CN106966384A - A kind of preparation method of molybdenum disulfide/graphene stratiform assembly - Google Patents
A kind of preparation method of molybdenum disulfide/graphene stratiform assembly Download PDFInfo
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- CN106966384A CN106966384A CN201710192927.3A CN201710192927A CN106966384A CN 106966384 A CN106966384 A CN 106966384A CN 201710192927 A CN201710192927 A CN 201710192927A CN 106966384 A CN106966384 A CN 106966384A
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- C—CHEMISTRY; METALLURGY
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- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
The present invention relates to a kind of preparation method of molybdenum disulfide/graphene stratiform assembly, using single quartz ampoule, coordinate the tube furnace of double furnace；The SiO for having graphene film will be shifted2/ Si substrates, are placed in and are placed with above the container of molybdenum trioxide powder, the container for being placed with sulphur powder is placed in first heating furnace center of tube furnace；The container for being placed with molybdenum trioxide is put in second heating furnace center of tube furnace again；It is passed through argon gas；Under an argon atmosphere, tube furnace internal pressure is emphasized to 133.29Pa, the first heating zone is warming up to the volatilization temperature of sulphur powder, and the second heating zone is warming up to the volatilization temperature of molybdenum trioxide；Molybdenum disulfide is deposited on substrate, be then down to room temperature, obtain molybdenum disulfide/graphene stratiform assembly.With large area, high-quality feature, light intensity is 94 μ W/cm2, density of photocurrent reaches 3.0 μ A/cm2, photocurrent response completes in photoswitch moment 2.3s；With good application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of molybdenum disulfide/graphene stratiform assembly, belong to semiconductor film material
Preparation field.
Background technology
The strong electron-hole limit that two-dimensional layer material molybdenum disulfide, graphene are produced because of its unique planar structure
The properties such as domain, pliability, high transparency, make it have more in thinner, more flexible, the high performance field of photoelectric devices of the next generation
It is widely applied.But the phototransistor that individually molybdenum disulfide is prepared from has low photoresponse 7.5mA/W, because
The low carrier mobility of molybdenum disulfide, the schottky junction also formed in addition in device between molybdenum disulfide and electrode is (by electrode
The regulation and control of material) influence.Again because the absorbance of graphene only has the 2.3% of visible ray, photoelectricity prepared by independent graphene
The photoresponse of detector only has 6.1mA W-1, this just greatly limit application of the graphene in field of photoelectric devices.In consideration of it, burnt
Point is just lifting the photoresponse of phototransistor using molybdenum disulfide/graphene laminar composite.Utilize molybdenum disulfide
Light selectivity and the high carrier mobility property of graphene carry out light absorbs with molybdenum disulfide, while graphene is used as current-carrying
The passage of son migration, improves photoresponse.So the present invention combines graphene and MoS2Two kinds of materials, form a kind of new heterogeneous
Junction device, by MoS2The excellent electric property of sensitization and graphene to light combines, by two kinds of material advantage complementations,
Promote graphene and MoS2In the extensive use of electronic applications.
Preparing the method for molybdenum disulfide/graphene laminar composite mainly has three kinds：Hydrothermal synthesis method, physics construction from part
And chemical vapour deposition technique.All there are respective advantage and disadvantage in hydrothermal synthesis method and physics construction from part, prepared by wherein hydrothermal synthesis method
Molybdenum disulfide/graphene laminar composite lamella it is smaller, uneven, pattern cannot be controlled effectively, and yield is relatively low, and
Process-intensive, complex operation, are unfavorable for industrial volume production；Molybdenum disulfide/graphene stratiform assembly prepared by physics assembling method
Lamella there was only micron order, be unfavorable for the integrated and industrialization of photoelectric device, in addition physics assembling transfer process in introduce it is miscellaneous
Van der Waals force between matter and molybdenum disulfide and graphene layer is weaker, can all influence its photoelectric properties.And chemical vapour deposition technique system
Standby molybdenum disulfide/graphene stratiform assembly is the direct growth molybdenum disulfide in large-area graphene film, between the two
Van der Waals force is stronger, and obtain be large area molybdenum disulfide on graphene, can mass produce, obtained complex
Crystallinity, the quality of molybdenum disulfide can control well.
Although but using molybdenum disulfide/graphene stratiform assembly area prepared by chemical gas-phase method at present relatively
Greatly, there are still molybdenum disulfide crystal property is poor, the not high defect of crystalline quality.This will can influence assembly in photoelectric device
The performance in field.Wherein, influenceing the factor of double-deck molybdenum disulfide/graphene stratiform assembly crystalline quality includes：Molybdenum source
Mass ratio with sulphur source, prepare pressure, preparation temperature, carrier gas flux, heating rate etc..Probed into, optimized by a series of experiments
Experimentation, has obtained preparing the optimal of Layer by layer assembly body and has prepared pressure, temperature, carrier gas flux, heating rate.The present invention passes through
The mass ratio of molybdenum source and sulphur source is adjusted, two layers of molybdenum disulfide/graphene, three layers of molybdenum disulfide/graphene Layer by layer assembly are realized
The controllable preparation of body.
The present invention prepares double-deck molybdenum disulfide/graphene stratiform assembly using chemical vapour deposition technique, prepares big
It is area, high-quality composite assembled.On the whole chemical vapour deposition technique is controllable preparation molybdenum disulfide/graphene stratiform group
Body is filled, its excellent means in field of photoelectric devices integra-tion application is realized.
The content of the invention
It is an object of the invention to provide a kind of preparation method of molybdenum disulfide/graphene stratiform assembly, have in transfer
The SiO of graphene film2On/Si substrates, double-deck molybdenum disulfide is prepared by chemical vapour deposition technique, double-deck curing is just obtained
Molybdenum/graphene stratiform assembly.The semi-conducting material prepared by this method, with excellent opto-electronic conversion and photoelectric current
Response performance.
The present invention is realized by the following technical scheme：
A kind of preparation method of molybdenum disulfide/graphene stratiform assembly, including procedure below：
(1) single quartz ampoule is used, coordinates the tube furnace of double furnace；The SiO for having graphene film will be shifted2/ Si bases
Plate, is placed in and is placed with above the container of molybdenum trioxide powder, the container for being placed with sulphur powder is placed in first heating furnace of tube furnace
The heart；The container for being placed with molybdenum trioxide is put in second heating furnace center of tube furnace again；It is passed through argon gas；
(2) under an argon atmosphere, tube furnace internal pressure is emphasized to 133.29Pa, the first heating zone is warming up to waving for sulphur powder
Temperature is sent out, the second heating zone is warming up to the volatilization temperature of molybdenum trioxide；Molybdenum disulfide is deposited on substrate, be then down to room temperature,
Just obtain molybdenum disulfide/graphene stratiform assembly.
It is preferred that 160 DEG C of the volatilization temperature of sulphur powder
It is preferred that 650 DEG C of the volatilization temperature of molybdenum trioxide
It is preferred that SiO2/ Si substrates are failed to grow up in 1cm, wide to be not more than 1cm, thick 0.5mm.
It is preferred that the container for being placed with molybdenum trioxide powder is ship type porcelain boat.
It is preferred that ship type porcelain boat long 6cm, wide 3cm, deep 1cm.
It is preferred that molybdenum trioxide and the mass ratio of sulphur powder are 1~3:100.
It is described as follows：Following not limit unique method, graphene film prepared by other method etc. is suitable for this
Invention.
A kind of preparation method of molybdenum disulfide/graphene stratiform assembly of the present invention includes procedure below：
First, the preparation and transfer of graphene
(1) copper clad laminate is pre-processed：Copper foil is cut into a certain size, certain density acetic acid solution, acetone is respectively placed in
Ultrasonically treated a period of time in reagent, ethanol reagent, it is subsequently placed in acetone and preserves to use after；
(2) graphene is prepared:Treated copper foil is put into tube furnace, heating schedule is set, passes first into 500sccm's
Argon gas, by the air emptying in tube furnace；Then it is increased to 1030- under argon gas 300sccm and hydrogen 100sccm mixed atmospheres
1050 DEG C, keep 30-40min.Then cool, be passed through throughput 0.6-0.8sccm methane, along with the argon of certain throughput
Gas 1000sccm and hydrogen 10sccm, keeps 20min；Room temperature quickly finally is down under argon stream amount 300sccm, obtains big
Area graphite alkene film；
(3) transfer of graphene：10mg/ml PMMA solution is configured, it is then thin to above-mentioned graphene with desk-top sol evenning machine
Film carries out spin coating；Sample after spin coating is toasted into 10-20min at 150 DEG C, solidifies PMMA；It is molten with 20mg/ml sodium hydroxide
Liquid is as electrolyte, and anode is metal platinum, and negative electrode is the graphene/copper foil for scribbling PMMA, and applied voltage is set to -5 to -6V,
Copper foil surface is produced hydrogen using electrochemical reaction, PMMA/ graphene films are peeled off into copper foil surface, by PMMA/ graphenes
Film is placed in deionized water and cleaned；SiO is placed in after sample after cleaning is cut2On/Si substrates, after drying at 120 DEG C
15min is toasted, strengthens the adhesion between PMMA and substrate, is then respectively placed in acetone, isopropanol, chloroform and soaks
10min, removes PMMA films, then is dried up with nitrogen, and most graphene is successfully moved to new SiO at last2/ Si substrates are (childlike
It is wide to be not more than 1cm, thick 0.5mm in 1cm) on.
2nd, the preparation method of molybdenum disulfide/graphene stratiform assembly
(1) SiO for having graphene film will be shifted2/ Si substrates, are placed in the ship type for being placed with certain mass molybdenum trioxide powder
The surface of high-temperature resistant container, the ship type high-temperature resistant container for being placed with certain mass sulphur powder is placed in first heating furnace of tube furnace
(wherein sulphur powder consumption is 500mg, and the mass ratio of molybdenum trioxide and sulphur powder is 1~3 at center:100.1：100 mass-energy densities obtain 2
Layer molybdenum disulfide, 3：100 mass-energy densities obtain 3 layers of molybdenum disulfide)；The container for being placed with certain mass molybdenum trioxide is put in pipe again
Second heating furnace center of formula stove；A certain amount of argon gas is passed through before starting to warm up and drains quartzy inner air tube；
(2) and then under an argon atmosphere, tube furnace internal pressure is emphasized to 133.29Pa, the first heating zone is warming up to 160
DEG C, the second heating zone be warming up to 650 DEG C (in temperature-rise period keep two heating zones in same time, rise to corresponding temperature,
Heating-up time is 1 hour).Keeping temperature 10min, is then down to room temperature, just obtains molybdenum disulfide/graphene Layer by layer assembly respectively
Body.
Double-deck molybdenum disulfide/graphene stratiform assembly is prepared into ultra-large type phototransistor and its photo electric is tested
Can, excellent opto-electronic conversion and photocurrent response performance is obtained, is 94 μ W/cm in light intensity2, density of photocurrent can still reach
3.0μA/cm2, photocurrent response can be completed in light on-off moment in 2.3s, and photoelectric current is not obvious in 8 circulations
Decay.
The molybdenum disulfide that the present invention is prepared/graphene stratiform assembly has large area, high-quality feature, two
The field of optoelectronic devices such as primary cell, field-effect transistor, sensor, organic electroluminescent, electricity storage have good application
Prospect.
Brief description of the drawings
The optical photograph of the double-deck molybdenum disulfide obtained in Fig. 1 in (a) embodiment 1/graphene stratiform assembly；
The double-deck MoS obtained in Fig. 1 in (b) embodiment 12The optical photograph of/graphene stratiform assembly；
The double-deck MoS obtained in Fig. 1 in (c) embodiment 12The optical photograph of/graphene stratiform assembly；
In Fig. 2 in (a) embodiment 2 double-deck molybdenum disulfide/graphene stratiform assembly TEM image.
In Fig. 2 in (b) embodiment 2 double-deck molybdenum disulfide/graphene stratiform assembly TEM image.
The high power TEM image of the three layers of molybdenum disulfide obtained in Fig. 3 in (a) embodiment 3/graphene stratiform assembly.
The high power TEM image of the three layers of molybdenum disulfide obtained in Fig. 3 in (b) embodiment 3/graphene stratiform assembly.
Embodiment
The specific embodiment of the present invention is given below, is that the present invention is further illustrated, rather than the limitation present invention
Scope.
Embodiment 1：
The graphene used in this example is to be prepared using the method for the present invention and shifted what is obtained.
(1) SiO for having graphene film will be shifted2/ Si substrates, are placed in the ship type porcelain boat for being placed with 5mg molybdenum trioxide powders
Surface, the ship type porcelain boat for being placed with 500mg sulphur powders is placed in the first heating zone of tube furnace, then the porcelain boat that will be placed with molybdenum trioxide
The second heating zone of tube furnace is put in, argon gas is passed through before starting to warm up and drains quartzy inner air tube.
(2) under the protection of 50sccm argon gas, pressure is adjusted to 133.29Pa, within the time of one hour, by the first heating zone
160 DEG C are warming up to, the second heating zone is warming up to 650 DEG C simultaneously.Keeping temperature 10min, is then down to room temperature, just obtains bilayer two
Molybdenum sulfide/graphene stratiform assembly.
In the embodiment in the optical photograph such as Fig. 1 of sample (a), (b), shown in (c).Wherein figure (b) is square frame in figure (a)
The enlarged drawing in region, further contrast indicates the uniformity of large-area graphene, and large area molybdenum disulfide is in graphene
On uniformity.And scheme the enlarged drawing that (c) is the square area of figure (b), as can be seen from the figure large area molybdenum disulfide
It is grown on graphene film.The colour consistency of molybdenum disulfide can also illustrate that the crystalline quality of molybdenum disulfide is fine.
Double-deck molybdenum disulfide/graphene stratiform assembly is prepared into ultra-large type phototransistor and its photo electric is tested
Can, excellent opto-electronic conversion and photocurrent response performance is obtained, is 94 μ W/cm in light intensity2, density of photocurrent can still reach
3.0μA/cm2, photocurrent response can be completed in light on-off moment in 2.3s, and photoelectric current is not obvious in 8 circulations
Decay.
Embodiment 2：
The graphene used in this example is purchased from Nanjing Xian Feng Nono-material Science ＆ Technology Ltd., and numbering is：XF040,
Parameter is：Individual layer, size 1cm*1cm.
(1) SiO for having graphene film will be shifted2/ Si substrates, are placed in the ship type porcelain boat for being placed with 10mg molybdenum trioxide powders
Surface, the ship type porcelain boat for being placed with 500mg sulphur powders is placed in the first heating zone of tube furnace, then the porcelain boat that will be placed with molybdenum trioxide
The second heating zone of tube furnace is put in, argon gas is passed through before starting to warm up and drains quartzy inner air tube.
(2) under the protection of 50sccm argon gas, pressure is adjusted to 133.29Pa, within the time of one hour, by the first heating zone
160 DEG C are warming up to, the second heating zone is warming up to 650 DEG C simultaneously.Keeping temperature 10min, is then down to room temperature respectively, just obtains double
Layer molybdenum disulfide/graphene stratiform assembly.
The result obtained in the embodiment is as shown in Fig. 2 in Fig. 2 (a), (b) briefly understands molybdenum disulfide in graphene
Growth course in template, molybdenum disulfide is deposited on the molybdenum disulfide particles that graphenic surface is initially formed tens Nano grades,
Reaction is further carried out, and micron class molybdenum disulfide continues to connect into schemed the large area molybdenum disulfide as shown in (b) in graphene
On.
Embodiment 3：
The graphene used in this example is according to document：Li X,Cai W,An J,et al.Large-area
synthesis of high-quality and uniform graphene films on copper foils.[J]
.Science,2009,324(5932):1312. are prepared.
(1) SiO for having graphene film will be shifted2/ Si substrates, are placed in the ship type porcelain boat for being placed with 15mg molybdenum trioxide powders
Surface, the ship type porcelain boat for being placed with 500mg sulphur powders is placed in the first heating zone of tube furnace, then the porcelain boat that will be placed with molybdenum trioxide
The second heating zone of tube furnace is put in, argon gas is passed through before starting to warm up and drains quartzy inner air tube.
(2) and then under the protection of 50sccm argon gas, pressure is adjusted to 133.29Pa.Within the time of one hour, first is added
Hot-zone is warming up to 160 DEG C, and the second heating zone is warming up to 650 DEG C simultaneously.Keeping temperature 10min, is then down to room temperature respectively, must
To three layers of molybdenum disulfide/graphene stratiform assembly.
The transmission electron microscope photo of sample is as shown in Figure 3 in the embodiment.It can be clearly seen in Fig. 3, two obtained sulphur
Change molybdenum good crystallinity.
Claims (7)
1. the preparation method of a kind of molybdenum disulfide/graphene stratiform assembly, it is characterised in that including procedure below：
(1) single quartz ampoule is used, coordinates the tube furnace of double furnace；The SiO for having graphene film will be shifted2/ Si substrates, put
In being placed with above the container of molybdenum trioxide powder, the container for being placed with sulphur powder is placed in first heating furnace center of tube furnace；Again
The container for being placed with molybdenum trioxide is put in second heating furnace center of tube furnace；It is passed through argon gas；
2) under an argon atmosphere, tube furnace internal pressure is emphasized to 133.29Pa, the first heating zone is warming up to the volatilization temperature of sulphur powder
Degree, the second heating zone is warming up to the volatilization temperature of molybdenum trioxide；Molybdenum disulfide is deposited on substrate, be then down to room temperature, must
To molybdenum disulfide/graphene stratiform assembly.
2. the method as described in claim 1, it is characterized in that SiO2/ Si substrates are failed to grow up in 1cm, wide to be not more than 1cm, thickness
0.5mm。
3. the method as described in claim 1, it is characterized in that the container for being placed with molybdenum trioxide powder is ship type porcelain boat.
4. method as claimed in claim 3, it is characterized in that ship type porcelain boat long 6cm, wide 3cm, deep 1cm.
5. the method as described in claim 1, it is characterized in that molybdenum trioxide and the mass ratio of sulphur powder are 1~3:100.
6. the method as described in claim 1, it is characterized in that 160 DEG C of the volatilization temperature of sulphur powder.
7. the method as described in claim 1, it is characterized in that 650 DEG C of the volatilization temperature of molybdenum trioxide.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108636426A (en) * | 2018-03-22 | 2018-10-12 | 西北工业大学 | Three-dimensional order is orientated molybdenum disulfide/graphene high-efficiency photocatalysis hydrogen production composite nano materials and preparation method |
| CN108666381A (en) * | 2018-05-09 | 2018-10-16 | 深圳大学 | A kind of heterojunction photovoltaic sensor and preparation method thereof |
| CN109336181A (en) * | 2018-09-20 | 2019-02-15 | 天津大学 | A kind of preparation method of two dimension Transition-metal dichalcogenide |
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|---|---|---|---|---|
| CN102191476A (en) * | 2011-04-11 | 2011-09-21 | 兰州大学 | Method for preparing sulfur-doped graphene films |
| CN103840158A (en) * | 2014-03-21 | 2014-06-04 | 新疆大学 | Preparation method for graphene/molybdenum disulfide composite material |
| CN105271800A (en) * | 2015-11-06 | 2016-01-27 | 天津大学 | Preparation method of large-area molybdenum disulfide film material |
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2017
- 2017-03-28 CN CN201710192927.3A patent/CN106966384A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102191476A (en) * | 2011-04-11 | 2011-09-21 | 兰州大学 | Method for preparing sulfur-doped graphene films |
| CN103840158A (en) * | 2014-03-21 | 2014-06-04 | 新疆大学 | Preparation method for graphene/molybdenum disulfide composite material |
| CN105271800A (en) * | 2015-11-06 | 2016-01-27 | 天津大学 | Preparation method of large-area molybdenum disulfide film material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108636426A (en) * | 2018-03-22 | 2018-10-12 | 西北工业大学 | Three-dimensional order is orientated molybdenum disulfide/graphene high-efficiency photocatalysis hydrogen production composite nano materials and preparation method |
| CN108666381A (en) * | 2018-05-09 | 2018-10-16 | 深圳大学 | A kind of heterojunction photovoltaic sensor and preparation method thereof |
| CN108666381B (en) * | 2018-05-09 | 2020-08-25 | 深圳大学 | Heterojunction photoelectric sensor and preparation method thereof |
| CN109336181A (en) * | 2018-09-20 | 2019-02-15 | 天津大学 | A kind of preparation method of two dimension Transition-metal dichalcogenide |
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Application publication date: 20170721 |