CN105734528A - Growth method for layered molybdenum disulfide films on basis of pulse airflow method - Google Patents
Growth method for layered molybdenum disulfide films on basis of pulse airflow method Download PDFInfo
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- CN105734528A CN105734528A CN201610133290.6A CN201610133290A CN105734528A CN 105734528 A CN105734528 A CN 105734528A CN 201610133290 A CN201610133290 A CN 201610133290A CN 105734528 A CN105734528 A CN 105734528A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
Abstract
The invention discloses a growth method for layered molybdenum disulfide films on the basis of the pulse airflow method. The growth method comprises the steps of 1, placing a substrate into a PEMOCVD reaction chamber, guiding argon gas into the reaction chamber for removing air in the reaction chamber and adjusting the vacuum degree of the reaction chamber to be lower than 10-3 Pa, wherein the temperature ranges from 700 DEG C to 800 DEG C and the heating rate ranges from 40 DEG C/min to 60 DEG C/min; 2, adopting the argon gas as a carrier, heating and evaporating molybdenum oxide powder and sulfur powder for forming reaction source gas, guiding the reaction source gas into the PEMOCVD reaction chamber in a pulse mode for being nucleated and growing on the substrate and obtaining the molybdenum disulfide films with specific layers by controlling the input flow of the reaction source gas and the pulse input mode. According to the growth method, the high-quality and large-size molybdenum disulfide films with the number of layers controllable can be obtained by controlling the input flow of the reaction source gas and the pulse input mode.
Description
Technical field
The present invention relates to the preparing technical field of molybdenum disulfide film, be related specifically to a kind of based on pulse air
The method of stream method growth stratiform 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.That the most stably repeats prepares high-quality large scale stratiform MoS on a large scale2It is to realize it
One of major issue of potential application.
Summary of the invention
It is an object of the invention to provide a kind of side based on air pulse method growth stratiform molybdenum disulfide film
Method, by input flow rate and the pulse input mode of reaction source gas, can obtain high-quality and the number of plies is controlled
Large scale molybdenum disulfide film.
To this end, the present invention is by the following technical solutions:
A kind of method based on air pulse method growth stratiform molybdenum disulfide film, comprises the steps:
1) substrate is placed in PEMOCVD reative cell, is passed through argon and removes the air in reative cell, regulation
Reative cell vacuum is below 10-3Pa, and temperature is 700 DEG C～800 DEG C, and heating rate is 40～60 DEG C/min；
2) with argon as carrier, it is reaction source gas by molybdenum oxide powder and sulfur powder heating evaporation respectively, arteries and veins
The formula of punching is passed into nucleation growth on substrate in PEMOCVD reative cell, by controlling the input of reaction source gas
Flow and pulse input mode, it is thus achieved that the molybdenum disulfide film of the specific number of plies.
Preferably, described substrate is the sapphire through cleaning treatment, quartz or silicon.
Preferably, the temperature of described molybdenum oxide powder heating evaporation is 550 DEG C～650 DEG C, and heating rate is
40～60 DEG C/min；The temperature of described sulfur powder heating evaporation is 150 DEG C～250 DEG C, and heating rate is 15～25 DEG C
/min。
Preferably, the input flow rate of described molybdenum oxide reaction source gas is 10～100sccm；Described reaction of Salmon-Saxl source
The input flow rate of gas is 50～200sccm.
Preferably, described molybdenum oxide and reaction of Salmon-Saxl source gas pulses interval are input in PEMOCVD reative cell,
Its mode is:
t1In=10s, molybdenum oxide and reaction of Salmon-Saxl source gas pulses are closed；
t2In=12s, molybdenum oxide and reaction of Salmon-Saxl source gas pulses are opened；
t1-t2It is a pulse period, becomes with reaction of Salmon-Saxl source gas nucleation on substrate at pulse period internal oxidition molybdenum
Long, repeat the pulse period of certain number of times, it is thus achieved that the molybdenum disulfide film of the specific number of plies.
Preferably, the number of times in described repetition pulse cycle is 80～300 times, and the molybdenum bisuphide i.e. obtaining 1～3 layer is thin
Film.
Preferably, described molybdenum oxide reaction source gas pulse persistance is input in PEMOCVD reative cell；Described
Reaction of Salmon-Saxl source channel interval is input in PEMOCVD reative cell, and its mode is:
t1In=20s, reaction of Salmon-Saxl source gas pulses is closed；
t2In=5s, reaction of Salmon-Saxl source gas pulses is opened；
t3In=20s, reaction of Salmon-Saxl source gas pulses is closed；
t4In=20s, reaction of Salmon-Saxl source gas pulses is opened；
t1-t4It is a pulse period, becomes with reaction of Salmon-Saxl source gas nucleation on substrate at pulse period internal oxidition molybdenum
Long, repeat the pulse period of certain number of times, it is thus achieved that the molybdenum disulfide film of the specific number of plies.
Preferably, the number of times in described repetition pulse cycle is 30～150 times, and the molybdenum bisuphide i.e. obtaining 1～3 layer is thin
Film.
Preferably, described method also includes the molybdenum disulfide film obtained on substrate in the reactor chamber to be less than
The speed of 10 DEG C/min is taken out after being cooled to room temperature.
The present invention uses above technical scheme, by accurately controlling input flow rate and the pulse of reaction source gas
Input mode, regulation and control molybdenum disulfide film nucleation and the speed of growth, it is possible to obtain tactical rule, surface is put down
Whole high-quality large-sized platelike molybdenumdisulfide thin film.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the embodiment of the present invention one reaction source gas pulse input mode.
Fig. 2 is that the Electronic Speculum of the single-layer molybdenum disulfide film that the present invention grows based on embodiment one air pulse method is swept
Tracing.
Fig. 3 is the Raman light of the single-layer molybdenum disulfide film that the present invention grows based on embodiment one air pulse method
Spectrogram.
Fig. 4 is the schematic diagram of the embodiment of the present invention two reaction source gas pulse input mode.
Detailed description of the invention
In order to make objects, features and advantages of the present invention more clear, below in conjunction with drawings and Examples,
The detailed description of the invention of the present invention is made more detailed description, in the following description, elaborates a lot
Concrete details is so that sufficiently understanding the present invention, but the present invention can be to be much different from its of description
He implements mode.Therefore, the present invention not by following discloses be embodied as limited.
Embodiment one
A kind of method based on air pulse method growth stratiform molybdenum disulfide film, comprises the steps:
1) substrate is placed in PEMOCVD reative cell, is passed through argon and removes the air in reative cell, regulation
Reative cell vacuum is below 10-3Pa, and temperature is 700 DEG C～800 DEG C, and heating rate is 40～60 DEG C/min；
2) with argon as carrier, it is reaction source gas by molybdenum oxide powder and sulfur powder heating evaporation respectively, arteries and veins
The formula of punching is passed into nucleation growth on substrate in PEMOCVD reative cell, by controlling the input of reaction source gas
Flow and pulse input mode, it is thus achieved that the molybdenum disulfide film of the specific number of plies.
Wherein, described substrate is the sapphire through cleaning treatment, quartz or silicon.
Wherein, the temperature of described molybdenum oxide powder heating evaporation is 550 DEG C～650 DEG C, and heating rate is
40～60 DEG C/min；The temperature of described sulfur powder heating evaporation is 150 DEG C～250 DEG C, and heating rate is 15～25 DEG C
/min。
Wherein, the input flow rate of described molybdenum oxide reaction source gas is 10～100sccm；Described reaction of Salmon-Saxl source gas
The input flow rate of body is 50～200sccm.
Wherein, described molybdenum oxide and reaction of Salmon-Saxl source gas pulses interval are input in PEMOCVD reative cell, its
Mode as it is shown in figure 1,
t1In=10s, molybdenum oxide and reaction of Salmon-Saxl source gas pulses are closed；
t2In=12s, molybdenum oxide and reaction of Salmon-Saxl source gas pulses are opened；
t1-t2It is a pulse period, becomes with reaction of Salmon-Saxl source gas nucleation on substrate at pulse period internal oxidition molybdenum
Long, repeat the pulse period of certain number of times, it is thus achieved that the molybdenum disulfide film of the specific number of plies.
Wherein, the number of times in described repetition pulse cycle is 80～300 times, i.e. obtains the molybdenum disulfide film of 1～3 layer.
Wherein, described method also includes the molybdenum disulfide film obtained on substrate in the reactor chamber to be less than
The speed of 10 DEG C/min is taken out after being cooled to room temperature.
Growing single-layer molybdenum disulfide film based on said method, selection sapphire is substrate, described molybdenum oxide powder
The temperature of end heating evaporation is 600 DEG C, and heating rate is 50 DEG C/min；The temperature of described sulfur powder heating evaporation
Being 200 DEG C, heating rate is 20 DEG C/min；Vacuum in described PEMOCVD reative cell is 10-3Below Pa,
Temperature is 760 DEG C, and heating rate is 50 DEG C/min.Set the input flow rate of molybdenum oxide reaction source gas as
50sccm；The input flow rate of described reaction of Salmon-Saxl source gas is 100sccm, repetition pulse cycle times 95 times,
To single-layer molybdenum disulfide film sample.Being characterized by the molybdenum disulfide film sample obtained, Fig. 2 is this sample
Electron-microscope scanning figure, as it can be seen, the molybdenum bisuphide regular shape on substrate, surfacing；Fig. 3 is for being somebody's turn to do
The Raman spectrogram of sample, as it can be seen, being spaced in of two main raman characteristic peaks of molybdenum disulfide film
20cm-1Left and right, shows the molybdenum disulfide film that prepared sample is monolayer.
Embodiment two
A kind of method based on air pulse method growth stratiform molybdenum disulfide film, comprises the steps:
1) substrate is placed in PEMOCVD reative cell, is passed through argon and removes the air in reative cell, regulation
Reative cell vacuum is below 10-3Pa, and temperature is 700 DEG C～800 DEG C, and heating rate is 40～60 DEG C/min；
2) with argon as carrier, it is reaction source gas by molybdenum oxide powder and sulfur powder heating evaporation respectively, arteries and veins
The formula of punching is passed into nucleation growth on substrate in PEMOCVD reative cell, by controlling the input of reaction source gas
Flow and pulse input mode, it is thus achieved that the molybdenum disulfide film of the specific number of plies.
Wherein, described substrate is the sapphire through cleaning treatment, quartz or silicon.
Wherein, the temperature of described molybdenum oxide powder heating evaporation is 550 DEG C～650 DEG C, and heating rate is
40～60 DEG C/min；The temperature of described sulfur powder heating evaporation is 150 DEG C～250 DEG C, and heating rate is 15～25 DEG C
/min。
Wherein, the input flow rate of described molybdenum oxide reaction source gas is 10～100sccm；Described reaction of Salmon-Saxl source gas
The input flow rate of body is 50～200sccm.
Wherein, the most described molybdenum oxide reaction source gas pulse persistance is input to PEMOCVD reative cell
In；Described reaction of Salmon-Saxl source channel interval is input in PEMOCVD reative cell, and its mode is:
t1In=20s, reaction of Salmon-Saxl source gas pulses is closed；
t2In=5s, reaction of Salmon-Saxl source gas pulses is opened；
t3In=20s, reaction of Salmon-Saxl source gas pulses is closed；
t4In=20s, reaction of Salmon-Saxl source gas pulses is opened；
t1-t4It is a pulse period, becomes with reaction of Salmon-Saxl source gas nucleation on substrate at pulse period internal oxidition molybdenum
Long, repeat the pulse period of certain number of times, it is thus achieved that the molybdenum disulfide film of the specific number of plies.
Wherein, the number of times in described repetition pulse cycle is 30～150 times, i.e. obtains the molybdenum disulfide film of 1～3 layer.
Wherein, described method also includes the molybdenum disulfide film obtained on substrate in the reactor chamber to be less than
The speed of 10 DEG C/min is taken out after being cooled to room temperature.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this
Any amendment, equivalent and the improvement etc. made within bright spirit and principle, should be included in the present invention
Protection domain within.
Claims (9)
1. a method based on air pulse method growth stratiform molybdenum disulfide film, it is characterised in that include
Following steps:
1) substrate is placed in PEMOCVD reative cell, is passed through argon and removes the air in reative cell, regulation
Reative cell vacuum is 10-3Below Pa, temperature is 700 DEG C～800 DEG C, and heating rate is 40～60 DEG C/min；
2) with argon as carrier, it is reaction source gas by molybdenum oxide powder and sulfur powder heating evaporation respectively, arteries and veins
The formula of punching is passed into nucleation growth on substrate in PEMOCVD reative cell, by controlling the defeated of reaction source gas
Inbound traffics and pulse input mode, it is thus achieved that the molybdenum disulfide film of the specific number of plies.
A kind of side based on air pulse method growth stratiform molybdenum disulfide film the most according to claim 1
Method, it is characterised in that described substrate is the sapphire through cleaning treatment, quartz or silicon.
A kind of side based on air pulse method growth stratiform molybdenum disulfide film the most according to claim 1
Method, it is characterised in that the temperature of described molybdenum oxide powder heating evaporation is 550 DEG C～650 DEG C, heating rate
It is 40～60 DEG C/min；The temperature of described sulfur powder heating evaporation is 150 DEG C～250 DEG C, and heating rate is
15～25 DEG C/min.
A kind of side based on air pulse method growth stratiform molybdenum disulfide film the most according to claim 1
Method, it is characterised in that the input flow rate of described molybdenum oxide reaction source gas is 10～100sccm；Described sulfur is anti-
The input flow rate answering source gas is 50～200sccm.
A kind of side based on air pulse method growth stratiform molybdenum disulfide film the most according to claim 1
Method, it is characterised in that described molybdenum oxide and reaction of Salmon-Saxl source gas pulses interval are input to PEMOCVD reaction
In room, its mode is:
t1In=10s, molybdenum oxide and reaction of Salmon-Saxl source gas pulses are closed；
t2In=12s, molybdenum oxide and reaction of Salmon-Saxl source gas pulses are opened；
t1-t2It is a pulse period, becomes with reaction of Salmon-Saxl source gas nucleation on substrate at pulse period internal oxidition molybdenum
Long, repeat the pulse period of certain number of times, it is thus achieved that the molybdenum disulfide film of the specific number of plies.
A kind of side based on air pulse method growth stratiform molybdenum disulfide film the most according to claim 5
Method, it is characterised in that the number of times in described repetition pulse cycle is 80～300 times, i.e. obtains two sulfur of 1～3 layer
Change molybdenum film.
A kind of side based on air pulse method growth stratiform molybdenum disulfide film the most according to claim 1
Method, it is characterised in that described molybdenum oxide reaction source gas pulse persistance is input in PEMOCVD reative cell；
Described reaction of Salmon-Saxl source channel interval is input in PEMOCVD reative cell, and its mode is:
t1In=20s, reaction of Salmon-Saxl source gas pulses is closed；
t2In=5s, reaction of Salmon-Saxl source gas pulses is opened；
t3In=20s, reaction of Salmon-Saxl source gas pulses is closed；
t4In=20s, reaction of Salmon-Saxl source gas pulses is opened；
t1-t4It is a pulse period, becomes with reaction of Salmon-Saxl source gas nucleation on substrate at pulse period internal oxidition molybdenum
Long, repeat the pulse period of certain number of times, it is thus achieved that the molybdenum disulfide film of the specific number of plies.
A kind of side based on air pulse method growth stratiform molybdenum disulfide film the most according to claim 7
Method, it is characterised in that the number of times in described repetition pulse cycle is 30～150 times, i.e. obtains two sulfur of 1～3 layer
Change molybdenum film.
A kind of side based on air pulse method growth stratiform molybdenum disulfide film the most according to claim 1
Method, it is characterised in that described method also include by the molybdenum disulfide film that obtains on substrate in the reactor chamber with
Speed less than 10 DEG C/min is taken out after being cooled to room temperature.
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| CN106238077A (en) * | 2016-07-28 | 2016-12-21 | 中国地质大学（北京） | A kind of carbon fiber@molybdenum disulfide nano sheet core-shell structure and preparation method thereof |
| CN110863189A (en) * | 2019-11-11 | 2020-03-06 | 中国科学院上海技术物理研究所 | Method for growing single-layer telluride doped structure by pulse type injection of reactant |
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