CN205473973U - Chemical vapor deposition equipment based on pulsating gas flow growth molybdenum disulfide film - Google Patents
Chemical vapor deposition equipment based on pulsating gas flow growth molybdenum disulfide film Download PDFInfo
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- CN205473973U CN205473973U CN201620184845.5U CN201620184845U CN205473973U CN 205473973 U CN205473973 U CN 205473973U CN 201620184845 U CN201620184845 U CN 201620184845U CN 205473973 U CN205473973 U CN 205473973U
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- molybdenum disulfide
- chemical vapor
- disulfide film
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- gas
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Abstract
The utility model discloses a chemical vapor deposition equipment based on pulsating gas flow growth molybdenum disulfide film, its characterized in that: equipment includes brace table, quartz capsule, a tube heating furnace thorax, no. Two tube heating furnace thoraxes, constant temperature tympanic bulla bottle, air intake system and tail gas systems, the quartz capsule passes through the supporting mechanism to be fixed on the brace table, a tube heating furnace thorax and no. Two tube heating furnace thoraxes pass through the slide rail and radially slide along the quartz capsule external diameter, establish respectively to the inlet end and the end of giving vent to anger at the quartz capsule both ends, the inlet end all is equipped with the sealing flange with the end of giving vent to anger, the inlet end is through sealed flange joint air intake system and constant temperature tympanic bulla bottle, give vent to anger the end through sealed flange joint tail gas system. Adopt chemical vapor deposition equipment can obtain the large size stratiform molybdenum disulfide film of high quality, for the preparation TMDs photoelectric device take a firm foundation.
Description
Technical field
This utility model relates to technical field prepared by molybdenum disulfide film, is related specifically to a kind of based on arteries and veins
The chemical vapor depsotition equipment of qi of chong channel ascending adversely stream growth molybdenum disulfide film.
Background technology
Platelike molybdenumdisulfide (MoS2) it is one of the typical material of two dimension Transition-metal dichalcogenide, have solely
Special character: 1) its single layer structure has class graphene-structured；2) monolayer MoS2 has and is similar to Sanming City
The structure of the S-Mo-S controlled, belongs to hexagonal crystal system；3) along with the reduction of film thickness, its band gap increases,
When thickness is reduced to monolayer, it is become direct band-gap semicondictor material by indirect band-gap semiconductor, its band gap
Being about 1.9eV, its luminous efficiency is greatly enhanced；4) there is good carrier transport performance, micro-
The numerous areas such as organic electronic, energy storage device, sensor, display floater and solaode all have widely
Potential application foreground, as with monolayer molybdenum bisuphide (MoS2) field-effect transistor prepared, its switch current ratio
Up to 108, energy consuming ratio traditional silicon transistor is little 100,000 times at steady state；5) have significant photic glimmering
Optical phenomenon, under excitation light irradiation, due to the transition of AB exciton, can～670nm and～620nm at
Launch fluorescence.
But, preparation is based on MoS2High performance device be limited to the controlling of MoS2 of large scale high weight
Standby.At present, monolayer MoS2Preparation method be broadly divided into: " from top to bottom " and " from bottom to top " two kinds.
" from top to bottom " preparation method specifically includes that micromechanics stripping method, liquid phase chemical stripping method, laser subtract
Bao Fa etc..These methods are obtained in that the MoS of monolayer2Thin film, but the MoS obtained2Film dimensions is little,
And size and THICKNESS CONTROL poor." from bottom to top " preparation method is mainly by different molybdenum sources and sulfur
Source is reacted, and obtains large-area MoS by vapour deposition2Thin film." from bottom to top " preparation method
Specifically include that electron beam evaporation, thermal decomposition, molecular beam epitaxial growth method and chemical vapour deposition technique etc..
In these methods, deposited by electron beam evaporation Mo metal carries out the method vulcanized again, preparation process in two steps, the number of plies
It is poor to control, difficult acquisition monolayer；With (NH4) MoS4The method carrying out for source thermally decomposing, tail gas pollution, can only
Prepare three layers and above MoS2Thin film；Patent 201510134872.1 discloses the curing of a kind of stratiform
The preparation method of molybdenum film, uses molecular beam epitaxial growth method, by accurately controlling sulfur source and the input in molybdenum source,
Obtain stratiform MoS2, and it is limited to growth apparatus size by molecular beam epitaxial growth method, it is difficult to obtain big chi
Very little monolayer MoS2Material；And traditional chemical vapour deposition technique is directly by solid-state sulfur powder and MoO3Same
Evaporation is also reacted in tube furnace, lacks the accurate control to its flow, thus the number of plies and the repeatability of size,
Less stable.Our company proposes a kind of method based on air pulse method growth stratiform molybdenum disulfide film,
By input flow rate and the pulse input mode of reaction source gas in PEMOCVD reative cell, can obtain
High-quality and the controlled large scale molybdenum disulfide film of the number of plies.But traditional chemical vapor depsotition equipment is difficult to
Control molybdenum oxide and the pulse input mode of reaction of Salmon-Saxl source of the gas, it is achieved patent of invention number) propose based on arteries and veins
The method of qi of chong channel ascending adversely stream method growth stratiform molybdenum disulfide film, obtains the large-sized platelike molybdenumdisulfide of high-quality thin
Film.
Utility model content
The purpose of this utility model is to propose a kind of chemical gas based on air pulse growth molybdenum disulfide film
Phase depositing device, it is possible to obtain high-quality large-sized platelike molybdenumdisulfide thin film, for preparation TMDs phototube
Part is taken a firm foundation.
To this end, this utility model is by the following technical solutions:
A kind of chemical vapor depsotition equipment based on air pulse growth molybdenum disulfide film, described equipment includes
Support platform, quartz ampoule, tubular heater thorax, No. two tubular heater thoraxes, constant temperature bubbling bottle, air inlets
System and exhaust system；Described quartz ampoule is fixed on support platform by supporting mechanism, a described tubular type
Heating furnace and No. two tubular heater thoraxes are radially slided along quartz ampoule external diameter by slide rail；Described quartz ampoule two
End is set to inlet end and outlet side, and described inlet end and outlet side are equipped with sealing flange；Described air inlet
Holding and connect gas handling system and constant temperature bubbling bottle by sealing flange, described outlet side connects tail by sealing flange
Gas system.
Preferably, a described tubular heater thorax is near inlet end, and No. two tubular heater thoraxes are near giving vent to anger
End.
Preferably, described gas handling system includes gas cylinder, 2 gas mass flow controllers, 3/2 intake valves and 3
Individual pneumatic operated valve, described gas cylinder, 1 gas mass flow controller and 1 pneumatic operated valve are by stainless steel tube 200 even
Logical quartz ampoule inlet end sealing flange；Described gas cylinder and 1 gas mass flow controller pass through stainless steel tube
200 connection constant temperature bubbling bottles；Described constant temperature bubbling bottle connects 3/2 intake valve, and 1 pneumatic operated valve passes through rustless steel
Pipe 300 connects quartz ampoule inlet end sealing flange, and and 1 pneumatic operated valve cross stainless steel tube 300 and be connected to tail gas
System.
Preferably, described exhaust system include chamber pressure detector, chamber pressure control butterfly valve, pneumatic operated valve,
Manual ball valve, sulfur filter, molecular pump, mechanical pump and exhaust gas processing device, described chamber pressure detector
It is positioned on the sealing flange of outlet side；Described chamber pressure controls butterfly valve, pneumatic operated valve and manual ball valve by not
Rust steel pipe 300 connects sulfur filter, and described sulfur filter, molecular pump, mechanical pump and exhaust gas processing device pass through
Stainless steel tube 200 connects.
Preferably, the outer layer of described stainless steel tube 300 uses heated at constant temperature band parcel.
Preferably, described chamber pressure controls butterfly valve, pneumatic operated valve and manual ball valve and uses heating clothing parcel, anti-
Only tail gas condensing blocks.
Preferably, described sealing flange uses circulating water.
This utility model uses above technical scheme, uses the input controllable precise of above-mentioned reaction source gas with anti-
Answer the chemical vapor depsotition equipment that chamber pressure is controlled, by accurately control reaction source gas input flow rate and
Pulse input mode, regulation and control molybdenum disulfide film nucleation and the speed of growth, it is possible to obtain tactical rule, table
High-quality large-sized platelike molybdenumdisulfide thin film that face is smooth.
Accompanying drawing explanation
Fig. 1 is this utility model chemical vapor depsotition equipment based on air pulse growth molybdenum disulfide film
Structural representation.
Fig. 2 is the schematic diagram of this utility model embodiment reaction source gas pulse input mode.
Fig. 3 is the electron-microscope scanning figure of the single-layer molybdenum disulfide film that this utility model embodiment obtains.
Fig. 4 is the Raman spectrogram of the single-layer molybdenum disulfide film that this utility model embodiment obtains.
Detailed description of the invention
In order to make the purpose of this utility model, feature and advantage more clear, below in conjunction with accompanying drawing and enforcement
Example, makes more detailed description to detailed description of the invention of the present utility model, in the following description, explains
State a lot of concrete details so that sufficiently understanding this utility model, but this utility model can be with very
Other modes being different from description are implemented more.Therefore, this utility model is not embodied as by following discloses
Restriction.
A kind of chemical vapor depsotition equipment based on air pulse growth molybdenum disulfide film, as it is shown in figure 1, institute
The equipment of stating includes supporting platform 1, quartz ampoule 3, No. two tubular heater thoraxes 4 of 2, tubular heater thorax, perseverance
Temperature bubbling bottle 5, gas handling system 6 and exhaust system 7；Described quartz ampoule 2 is fixed on support by supporting mechanism
On platform 1, a described tubular heater thorax 3 and No. two tubular heater thoraxes 4 pass through slide rail 8 along quartz ampoule 2 external diameter
Radially slide；Described quartz ampoule 2 two ends are set to inlet end 21 and outlet side 22, described inlet end 21 and going out
Gas end 22 is equipped with sealing flange；Described inlet end 21 connects gas handling system 6 and constant temperature drum by sealing flange 91
Bubble vial 5, described outlet side 22 connects exhaust system 7 by sealing flange 92.
Wherein, a described tubular heater thorax 3 is near inlet end 21, and No. two tubular heater thoraxes 4 are near going out
Gas end 22.
Wherein, described gas handling system 6 includes 61,2 gas mass flow controller 62,3/2 intake valves of gas cylinder
63 and 3 pneumatic operated valves 64,61,1 gas mass flow controller 621 of described gas cylinder and 1 pneumatic operated valve 641 lead to
Cross stainless steel tube 200 and connect quartz ampoule inlet end sealing flange 91；Described gas cylinder 61 and 1 gas mass flow
Controller 622 connects constant temperature bubbling bottle 5 by stainless steel tube 200；Described constant temperature bubbling bottle 5 connects 3/2 intake valve
63, connect quartz ampoule inlet end sealing flange 91, and and 1 with 1 pneumatic operated valve 642 by stainless steel tube 300
Individual pneumatic operated valve 643 is crossed stainless steel tube 300 and is connected to exhaust system 7.
Wherein, described exhaust system 7 includes that chamber pressure detector 71, chamber pressure control butterfly valve 72, pneumatic
Valve 73, manual ball valve 74, sulfur filter 75, molecular pump 76, mechanical pump 77 and exhaust gas processing device 78, institute
State chamber pressure detector 71 to be positioned on the sealing flange 92 of outlet side；Described chamber pressure control butterfly valve 72,
Pneumatic operated valve 73 and manual ball valve 74 connects sulfur filter 75 by stainless steel tube 300, described sulfur filter 75, point
Sub-pump 76, mechanical pump 77 are connected by stainless steel tube 200 with exhaust gas processing device 78.
Wherein, the outer layer of described stainless steel tube 300 uses heated at constant temperature band parcel.
Wherein, described chamber pressure controls butterfly valve 72, pneumatic operated valve 73 and manual ball valve 74 and uses heating clothing parcel,
Prevent tail gas condensing from blocking.
Wherein, described sealing flange uses circulating water.
Illustrate to utilize chemical gaseous phase described in the utility model with growth single-layer molybdenum disulfide film for embodiment
Depositing device prepares platelike molybdenumdisulfide thin film based on air pulse method:
1) the solid-state sulfur powder of 4N purity being placed in constant temperature bubbling bottle 5, the temperature of constant temperature bubbling bottle 5 sets
It it is 20 DEG C, the MoO of 4N purity3Utilize quartz boat to load and be placed on tubular heater thorax 3 flat-temperature zone,
The Sapphire Substrate that cleaning is completed is placed in tubular heater thorax 3 flat-temperature zone；The heating tape of Stainless Steel pipe 300
Temperature is set as 180 DEG C.
2) argon gas cylinder 61 and gas mass flow controller 621 and gas mass flow controller are opened
622, wherein, the flow of gas mass flow controller 621 is 100sccm (set point is 50-200sccm),
The flow of gas mass flow controller 622 is 50sccm (10-100sccm).Open mechanical pump 77.Open
Open manual ball valve 74 and make pneumatic operated valve 641,643 and 73 be closed, by controlling pneumatic operated valve 642
Opening and closing, remove the air of remaining in tube furnace.When in tube furnace, gas pressure reaches below 20Pa,
Open molecular pump, make pressure in tube furnace reach 10-3Below pa, closes manual ball valve 74.
3) open pneumatic operated valve 643, and make 3/2 intake valve 63 be in normally off, i.e. from constant temperature bubbling bottle 5
In gas out can flow to exhaust gas processing device 78 through pneumatic operated valve 643.Constant temperature bubbling bottle 5 temperature is set
Being 200 DEG C, heating rate is set as that 20 DEG C/min, tubular heater thorax 3 temperature are set as 600 DEG C,
Heating rate is set as that 50 DEG C/min, No. two tubular heater thorax 4 temperature are set as 760 DEG C, and heating rate sets
It is set to 50 DEG C/min.
4) when equal at 5, tubular heater thorax 3 of constant temperature bubbling bottle and No. two tubular heater thorax 4 temperature
When arriving setting value, open 3/2 intake valve 63, close pneumatic operated valve 643, and open simultaneously pneumatic operated valve 641,
642 and 73, sulfur steam and MoO3With the help of carrier gas, enter into reative cell and react and at sapphire
Nucleation and growth process on substrate.By butterfly valve 72 and the pressure in gas gauge linkage regulation reaction chamber, make reaction
Cavity pressure is constant is 10-3pa.Reaction t1After time (10s), close 3/2 intake valve 63, open pneumatic operated valve
643, and simultaneously close off pneumatic operated valve 641,642 and 73.t2After time (12s), open 3/2 intake valve 63,
Close pneumatic operated valve 643, and open pneumatic operated valve 641,642 and 73 simultaneously.As in figure 2 it is shown, the rest may be inferred,
After reacting 95 pulses, close 3/2 intake valve 63, open pneumatic operated valve 643, and simultaneously close off pneumatic operated valve 641,
642 and 73.
5) close the temperature of constant temperature bubbling bottle 5, close a tubular heater thorax 3 and No. two tubular heaters
Thorax 4, and open bell, allow it cool down rapidly.Close molecular pump, mechanical pump successively.Treat that tube furnace temperature is cold
But to after room temperature, opening pneumatic operated valve 642, after intraductal pressure returns to normal pressure, uncap, taking-up grown
MoS2The sample of thin film.
Being characterized by the molybdenum disulfide film sample obtained, Fig. 2 is the electron-microscope scanning figure of this sample, such as figure
Shown in, the molybdenum bisuphide regular shape on substrate, surfacing；Fig. 3 is the Raman spectrogram of this sample,
As it can be seen, two main raman characteristic peaks of molybdenum disulfide film be spaced in 20cm-1Left and right, shows made
Standby sample is the molybdenum disulfide film of monolayer.
The foregoing is only preferred embodiment of the present utility model, not in order to limit this utility model,
All any amendment, equivalent and improvement etc. made within spirit of the present utility model and principle, all should
Within being included in protection domain of the present utility model.
Claims (7)
1. a chemical vapor depsotition equipment based on air pulse growth molybdenum disulfide film, it is characterised in that: described equipment includes supporting platform, quartz ampoule, tubular heater thorax, No. two tubular heater thoraxes, constant temperature bubbling bottle, gas handling system and exhaust system；Described quartz ampoule is fixed on support platform by supporting mechanism, and a described tubular heater thorax and No. two tubular heater thoraxes are radially slided along quartz ampoule external diameter by slide rail；Described quartz ampoule two ends are set to inlet end and outlet side, and described inlet end and outlet side are equipped with sealing flange；Described inlet end connects gas handling system and constant temperature bubbling bottle by sealing flange, and described outlet side connects exhaust system by sealing flange.
A kind of chemical vapor depsotition equipment based on air pulse growth molybdenum disulfide film the most according to claim 1, it is characterised in that: a described tubular heater thorax is near inlet end, and No. two tubular heater thoraxes are near outlet side.
A kind of chemical vapor depsotition equipment based on air pulse growth molybdenum disulfide film the most according to claim 1, it is characterized in that: described gas handling system includes that gas cylinder, 2 gas mass flow controllers, 3/2 intake valve and 3 pneumatic operated valves, described gas cylinder, 1 gas mass flow controller and 1 pneumatic operated valve connect quartz ampoule inlet end sealing flange by stainless steel tube 200；Described gas cylinder and 1 gas mass flow controller connect constant temperature bubbling bottle by stainless steel tube 200；Described constant temperature bubbling bottle connects 3/2 intake valve, connects quartz ampoule inlet end sealing flange with 1 pneumatic operated valve by stainless steel tube 300, and and 1 pneumatic operated valve cross stainless steel tube 300 and be connected to exhaust system.
A kind of chemical vapor depsotition equipment based on air pulse growth molybdenum disulfide film the most according to claim 1, it is characterized in that: described exhaust system includes that chamber pressure detector, chamber pressure control butterfly valve, pneumatic operated valve, manual ball valve, sulfur filter, molecular pump, mechanical pump and exhaust gas processing device, and described chamber pressure detector is positioned on the sealing flange of outlet side；Described chamber pressure control butterfly valve, pneumatic operated valve and manual ball valve are connected sulfur filter, described sulfur filter, molecular pump, mechanical pump and exhaust gas processing device by stainless steel tube 300 and are connected by stainless steel tube 200.
5. according to a kind of based on air pulse growth molybdenum disulfide film the chemical vapor depsotition equipment described in claim 3 or 4, it is characterised in that: the outer layer of described stainless steel tube 300 uses heated at constant temperature band parcel.
A kind of chemical vapor depsotition equipment based on air pulse growth molybdenum disulfide film the most according to claim 4, it is characterised in that: described chamber pressure controls butterfly valve, pneumatic operated valve and manual ball valve and uses heating clothing parcel, prevents tail gas condensing from blocking.
A kind of chemical vapor depsotition equipment based on air pulse growth molybdenum disulfide film the most according to claim 1, it is characterised in that: described sealing flange uses circulating water.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620184845.5U CN205473973U (en) | 2016-03-09 | 2016-03-09 | Chemical vapor deposition equipment based on pulsating gas flow growth molybdenum disulfide film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620184845.5U CN205473973U (en) | 2016-03-09 | 2016-03-09 | Chemical vapor deposition equipment based on pulsating gas flow growth molybdenum disulfide film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108130524A (en) * | 2017-12-22 | 2018-06-08 | 中国科学院电工研究所 | The method of plasma jet thin film deposition device and aufhellung surface trap energy level |
| CN108151529A (en) * | 2017-12-22 | 2018-06-12 | 合肥费舍罗热工装备有限公司 | A kind of dual temperature area open-type sliding rail stove |
| CN110079792A (en) * | 2019-05-29 | 2019-08-02 | 无锡盈芯半导体科技有限公司 | Bilateral symmetry formula CVD system |
-
2016
- 2016-03-09 CN CN201620184845.5U patent/CN205473973U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108130524A (en) * | 2017-12-22 | 2018-06-08 | 中国科学院电工研究所 | The method of plasma jet thin film deposition device and aufhellung surface trap energy level |
| CN108151529A (en) * | 2017-12-22 | 2018-06-12 | 合肥费舍罗热工装备有限公司 | A kind of dual temperature area open-type sliding rail stove |
| CN110079792A (en) * | 2019-05-29 | 2019-08-02 | 无锡盈芯半导体科技有限公司 | Bilateral symmetry formula CVD system |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160817 Termination date: 20200309 |