable energy especially hydrogen energy source of cleaning both contradictions it
Between have found an equalization point.At present, the mode of hydrogen is produced mostly using the consumption of fossil fuel as cost, caused environment
Problem allows this process to lose more than gain.It is that following most have can be generated electricity based on clean energy resource and be used to being electrolysed aquatic products hydrogen by gained electric energy
It can realize and the commercialized energy produces and storing mode.However, business level production hydrogen process needs the catalyst of efficient stable to carry
For enough avtive spots so as to reduce the overpotential of hydrolysis and accelerate the transfer of electronics.The preferable material of catalytic performance at present
Expect the noble metals such as main Pt and Pb, but since bullion content is less in the earth's crust, material cost is higher, so as to limit its business
The prospect of industryization application.Then, researcher have studied the catalyst of many rich ground prime elements, include the phosphatization of transition metal
Thing, sulfide, carbide etc..Wherein, due to the hydrogen particle absorption energy that its boundary and noble metal are closer to, the two of nanostructured
Molybdenum sulfide has received widespread attention and studies.
The active site of nanometer class molybdenum disulfide is mainly boundary unsaturation bonding atom, and atom does not have in face
There is catalytic activity, but in growth course, due to thermodynamic (al) effect, molybdenum disulfide is mainly shown as the two dimension of epitaxial growth
Plane, this makes it possible to contribute the atom number of catalytic activity extremely low, seriously constrains the catalytic hydrogen evolution ability of MoS2.Thus receive
The molybdenum disulfide of rice structuring is intended to greatly the number of increase avtive spot, the double dodecahedron films of molybdenum disulfide aided in such as template
Deposition, vertical-growth, size the mode such as diminishes.Except the number of avtive spot, electric conductivity also has catalytic performance very big
Influence.And uncontrollable defect is introduced on molybdenum disulfide basal plane and is directly bombarded including plasma, move back in reducing atmosphere
The basal plane of molybdenum disulfide can be divided into discontinuous domain by the modes such as fire, so as to influence the electric conductivity of molybdenum disulfide entirety, be reduced
Catalytic efficiency.
Therefore, research and develop that a kind of more number of active sites, electric conductivity and catalytic performance be good, the simple curing of preparation process
Molybdenum nanometer sheet is most important.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of system of pyramid molybdenum disulfide nano sheet
Preparation Method, the pyramid molybdenum disulfide nano sheet size uniform that method provided by the invention is prepared, there is more high density side
Boundary, has excellent conductive performance and catalytic performance.
The pyramid molybdenum disulfide nano sheet being prepared another object of the present invention is to provide the above method.
The pyramid molybdenum disulfide nano sheet conduct being prepared another object of the present invention is to provide the above method
Application of the catalyst in hydrogen is produced in hydrolysis.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of pyramid molybdenum disulfide nano sheet, the method are as follows：
S1：3~5min of immersion in hydrofluoric acid is placed in using glass slide as substrate, then cleaning removes surface silicates reaction generation
Product, drying, it is spare；
S2：With chemical vapour deposition technique, using sublimed sulfur and molybdenum trioxide, molybdenum chloride or four thio ammonium molybdate as sulphur source and
Molybdenum source, grows molybdenum disulfide with three-temperature-zone tube furnace in substrate；
Wherein, three warm area temperature of three-temperature-zone tube furnace described in growth course are regulated to：From room temperature through 5min~15min liters
Up to 300 DEG C~500 DEG C, keep 5~10min after again by 5~10min be warming up to 730 DEG C~750 DEG C and holding 5~
10min；Then 650 DEG C~700 DEG C DEG C are cooled to through 3~5min and open tube furnace fast cooling；
Air-flow is regulated in growth course：Heat up before reaching 650 DEG C~700 DEG C and open air-flow after tube furnace fast cooling
For 200sccm, during which air-flow is 25sccm~50sccm.
Preferably, in S1, the time of the immersion is 5min.
Preferably, in S1, the mass concentration of the hydrofluoric acid is 30~40%.
Preferably, in S1, the mass concentration of the hydrofluoric acid is 40%.
Preferably, the placement location in the tube furnace of three-temperature-zone is：Sulphur powder is placed on inlet end away from first warm area center 25cm
Place, substrate are placed on second warm area center；Pressure is normal pressure in growth course, first leads to high-purity argon with the flow of 500sccm
Gas（99.999%）10min is cleaned, is then evacuated to 1*10-4Pa, then ventilate to normal pressure.
Preferably, in S2, three warm area temperature of three-temperature-zone tube furnace described in growth course are regulated to：From 30 DEG C of warps
14min is increased to 300 DEG C, is warming up to 730 DEG C by 9min again after keeping 10min and keeps 10min；Then it is cooled to through 3min
700 DEG C and open tube furnace fast cooling；
Air-flow is regulated in growth course：Air-flow is before heating reaches 660 DEG C and after opening tube furnace fast cooling
200sccm, during which air-flow is 50sccm.
Preferably, the specification of the glass slide is the cm of 2.5cm × 1.5.
Preferably, in S1, the cleaning is selection deionized water, acetone, ethanol, each ultrasound of the order of deionized water
5min, ultrasonic power 180w, frequency 40KHz.
Preferably, in S1, the drying is to dry up glass slide elevated pressure nitrogen air gun, and is added on warm table in 150 DEG C
Hot 10min.
In the present invention, the model OTF-1200X- III of the three-temperature-zone tube furnace, manufacturer are Hefei section crystalline substance material
Expect Technology Co., Ltd..
The present invention protects the pyramid molybdenum disulfide nano sheet that above-mentioned preparation method is prepared at the same time.
Above-mentioned pyramid molybdenum disulfide nano sheet as catalyst hydrolysis produce hydrogen in application also the present invention guarantor
Within the scope of shield.
Compared with prior art, the present invention has the advantages that：
The pyramid molybdenum disulfide nano sheet size uniform that method provided by the invention is prepared, there is higher density boundary,
With excellent conductive performance and catalytic performance.And its preparation method is easy to operate, technological process is few, cost is low.
Brief description of the drawings
Fig. 1 is the preparation method flow chart for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides；
Fig. 2 is the schematic diagram and pictorial diagram of the preparation method for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides；
Fig. 3 is the SEM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides, and amplification factor is 12000 times；
Fig. 4 is the SEM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides, and amplification factor is 38000 times；
Fig. 5 is the SEM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides, and amplification factor is 76000 times；
Fig. 6 is the AFM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides；
Fig. 7 is the conductive AFM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides；
Fig. 8 is the TEM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides；
Fig. 9 is the TEM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides.
Embodiment
Further illustrate the present invention below in conjunction with specific embodiments and the drawings, but embodiment the present invention is not done it is any
The restriction of form.Unless stated otherwise, the reagent of the invention used, method and apparatus is the art conventional reagent, methods
And equipment.
Unless stated otherwise, agents useful for same and material of the present invention are purchased in market.
Embodiment 1
As shown in Figure 1, be a kind of preparation method flow chart of the pyramid molybdenum disulfide on high density border of the embodiment of the present invention,
Fig. 2 is the schematic diagram and pictorial diagram of preparation method.The pyramid molybdenum disulfide method on the high density border includes：
Step 101, the pretreatment of substrate；
Step 102, the cleaning of substrate；
Step 103, the drying of substrate；
Step 104, pyramid molybdenum disulfide is grown in substrate with the method for chemical vapor deposition；
In the processing in the step base：By the glass slide cut growth 2.5cm of commercialization, the small pieces of wide 1.5cm, Ran Hou
5 min are soaked in hydrofluoric acid solution, the concentration of hydrofluoric acid is 40%（Tianjin great Mao chemical reagent factories）.
In the cleaning of the step substrate：Glass slide after immersion is removed into the product of surface silicates reaction generation simultaneously
According to deionized water, acetone, ethanol, order each the ultrasound 5min, ultrasonic power 180W, frequency 40KHz of deionized water.
In the drying of the step substrate：Slide after ultrasound elevated pressure nitrogen air gun is dried up, and 150 on warm table
DEG C heating 10min.
In the method for the step chemical vapor deposition grows pyramid molybdenum disulfide in substrate：With chemical gas
The mutually method of deposition, using sublimed sulfur and molybdenum trioxide as sulphur source and molybdenum source, with three-temperature-zone tube furnace（Hefei section crystalline substance material
Technology Co., Ltd., OTF-1200X- III）Pyramid molybdenum disulfide is grown in substrate.
Material utilization amount includes 0.5g sulphur powders（Aladin, 99.99%）, 0.3mg MoO3（Aladin, 99.95%）；Place position
It is set to：Sulphur powder be placed on inlet end away from first warm area center 25cm at, substrate is placed on second warm area center；
Pressure is normal pressure in growth course, first leads to high-purity argon gas with the flow of 500sccm（99.999%）10min is cleaned, is then taken out
Vacuum is to 1*10-4Pa, then ventilate to normal pressure；
Three warm area temperature are regulated in growth course：From room temperature（30℃）300 DEG C are increased to by 14min, after keeping 10min
730 DEG C are being warming up to by 9min and is keeping 10min, are cooled to 700 DEG C through 3min and are opened tube furnace fast cooling.
Air-flow is regulated in growth course：Heat up before reaching 660 DEG C and open Ar gas gas after tube furnace fast cooling
Stream is 200sccm, and during which air-flow is 50sccm.
Fig. 3 is the SEM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides, and amplification factor is 12000 times, can
In the interior pyramid molybdenum disulfide for observing size uniform in a big way；
Fig. 4 is the SEM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides, and amplification factor is 38000 times, Observable
To the stratiform pyramid structure of grown molybdenum disulfide；
Fig. 5 is the SEM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides, and amplification factor is 76000 times, can be into one
Step observes the pyramid structure of the stacked in layers of grown molybdenum disulfide；
Fig. 6 is the AFM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides, it can be seen that the height of pyramid step
Spend poor, its provable stacked in layers structure；
Fig. 7 is the conductive AFM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides, can by adding small voltage to survey electric current
Reflect the good electric conductivity on direction in vertical plane；
Fig. 8 is the TEM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides, considerable to measure layer of molybdenum-disulfide shape stacking
Structure, every layer is concentric triangle, and size is successively successively decreased；
Fig. 9 is the TEM figures for the pyramid molybdenum disulfide that the embodiment of the present invention 1 provides, and can further observe layer of molybdenum-disulfide
The structure that shape stacks.
In conclusion the pyramid molybdenum disulfide nano sheet that embodiment 1 is prepared has preferable electric conductivity.
Embodiment 2
In the present embodiment, the mass concentration of the hydrofluoric acid in step 101 is 35%, scavenging period 5min.
In step 104, three warm area temperature are regulated in growth course：300 DEG C are increased to from 30 DEG C by 5min, is kept
It is being warming up to 750 DEG C by 10min after 5min and keeps 5min, be cooled to through 3 min, 650 DEG C and is opening the fast prompt drop of tube furnace
Temperature.
Air-flow is regulated in growth course：Heat up before reaching 650 DEG C and open Ar gas gas after tube furnace fast cooling
Stream is 200sccm, and during which air-flow is 25sccm.
Embodiment 3
In the present embodiment, the mass concentration of the hydrofluoric acid in step 101 is 30%, scavenging period 5min.
In step 104, three warm area temperature are regulated in growth course：400 DEG C are increased to from 30 DEG C by 15min, is protected
Hold, be warming up to 740 DEG C by 9 min after 8min and keep 8min, pass through, 5min is cooled to 680 DEG C and to open tube furnace quick
Cooling.
Air-flow is regulated in growth course：Heat up before reaching 700 DEG C and open Ar gas gas after tube furnace fast cooling
Stream is 200sccm, and during which air-flow is 40sccm.
Above-described embodiment, has carried out the purpose of the present invention, technical solution and beneficial effect further
Describe in detail, it should be understood that the foregoing is merely the embodiment of the present invention, be not intended to limit the present invention
Protection domain, the change or replacement that can be readily occurred in, should be covered by the protection scope of the present invention.Therefore, it is of the invention
Protection domain should be subject to the protection domain of claims.
Claims (10)
1. a kind of preparation method of pyramid molybdenum disulfide nano sheet, it is characterised in that the method is as follows：
S1：3~5min of immersion in hydrofluoric acid is placed in using glass slide as substrate, then cleaning removes surface silicates reaction generation
Product, drying, it is spare；
S2：With chemical vapour deposition technique, using sublimed sulfur and molybdenum trioxide, molybdenum chloride or four thio ammonium molybdate as sulphur source and
Molybdenum source, grows molybdenum disulfide with three-temperature-zone tube furnace in substrate；
Wherein, three warm area temperature of three-temperature-zone tube furnace described in growth course are regulated to：From room temperature through 5min~15min liters
Up to 300 DEG C~500 DEG C, keep 5~10min after again by 5~10min be warming up to 730 DEG C~750 DEG C and holding 5~
10min；Then 650 DEG C~700 DEG C are cooled to through 3~5min and open tube furnace fast cooling；
Air-flow is regulated in growth course：Heat up before reaching 650 DEG C~700 DEG C and open air-flow after tube furnace fast cooling
For 200sccm, during which air-flow is 25sccm~50sccm.
2. preparation method according to claim 1, it is characterised in that in S1, the time of the immersion is 5min.
3. preparation method according to claim 1, it is characterised in that in S1, the mass concentration of the hydrofluoric acid for 30~
40%。
4. preparation method according to claim 3, it is characterised in that in S1, the mass concentration of the hydrofluoric acid is 40%.
5. preparation method according to claim 1, it is characterised in that in S2, three-temperature-zone tube furnace described in growth course
Three warm area temperature are regulated to：300 DEG C are increased to from 30 DEG C through 14min, 730 DEG C are warming up to by 9min again after keeping 10min
And keep 10min；Then 700 DEG C are cooled to through 3min and open tube furnace fast cooling；
Air-flow is regulated in growth course：Air-flow is before heating reaches 660 DEG C and after opening tube furnace fast cooling
200sccm, during which air-flow is 50sccm.
6. preparation method according to claim 1, it is characterised in that the specification of the glass slide is the cm of 2.5cm × 1.5.
7. preparation method according to claim 1, it is characterised in that in S1, it is described cleaning for select deionized water, acetone,
Ethanol, the order of deionized water each ultrasound 5min, ultrasonic power 180w, frequency 40KHz.
8. preparation method according to claim 1, it is characterised in that in S1, the drying is by glass slide high pressure nitrogen
Rifle dries up, and heats 10min in 150 DEG C on warm table.
9. the pyramid molybdenum disulfide nano sheet that any preparation method of claim 1~8 is prepared.
10. application of the pyramid molybdenum disulfide nano sheet described in claim 9 as catalyst in hydrogen is produced in hydrolysis.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109881176A (en) * | 2019-03-08 | 2019-06-14 | 华南农业大学 | A kind of petal-like molybdenum disulfide two dimensional crystal material and its preparation method and application |
| CN110172736A (en) * | 2019-06-06 | 2019-08-27 | 华中科技大学 | A kind of chemical gas-phase deposition process for preparing of three layers of large scale vulcanization molybdenum single crystal |
| CN114380334A (en) * | 2022-01-26 | 2022-04-22 | 江西师范大学 | Preparation method and application of molybdenum disulfide with spiral pyramid structure |
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| KR20170042157A (en) * | 2015-10-08 | 2017-04-18 | 한국과학기술원 | Two-dimensional layred metal sulfide anchored to hollow carbon nanofibers as hydrogen evolution reaction catalysts and manufacturing method thereof |
| CN106865616A (en) * | 2017-03-30 | 2017-06-20 | 华南师范大学 | The method for preparing the porous two-dimentional molybdenum disulfide nano sheet of high density |
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| KR20170042157A (en) * | 2015-10-08 | 2017-04-18 | 한국과학기술원 | Two-dimensional layred metal sulfide anchored to hollow carbon nanofibers as hydrogen evolution reaction catalysts and manufacturing method thereof |
| CN106865616A (en) * | 2017-03-30 | 2017-06-20 | 华南师范大学 | The method for preparing the porous two-dimentional molybdenum disulfide nano sheet of high density |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109881176A (en) * | 2019-03-08 | 2019-06-14 | 华南农业大学 | A kind of petal-like molybdenum disulfide two dimensional crystal material and its preparation method and application |
| CN110172736A (en) * | 2019-06-06 | 2019-08-27 | 华中科技大学 | A kind of chemical gas-phase deposition process for preparing of three layers of large scale vulcanization molybdenum single crystal |
| CN114380334A (en) * | 2022-01-26 | 2022-04-22 | 江西师范大学 | Preparation method and application of molybdenum disulfide with spiral pyramid structure |
| CN114380334B (en) * | 2022-01-26 | 2023-09-19 | 江西师范大学 | Preparation method and application of molybdenum disulfide with spiral pyramid structure |
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