CN107338422A - A kind of method of ald molybdenum disulfide film - Google Patents
A kind of method of ald molybdenum disulfide film Download PDFInfo
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- CN107338422A CN107338422A CN201710497160.5A CN201710497160A CN107338422A CN 107338422 A CN107338422 A CN 107338422A CN 201710497160 A CN201710497160 A CN 201710497160A CN 107338422 A CN107338422 A CN 107338422A
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- molybdenum
- molybdenum disulfide
- disulfide film
- ald
- preset time
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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
-
- 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
- C23C16/45525—Atomic layer deposition [ALD]
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The present invention relates to a kind of method of ald molybdenum disulfide film, comprise the following steps：Molybdenum source is loaded into source bottle and heated, heating is placed with the reaction chamber of substrate sample；Molybdenum source is blown into reaction chamber using carrier gas, makes molybdenum source occur, from limitation chemisorbed, after molybdenum source is blown into end, to continue to be passed through carrier gas, byproduct of reaction and remaining molybdenum source are rinsed out with substrate sample surface；Hydrogen sulfide is blown into reaction chamber using carrier gas, makes hydrogen sulfide and molybdenum source occur to chemically react from limitation, in substrate sample Surface Creation molybdenum disulfide film, after hydrogen sulfide is blown into end, continues to be passed through carrier gas rinsing out byproduct of reaction and remaining hydrogen sulfide.Molybdenum disulfide film uniform quality prepared by the present invention, surfacing, thickness can be controlled accurately.
Description
Technical field
The present invention relates to technique for atomic layer deposition field, and in particular to a kind of preparation method of molybdenum disulfide film.
Background technology
In recent years, as a kind of molybdenum disulfide (MoS of stratiform transient metal sulfide2), due to excellent machinery,
Electricity, optics and catalytic performance and cause extensive concern, it rubs in hydrodesulfurization catalytic, photovoltaic cell, photocatalysis, nanometer
The fields such as wiping, lithium battery and dry lubrication cause one research boom.The common structure type of molybdenum disulfide has three kinds：1T shapes,
2H shapes, 3R shapes.Natural 2H-MoS2Crystal is that the distance between typical layer structure, molecular layer is 1.23nm, each point
The thickness of sublayer is 0.625nm.Each molybdenum disulfide molecular layer is divided into 3 atomic layers again, and middle one layer is molybdenum atom, up and down
Two layers is sulphur atom, and each molybdenum atom is surrounded by 6 sulphur atoms.Inside molecular layer, sulphur and molybdenum atom are with stable change
Learn key to be combined, be combined between molecular layer with very weak Van der Waals force.When by shearing force, easily formed between layers
Slide surface, the sliding can effectively reduce coefficient of friction, reduce the abrasion of material.Molybdenum disulfide is that a kind of performance relies on the number of plies
Semi-conducting material, when the number of plies is changed into individual layer from multilayer, it is changed into 1.9eV direct band from 1.2eV indirect band-gap semiconductor
Gap semiconductor, greatly increase luminous efficiency, molybdenum disulfide has caused widely in the potential application of field of optoelectronic devices
Pay attention to.
The method of generally use mechanical stripping prepares platelike molybdenumdisulfide film, and molybdenum disulfide prepared by this method has
Perfect crystal structure.But molybdenum disulfide film size prepared by this method is smaller, and efficiency is very low.Due to size
With the limitation of efficiency, the method that mechanical stripping prepares molybdenum disulfide film can not on a large scale should in fields such as IC manufacturings
With.Artificial synthesized growing large-area, the molybdenum disulfide film of high quality seem particularly urgent.Based on existing semi-conductor industry skill
Art, the method for the artificial synthesized molybdenum disulfide that research is more popular is chemical vapour deposition technique (CVD).This method is by molybdenum
Source (MoO3Or MoCl5) and sulphur source (S powder) heating, its is produced corresponding gas precursor, then by inert gas (Ar or
N2) they are transported to substrate proximity, required molybdenum disulfide film is generated on substrate.Although this method can obtain big face
Product, the molybdenum disulfide of high quality, but it there are the place of deficiency：(1) temperature of synthesis growth it is higher, it is necessary to 650 DEG C-
1000 DEG C, which has limited the application on non-refractory substrate；(2) because growth course is continuous, the thickness of film is made not
Easily accurate control；(3) for the structure of some high-aspect-ratios, such as hole and groove, CVD method can not depositing homogeneous film,
Material can be deposited on open edge.
Atom layer deposition process (ALD) is by certainly limitation chemical reaction deposit film of the presoma on substrate sample surface.
By being alternately passed through presoma pulse, ald can in the structure of high-aspect-ratio uniform deposition film, and film
Thickness can accurately be controlled by controlling cycle-index.Because depositing temperature is relatively low, the heat-resisting quantity of substrate will not
Ask, this method can be widely used.
The content of the invention
Technical problem：It is an object of the invention to provide a kind of preparation method of molybdenum disulfide film, pass through atomic layer deposition
Molybdenum disulfide film material prepared by area method, having the advantages that large area, thickness be controllable, uniform quality, this method is simple to operate,
It is adapted to automation, large-scale production.
Technical scheme：A kind of method of ald molybdenum disulfide film of the present invention comprises the following steps：
Molybdenum source is loaded source bottle by step 1, is heated to the first preset temperature and is remained to the first preset time, will be equipped with base
The reaction chamber of original pattern product is heated to the second preset temperature and remains to the second preset time；
Molybdenum source is sent into reaction chamber by step 2 using carrier gas, and the time terminated from be first introduced into being sent into is maintained at the 3rd
Preset time, molybdenum source is set to occur, from limitation chemisorbed, after molybdenum source steam feeding terminates, to continue to be passed through load with substrate sample surface
Gas simultaneously remains to the 4th preset time, and byproduct of reaction and remaining molybdenum source are rinsed well；
Hydrogen sulfide is sent into reaction chamber by step 3 using carrier gas, and the time terminated from be first introduced into being sent into is maintained at the
Five preset times, make hydrogen sulfide occur to chemically react from limitation with molybdenum source, molybdenum disulfide film is generated in substrate sample, vulcanize
After hydrogen is blown into end, continues to be passed through carrier gas and remain to the 6th preset time, byproduct of reaction and remaining hydrogen sulfide are rinsed out.
Wherein：
First preset temperature is 50~250 DEG C；Second preset temperature is 200~500 DEG C.
First preset time is 1~120min.
Second preset time is 1~120min.
3rd preset time is 0.1~300s.
4th preset time is 1~500s.
5th preset time is 0.1~300s.
6th preset time is 1~500s.
The molybdenum source is molybdenum pentachloride or hexacarbonylmolybdenum, the substrate sample be metal, sapphire, carborundum, silicon nitride,
Silicon, mica, quartz or silica.
The carrier gas is nitrogen or argon gas, and carrier gas flux is 10~500mL/min.
Two are contained in the preparation method from limitation chemical reaction, they form a complete circulation, pass through control
The number of cycles is made, the thickness of grown molybdenum disulfide film can be accurately controlled.
Beneficial effect：Using the method for the invention, the molybdenum disulfide film of growth has a uniform quality, surfacing,
The advantages that thickness can be controlled accurately.
Preparation method of the present invention is easy to operate, and the film quality grown is uniform, reproducible, for the substrate of labyrinth
It can grow, be adapted to extensive prepare and produce molybdenum disulfide film.
Brief description of the drawings
Fig. 1 is the schematic diagram that the present invention prepares molybdenum disulfide film using atomic layer deposition apparatus.Related mark name in Fig. 1
Claim as follows：1. vavuum pump；2. reaction cavity；3. cavity heater strip；4. substrate sample to be deposited；5.V2Pneumatic operated valve；6.H2S sources bottle；
7.MoCl5Source bottle heater strip；8.MoCl5Source bottle；9.V1Pneumatic operated valve；10. anti-suck bottle；11.NaOH solution；12.CuSO4Solution.
Fig. 2 is the SEM figures for the molybdenum disulfide film that the inventive method is prepared, and can be seen that what is grown from photo
Molybdenum disulfide film surfacing, uniformly.
Fig. 3 is the Raman spectrogram for the molybdenum disulfide film that the inventive method is prepared, as we can clearly see from the figure
Two characteristic peak 383cm of molybdenum disulfide film-1And 408cm-1。
Fig. 4 is the TEM figures for the molybdenum disulfide film that the inventive method is prepared, it can clearly be seen that two sulphur from photo
Change the layer structure of molybdenum.
Embodiment
The specific embodiment of the present invention is given below, the example of the embodiment is shown in the drawings, and the embodiment is
Further explanation to the present invention, rather than limitation the scope of the present invention.
The preparation method of molybdenum disulfide film according to embodiments of the present invention, as shown in figure 1, may comprise steps of：
Step S1. passes through MoCl5Source bottle heater strip 7, by MoCl5Source bottle 8 be heated to 50 DEG C~250 DEG C and keep 1~
120min, by cavity heater strip 3, the reaction cavity 2 for being placed with substrate sample 4 to be deposited is heated to 200~500 DEG C and protected
Hold 1~120min；
Step S2. opens V1Pneumatic operated valve 9, carrier gas N2By MoCl5It is sent into reaction cavity 2, MoCl5Deposited by chemisorbed
On the surface of substrate sample 4 to be deposited, V is closed1Pneumatic operated valve 9, V1Time of the pneumatic operated valve 9 from opening closing is 0.1~300s, after
It is continuous to be passed through carrier gas N2And 1~500s is kept, by MoCl remaining in reaction cavity 25Rinsed well with byproduct of reaction；
Step S3. opens V2Pneumatic operated valve 5, carrier gas N2By H2S is sent into reaction cavity 2, H2S is deposited on by chemisorbed
MoCl5Surface simultaneously reacts generation MoS2, close V2Pneumatic operated valve 5, V2Time of the pneumatic operated valve 5 from opening closing for 0.1~
300s, continue to be passed through carrier gas N2And 1~500s is kept, by H remaining in reaction cavity 22S and byproduct of reaction are rinsed well.
Step S2 and S3 contain two from limitation chemical reaction, and they form a complete circulation, should by control
Number of cycles, grown MoS can be accurately controlled2The thickness of film, obtain uniform quality, the MoS of surfacing2Film.
Anti-suck bottle 10, NaOH solution 11 and CuSO4Solution 12 is used for the H for cleaning remnants2S。
Claims (10)
- A kind of 1. method of ald molybdenum disulfide film, it is characterised in that this method comprises the following steps：Molybdenum source is loaded source bottle by step 1, is heated to the first preset temperature and is remained to the first preset time, will be equipped with substrate sample The reaction chamber of product is heated to the second preset temperature and remains to the second preset time；Molybdenum source is sent into reaction chamber by step 2 using carrier gas, and it is default that the time terminated from be first introduced into being sent into is maintained at the 3rd Time, molybdenum source is set to occur, from limitation chemisorbed, after molybdenum source steam feeding terminates, to continue to be passed through carrier gas simultaneously with substrate sample surface The 4th preset time is remained to, byproduct of reaction and remaining molybdenum source are rinsed well；Hydrogen sulfide is sent into reaction chamber by step 3 using carrier gas, and it is pre- that the time terminated from be first introduced into being sent into is maintained at the 5th If the time, make hydrogen sulfide occur to chemically react from limitation with molybdenum source, molybdenum disulfide film is generated in substrate sample, hydrogen sulfide blows After entering end, continue to be passed through carrier gas and remain to the 6th preset time, byproduct of reaction and remaining hydrogen sulfide are rinsed out.
- 2. the method for ald molybdenum disulfide film according to claim 1, it is characterised in that described first is default Temperature is 50~250 DEG C；Second preset temperature is 200~500 DEG C.
- 3. the method for ald molybdenum disulfide film according to claim 1 or 2, it is characterised in that described first Preset time is 1~120min.
- 4. the method for ald molybdenum disulfide film according to claim 1 or 2, it is characterised in that described second Preset time is 1~120min.
- 5. the method for ald molybdenum disulfide film according to claim 1 or 2, it is characterised in that the described 3rd Preset time is 0.1~300s.
- 6. the method for ald molybdenum disulfide film according to claim 1 or 2, it is characterised in that the described 4th Preset time is 1~500s.
- 7. the method for ald molybdenum disulfide film according to claim 1 or 2, it is characterised in that the described 5th Preset time is 0.1~300s.
- 8. the method for ald molybdenum disulfide film according to claim 1 or 2, it is characterised in that the described 6th Preset time is 1~500s.
- 9. the method for ald molybdenum disulfide film according to claim 1 or 2, it is characterised in that the molybdenum source It is molybdenum pentachloride or hexacarbonylmolybdenum, the substrate sample is metal, sapphire, carborundum, silicon nitride, silicon, mica, quartz or oxygen SiClx.
- 10. the method for ald molybdenum disulfide film according to claim 1 or 2, it is characterised in that the carrier gas It is nitrogen or argon gas, carrier gas flux is 10~500mL/min.
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| CN201710497160.5A CN107338422A (en) | 2017-06-26 | 2017-06-26 | A kind of method of ald molybdenum disulfide film |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059189A (en) * | 2017-12-26 | 2018-05-22 | 佛山科学技术学院 | A kind of preparation method of molybdenum disulfide nano tube |
| CN108365012A (en) * | 2018-01-23 | 2018-08-03 | 东南大学 | A method of molybdenum disulfide field-effect tube is prepared based on atomic layer deposition |
| CN109136984A (en) * | 2018-09-30 | 2019-01-04 | 东南大学 | A kind of three-dimensional composite catalyst Au NPs/MoS for efficient liberation of hydrogen2/ CFP and preparation method thereof |
| CN109487231A (en) * | 2018-12-30 | 2019-03-19 | 金堆城钼业股份有限公司 | A kind of device and method preparing triangle molybdenum disulfide film |
| CN108165938B (en) * | 2017-12-20 | 2019-12-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of hetero-junctions photochemistry array and products thereof and application |
| CN111943270A (en) * | 2020-08-21 | 2020-11-17 | 南京工程学院 | Equipment and process method for manufacturing molybdenum disulfide quantum dot array |
| CN111979526A (en) * | 2020-08-21 | 2020-11-24 | 南京工程学院 | Method and equipment for manufacturing zinc sulfide, lead sulfide and cadmium sulfide quantum dots |
| CN112607778A (en) * | 2020-12-31 | 2021-04-06 | 东南大学 | Preparation method of molybdenum disulfide nanotube and molybdenum disulfide nanotube |
| CN113774356A (en) * | 2021-09-15 | 2021-12-10 | 复旦大学 | Wafer-level two-dimensional material growth method |
| CN114318288A (en) * | 2020-10-09 | 2022-04-12 | 昆山微电子技术研究院 | Atomic layer deposition preparation method of high-quality molybdenum disulfide film |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108165938B (en) * | 2017-12-20 | 2019-12-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of hetero-junctions photochemistry array and products thereof and application |
| CN108059189A (en) * | 2017-12-26 | 2018-05-22 | 佛山科学技术学院 | A kind of preparation method of molybdenum disulfide nano tube |
| CN108365012A (en) * | 2018-01-23 | 2018-08-03 | 东南大学 | A method of molybdenum disulfide field-effect tube is prepared based on atomic layer deposition |
| CN109136984A (en) * | 2018-09-30 | 2019-01-04 | 东南大学 | A kind of three-dimensional composite catalyst Au NPs/MoS for efficient liberation of hydrogen2/ CFP and preparation method thereof |
| CN109487231A (en) * | 2018-12-30 | 2019-03-19 | 金堆城钼业股份有限公司 | A kind of device and method preparing triangle molybdenum disulfide film |
| CN109487231B (en) * | 2018-12-30 | 2023-08-22 | 金堆城钼业股份有限公司 | Device and method for preparing triangular molybdenum disulfide film |
| CN111943270A (en) * | 2020-08-21 | 2020-11-17 | 南京工程学院 | Equipment and process method for manufacturing molybdenum disulfide quantum dot array |
| CN111979526A (en) * | 2020-08-21 | 2020-11-24 | 南京工程学院 | Method and equipment for manufacturing zinc sulfide, lead sulfide and cadmium sulfide quantum dots |
| CN111943270B (en) * | 2020-08-21 | 2023-04-25 | 南京工程学院 | Equipment and process method for manufacturing molybdenum disulfide quantum dot array |
| CN114318288A (en) * | 2020-10-09 | 2022-04-12 | 昆山微电子技术研究院 | Atomic layer deposition preparation method of high-quality molybdenum disulfide film |
| CN112607778A (en) * | 2020-12-31 | 2021-04-06 | 东南大学 | Preparation method of molybdenum disulfide nanotube and molybdenum disulfide nanotube |
| CN113774356A (en) * | 2021-09-15 | 2021-12-10 | 复旦大学 | Wafer-level two-dimensional material growth method |
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Application publication date: 20171110 |