CN113774356A - Wafer-level two-dimensional material growth method - Google Patents
Wafer-level two-dimensional material growth method Download PDFInfo
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- CN113774356A CN113774356A CN202111078973.3A CN202111078973A CN113774356A CN 113774356 A CN113774356 A CN 113774356A CN 202111078973 A CN202111078973 A CN 202111078973A CN 113774356 A CN113774356 A CN 113774356A
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- 238000000034 method Methods 0.000 title claims abstract description 54
- 239000000463 material Substances 0.000 title claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 239000000758 substrate Substances 0.000 claims abstract description 24
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical compound Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 9
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 8
- RLECCBFNWDXKPK-UHFFFAOYSA-N bis(trimethylsilyl)sulfide Chemical compound C[Si](C)(C)S[Si](C)(C)C RLECCBFNWDXKPK-UHFFFAOYSA-N 0.000 claims abstract description 6
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 22
- 238000010926 purge Methods 0.000 claims description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 239000006227 byproduct Substances 0.000 claims description 6
- 229910052961 molybdenite Inorganic materials 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 239000010408 film Substances 0.000 abstract description 21
- 239000010409 thin film Substances 0.000 abstract description 5
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 7
- 229910015221 MoCl5 Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002210 silicon-based material Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
-
- 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
- C23C16/56—After-treatment
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a method for growing a wafer-level two-dimensional material. Molybdenum pentachloride and hexamethyldisilthiane are used as reaction precursors, the substrate is alternately exposed to gas pulses of the molybdenum pentachloride and the hexamethyldisilthiane by controlling the parameters of the atomic layer deposition process, and the gas is adsorbed on the surface of the substrate and undergoes chemical reaction to form wafer-level MoS with accurately controllable thickness2A film; and then annealing treatment is carried out. The method can realize the growth of 4-inch wafer-level large-area molybdenum disulfide, and the on-off ratio of a device prepared on the basis of the thin film reaches 106Carrier mobility of 10cm2V‑1s‑1The above.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a method for growing a wafer-level two-dimensional material.
Background
Two-dimensional MoS2The method has the advantages of high carrier mobility, adjustable semiconductor band gap along with thickness and the like, and is widely researched and applied to micro-nano photoelectronic devices. Two-dimensional MoS compared to conventional bulk silicon materials2Has excellent grid regulation capability under the condition of extremely small thickness, and can haveEffectively suppressing short channel effects. In the post Moore's Law era, two-dimensional MoS2Is expected to enter industrialized application, and can be used as a supplement to silicon-based materials or even partially replace the silicon-based materials.
Currently, two-dimensional MoS is limited2The main obstacle of the industrial application of the material is the lack of a set of film development process which is compatible with the current CMOS, can be grown in a large scale and controlled manner, and has high uniformity and high performance.
The conventional mechanical stripping method is only suitable for preparing small-scale device circuits, while the conventional Chemical Vapor Deposition (CVD) method has the problems of difficulty in controlling the film thickness, poor uniformity on a large-size substrate and the like.
Disclosure of Invention
The invention discloses a wafer-level two-dimensional material growth method, which comprises the following steps:
molybdenum pentachloride and hexamethyldisilthiane are used as reaction precursors, the substrate is alternately exposed to gas pulses of the molybdenum pentachloride and the hexamethyldisilthiane by controlling the parameters of the atomic layer deposition process, and the gas is adsorbed on the surface of the substrate and undergoes chemical reaction to form wafer-level MoS with accurately controllable thickness2A film; and carrying out subsequent annealing treatment.
In the wafer-level two-dimensional material growth method of the present invention, preferably, the process parameters include precursor pulse time, precursor temperature, reaction chamber temperature, and cycle number.
In the wafer-level two-dimensional material growth method, preferably, molybdenum pentachloride is pulsed into the atomic layer deposition reaction cavity in a growth cycle period to be adsorbed on the surface of the substrate, and the pulse time of the molybdenum pentachloride is 2 s; then, high-purity N is pulsed into the reaction cavity2Purging to clean excessive molybdenum pentachloride and reaction byproducts, wherein the pulse time is 8 s;
then, introducing hexamethyldisilazane in a pulse mode into the reaction cavity to enable the hexamethyldisilazane to be adsorbed on the surface of the substrate, wherein the pulse time of the hexamethyldisilazane is 1 s; then, high-purity N is pulsed into the reaction cavity2Purging was performed to purge excess hexamethyldisilazane and reaction by-products for a pulse time of 5 s.
In the wafer-level two-dimensional material growth method, preferably, the temperature of the molybdenum pentachloride precursor is set to be 115 ℃, and the temperature of the hexamethyldisilazane precursor is set to be room temperature.
In the wafer-level two-dimensional material growth method, the reaction chamber is preferably at a temperature of 350-450 ℃.
In the wafer-level two-dimensional material growth method, preferably, the annealing furnace tube is divided into two temperature zones, the first temperature zone is used for placing the film sample, the second temperature zone is used for placing sufficient sulfur powder to produce a sulfur-rich atmosphere, and low-flow high-purity Ar gas is introduced all the time in the whole process.
In the wafer-level two-dimensional material growth method of the present invention, preferably, the Ar flow rate is maintained at 10 sccm.
In the wafer-level two-dimensional material growth method of the present invention, preferably, the target temperature of the first temperature zone is set to 900 ℃, and the target temperature of the second temperature zone is set to 350 ℃.
In the wafer-level two-dimensional material growth method of the present invention, preferably, the temperature is maintained for 60min after both temperature zones reach the target temperature.
In the wafer-level two-dimensional material growth method of the present invention, preferably, the wafer-level MoS is2The thickness precision of the film can be controlled in the order of 0.1 nm.
Drawings
FIG. 1 is a wafer level MoS2Flow chart of a method for growing a thin film.
FIG. 2 is an atomic layer deposition MoS2Growth principle diagram of the film.
FIG. 3 is a graph illustrating the effect of growth temperature and cycle number on the growth mode of a thin film.
Fig. 4 is a scanned transmission image of films grown at different growth temperatures.
FIG. 5 is a time-dependent temperature profile of the first and second temperature zones of the furnace tube.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly and completely understood, the technical solutions in the embodiments of the present invention will be described below with reference to the accompanying drawings in the embodiments of the present invention, and it should be understood that the specific embodiments described herein are only for explaining the present invention and are not intended to limit the present invention. The described embodiments are only some embodiments of the invention, not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "vertical", "horizontal", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Furthermore, numerous specific details of the invention, such as structure, materials, dimensions, processing techniques and techniques of the devices are described below in order to provide a more thorough understanding of the invention. However, as will be understood by those skilled in the art, the present invention may be practiced without these specific details. Unless otherwise specified below, each part in the device may be formed of a material known to those skilled in the art, or a material having a similar function developed in the future may be used.
FIG. 1 is a wafer level MoS2Flow chart of a method for growing a thin film. As shown in fig. 1, the method comprises the following steps:
step S1, the substrate is cleaned. Before the substrate is placed into a reaction cavity of the atomic layer deposition equipment, cleaning is carried out to remove pollutants possibly existing on the surface of the substrate, and the method comprises the following specific steps:
1) putting the substrate into an acetone solution for ultrasonic cleaning for about 10 min;
2) putting the substrate into an absolute ethyl alcohol solution for ultrasonic cleaning for about 5 min;
3) and putting the substrate into deionized water for ultrasonic cleaning for about 5 min.
4) The substrate was completely blown dry with nitrogen without leaving water stain.
In step S2, device parameters are set. After the substrate is placed in the reaction chamber, before deposition begins, it is necessary to ensure that all parameters of the apparatus have reached set values, and the specific parameters are set as follows:
the source bottle (bottle containing the precursor) was set to a temperature of: molybdenum pentachloride (MoCl)5) The source bottle temperature was set to 115 deg.C and the Hexamethyldisilazane (HMDST) source bottle temperature was set to room temperature, i.e., 25 deg.C. When the temperature of the heat source is lower than the saturated vapor pressure temperature, the heat source inlet amount is insufficient, the grown film has the phenomenon that the air inlet is thick and the air outlet is thin, and when the temperature of the heat source is too high, the heat source inlet amount is too much, so that waste is caused and the control is difficult.
The temperature of the reaction cavity is set to 350-450 ℃, and the optimal temperature is 450 ℃. The high-temperature growth can effectively improve the crystallinity of the film, reduce defects and improve the performance of the device.
And step S3, adjusting the process parameters. The whole atomic layer deposition process is that a substrate is alternately exposed to MoCl5And HMDST gas pulses, the process of gas adsorption on the substrate surface and chemical reaction proceeds as shown in fig. 2. With high purity N2As carrier gas and purge gas, the specific parameters of the whole process cycle are as follows:
(1) first, the HMDST pretreatment is carried out, the HMDST pulse time is 30s, and then N is used2And purging for 60 s.
(2) Then pulse-introducing MoCl into the reaction cavity5Adsorbing the substrate on the surface of the substrate, and introducing MoCl5The pulse time of (2) s; then, high-purity N is pulsed into the reaction cavity2Purging to clean excess MoCl5And reaction by-products, pulse time 8 s.
(3) Then, pulse introducing HMDST into the reaction cavity to enable the HMDST to be adsorbed on the surface of the substrate, wherein the pulse time of introducing the HMDST is 1 s; then, high-purity N is pulsed into the reaction cavity2Purging to clean excessHMDST and reaction by-products, pulse time 5 s.
The steps (2) to (3) are a growth cycle period, in each ALD cycle, the amount of the precursor is controlled by adjusting the pulse time, when the amount of the precursor is insufficient, the phenomenon that the thickness of the air inlet film is uneven and the thickness of the air outlet film is uneven is easily caused, and when the amount of the precursor entering is excessive, the etching effect and waste are caused. At the same time, in each growth cycle period, adjusting and controlling N2And the purging time is used for preventing the accumulation of the precursor from influencing the uniformity of the film.
Setting the number of cycle cycles required to obtain a desired MoS thickness based on the growth rate2A film. The growth appearance of the two-dimensional material can be controlled by adjusting the growth temperature (namely the temperature of the reaction cavity) and the cycle number (namely the thickness). The growth temperature window is 350-450 ℃, the roughness of the film is reduced along with the increase of the temperature, the uniformity is improved, the crystallinity is better, and the quality is better (shown in the aspects of electrical performance and the like). When the growth temperature exceeds 450 c and the film thickness exceeds 6 layers, the film growth mode starts to be changed from the horizontal growth to the vertical growth, as shown in fig. 3 and 4.
Step S4, annealing. The whole annealing furnace pipe is divided into two temperature zones, the first temperature zone is used for placing a film sample, the temperature is set to be 900 ℃, the second temperature zone is used for placing sufficient sulfur powder, the temperature is set to be 350 ℃, a sulfur-rich atmosphere is manufactured, and low-flow high-purity Ar gas is introduced all the time in the whole process.
Fig. 5 shows the temperature profile of the first temperature zone and the second temperature zone over time. The details of the whole furnace tube annealing process steps are as follows:
first, the sample and sulfur powder were placed in preparation for furnace tube heating. In particular, the method of manufacturing a semiconductor device,
placing a sample film on a quartz boat, wherein the surface of the film faces upwards, and the quartz boat is placed at the downstream of a furnace tube, namely a first temperature zone;
weighing a proper amount of sulfur powder (about 500mg) and placing the sulfur powder in a quartz boat, and placing the whole body in the downstream of a furnace tube, namely a second temperature zone;
the furnace tube is pumped to low vacuum (about 0.1Pa), and the furnace tube is subjected to water vapor removal treatment, namely, the temperature of two temperature regions of the furnace tube is increased to 100 ℃, and inert gas (Ar) with large flow rate of 500sccm is introduced and maintained for 10 min.
Then, an annealing process is carried out:
in the temperature rise stage, the target temperature of the first temperature zone is set to 900 ℃, the temperature rise time is 40min, the temperature rise rate is about 20 ℃/min, the target temperature of the second temperature zone is set to 350 ℃, the temperature rise time is 40min, and the temperature rise rate is about 6 ℃/min. The Ar flow rate in this process was set to 10 sccm.
When the target temperature of the first temperature zone is increased to 900 ℃, the target temperature of the second temperature zone is increased to 350 ℃, and the temperature is kept for 60 min. The Ar flow was maintained at 10sccm during this process.
And finally, entering a cooling stage:
the temperatures of the two areas are set to be 20 ℃, and the furnace tube is naturally cooled to the room temperature from the high temperature. The Ar flow was still maintained at 10 sccm.
At present, the two-dimensional material film which has large-area uniformity, low surface roughness and high performance and high quality is difficult to obtain by utilizing an atomic layer deposition method to prepare the two-dimensional material. The method can realize the growth of 4-inch wafer-level large-area molybdenum disulfide, and the on-off ratio of a device prepared on the basis of the thin film reaches 106Carrier mobility of 10cm2V-1s-1The above.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (10)
1. A method for growing a wafer-level two-dimensional material,
the method comprises the following steps:
molybdenum pentachloride and hexamethyldisilthiane are used as reaction precursors, the substrate is alternately exposed to gas pulses of the molybdenum pentachloride and the hexamethyldisilthiane by controlling the parameters of the atomic layer deposition process, and the gas is adsorbed on the surface of the substrate and undergoes chemical reaction to form wafer-level MoS with accurately controllable thickness2A film;
and carrying out subsequent annealing treatment.
2. The wafer-level two-dimensional material growth method of claim 1,
the process parameters comprise precursor pulse time, precursor temperature, reaction chamber temperature and cycle number.
3. The wafer-level two-dimensional material growth method of claim 2,
pulse-introducing molybdenum pentachloride into the atomic layer deposition reaction cavity in a growth cycle period to enable the molybdenum pentachloride to be adsorbed on the surface of the substrate, wherein the pulse time of introducing the molybdenum pentachloride is 2 s; then, high-purity N is pulsed into the reaction cavity2Purging to clean excessive molybdenum pentachloride and reaction byproducts, wherein the pulse time is 8 s;
then, introducing hexamethyldisilazane in a pulse mode into the reaction cavity to enable the hexamethyldisilazane to be adsorbed on the surface of the substrate, wherein the pulse time for introducing the hexamethyldisilazane is 1 s; then, high-purity N is pulsed into the reaction cavity2Purging was performed to purge excess hexamethyldisilazane and reaction by-products for a pulse time of 5 s.
4. The wafer-level two-dimensional material growth method of claim 2,
the temperature of the molybdenum pentachloride precursor is set to 115 ℃, and the temperature of the hexamethyldisilazane precursor is set to room temperature.
5. The wafer-level two-dimensional material growth method of claim 2,
the temperature of the reaction cavity is 350-450 ℃.
6. The wafer-level two-dimensional material growth method of claim 1,
the furnace tube for annealing is divided into two temperature zones, wherein a film sample is placed in the first temperature zone, sufficient sulfur powder is placed in the second temperature zone, a sulfur-rich atmosphere is produced, and low-flow high-purity Ar gas is introduced all the time in the whole process.
7. The wafer-level two-dimensional material growth method of claim 6,
the Ar flow rate was maintained at 10 sccm.
8. The wafer-level two-dimensional material growth method of claim 6,
the target temperature of the first temperature zone is set to 900 ℃, and the target temperature of the second temperature zone is set to 350 ℃.
9. The wafer-level two-dimensional material growth method of claim 8,
when both temperature zones reach the target temperature, the temperature is maintained for 60 min.
10. The wafer-level two-dimensional material growth method of claim 1,
the wafer level MoS2The thickness precision of the film can be controlled in the order of 0.1 nm.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2899295A1 (en) * | 2014-01-24 | 2015-07-29 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Method for producing a thin layer of formula myx by ald |
CN107338422A (en) * | 2017-06-26 | 2017-11-10 | 东南大学 | A kind of method of ald molybdenum disulfide film |
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 |
CN109378341A (en) * | 2018-09-20 | 2019-02-22 | 复旦大学 | A kind of molybdenum disulfide tunneling transistor and preparation method thereof |
CN110767533A (en) * | 2019-10-24 | 2020-02-07 | 华南理工大学 | Wafer-level MoS2Method for preparing single-layer film |
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- 2021-09-15 CN CN202111078973.3A patent/CN113774356A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2899295A1 (en) * | 2014-01-24 | 2015-07-29 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Method for producing a thin layer of formula myx by ald |
CN107338422A (en) * | 2017-06-26 | 2017-11-10 | 东南大学 | A kind of method of ald molybdenum disulfide film |
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 |
CN109378341A (en) * | 2018-09-20 | 2019-02-22 | 复旦大学 | A kind of molybdenum disulfide tunneling transistor and preparation method thereof |
CN110767533A (en) * | 2019-10-24 | 2020-02-07 | 华南理工大学 | Wafer-level MoS2Method for preparing single-layer film |
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Application publication date: 20211210 |