KR20170056386A - Method of manufacturing thin layer of molybdenum disulfide - Google Patents
Method of manufacturing thin layer of molybdenum disulfide Download PDFInfo
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- KR20170056386A KR20170056386A KR1020150160000A KR20150160000A KR20170056386A KR 20170056386 A KR20170056386 A KR 20170056386A KR 1020150160000 A KR1020150160000 A KR 1020150160000A KR 20150160000 A KR20150160000 A KR 20150160000A KR 20170056386 A KR20170056386 A KR 20170056386A
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- thin film
- molybdenum disulfide
- disulfide thin
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 123
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 239000010409 thin film Substances 0.000 claims abstract description 159
- 239000000758 substrate Substances 0.000 claims abstract description 58
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000001301 oxygen Substances 0.000 claims abstract description 35
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 27
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011593 sulfur Substances 0.000 claims abstract description 15
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 15
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 13
- 239000011733 molybdenum Substances 0.000 claims abstract description 13
- 239000010410 layer Substances 0.000 claims description 46
- 238000005229 chemical vapour deposition Methods 0.000 claims description 15
- 239000002356 single layer Substances 0.000 claims description 12
- 238000009832 plasma treatment Methods 0.000 claims description 10
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 8
- 229910001882 dioxygen Inorganic materials 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000001069 Raman spectroscopy Methods 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- 238000012545 processing Methods 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 230000009257 reactivity Effects 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 238000001237 Raman spectrum Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000003086 colorant Substances 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 238000001106 transmission high energy electron diffraction data Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 125000004430 oxygen atom Chemical group O* 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/02557—Sulfides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/02274—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition in the presence of a plasma [PECVD]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02439—Materials
- H01L21/02469—Group 12/16 materials
- H01L21/02474—Sulfides
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- H01L21/205—
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/46—Generating plasma using applied electromagnetic fields, e.g. high frequency or microwave energy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/10—Details of semiconductor or other solid state devices to be connected
- H01L2924/102—Material of the semiconductor or solid state bodies
- H01L2924/1025—Semiconducting materials
- H01L2924/1026—Compound semiconductors
- H01L2924/1072—Layered
- H01L2924/10722—Molybdenum disulfide [MoS2]
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- Plasma & Fusion (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Thin Film Transistor (AREA)
Abstract
Description
The present invention relates to a method for preparing a molybdenum disulfide thin film, and more particularly, to a method for depositing a molybdenum disulfide thin film on a substrate by controlling the number of layers.
Molybdenum disulfide is a kind of transition metal dichalcogenide (TMD) compound, which has a band gap between a valence band and a conduction band and has a semiconducting property. Particularly, since molybdenum disulfide has a bandgap different from that of graphene, it is evaluated as a material having excellent physical and chemical electrical properties and flexibility. Therefore, it is widely regarded as a new material material that can be used in various fields of future nano devices and optoelectronics .
When molybdenum disulfide is used as a nano thin film and used as a channel layer of a thin film transistor, the transistor has band gap energy of 1.2 to 1.9 eV depending on its thickness, so that characteristics of the transistor are changed by controlling the thickness of the molybdenum disulfide thin film. Therefore, it is important to control the thickness of the molybdenum disulfide thin film. Conventional methods of producing molybdenum disulfide thin films include mechanical peeling and liquid peeling, and both methods have a problem in that it is difficult to control the thickness of the molybdenum disulfide thin film.
As a technique for controlling the thickness of the molybdenum disulfide thin film, sulfur trioxide or molybdenum trioxide may be sulphurized using a sulfur source, or ammonium thiomolybdate ((NH4) 2MoS4) may be added to the substrate surface for depositing a thin film. And then molybdenum disulfide is synthesized through heat treatment of sulfur and argon. However, when a thin film transistor is manufactured using the molybdenum disulfide thin film produced by such a method, the electron mobility is low and the on / off ratio (Ion / Ioff) of the current is low.
The present invention is directed to a method for manufacturing a molybdenum disulfide thin film, and more particularly, to a method for manufacturing a molybdenum disulfide thin film, which can adjust the thickness of a molybdenum disulfide thin film formed on a substrate by performing oxygen plasma treatment on the substrate, And a method for producing the same.
According to an aspect of the present invention, there is provided a method of manufacturing a molybdenum disulfide thin film, comprising: exposing an insulating substrate to an oxygen plasma; And forming a molybdenum disulfide thin film on the substrate by reacting molybdenum and sulfur. The thickness of the molybdenum disulfide thin film can be controlled by controlling the oxygen plasma exposure time of the insulating substrate.
In one embodiment, the step of forming the molybdenum disulfide thin film may include a chemical vapor deposition (CVD) process using a molybdenum source and a sulfur source.
In one embodiment, the molybdenum disulfide thin film may be composed of three or less molecular layers.
In one embodiment, the molybdenum disulfide thin film may be formed in the thin film forming step when the oxygen plasma exposure time is less than 120 seconds, and the plasma processing time of the plasma step is 120 seconds or more and 300 seconds , Two layers of molybdenum disulfide thin films may be formed in the thin film formation step, and when the plasma treatment time of the plasma step is 300 seconds or more, three layers of molybdenum disulfide thin films may be formed in the thin film formation step.
According to another embodiment of the present invention, there is provided a method of manufacturing a molybdenum disulfide thin film comprising: exposing an insulating substrate to an oxygen plasma; And forming a molybdenum disulfide thin film on the substrate by reacting molybdenum and sulfur, wherein the pressure in the chamber, the power applied to the oxygen plasma, and the oxygen injected to produce the oxygen plasma The thickness of the molybdenum disulfide thin film can be controlled by adjusting at least one of the flow rate of the gas.
The thin film transistor according to another embodiment of the present invention may use the molybdenum disulfide thin film produced by any one of the above embodiments as a channel layer.
As described above, the thickness of the molybdenum disulfide thin film can be controlled by atomically producing a single layer, a two-layer, and a three-layer molybdenum disulfide thin film by controlling the time of oxygen plasma treatment on the substrate on which the molybdenum disulfide thin film is deposited There is an effect to make.
Also, by manufacturing a thin film transistor using a molybdenum disulfide thin film having a controlled thickness, it is possible to manufacture a thin film transistor having different electrical characteristics according to the thickness of the molybdenum disulfide thin film.
BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a diagram illustrating steps of a method for producing a molybdenum disulfide thin film according to Examples 1 to 3 of the present invention. FIG.
2 is a view showing a side view of a chemical vapor deposition apparatus for manufacturing
FIGS. 3A to 3C are photographs of the molybdenum disulfide thin films of Examples 1 to 3 of the present invention, respectively, taken by an optical microscope. FIG.
FIGS. 3D to 3F are photographs of the molybdenum disulfide thin films of Examples 1 to 3, taken with an atomic force microscope.
4 is a graph showing the results of Raman spectrum measurement of a single layer, two layers and three layers of a molybdenum disulfide thin film.
5 is a graph showing the average values of Raman shift differences of A mode and E mode in the area of
FIG. 6 is a diagram showing transmission electron microscope images and SAED (Selective Area Electron Diffraction) patterns for crystal structure analysis of Examples 1 to 3 of the present invention. FIG.
FIG. 7 is a diagram showing a transmission electron microscope measurement image of the folded regions of the thin films of Examples 1 to 3 of the present invention. FIG.
FIG. 8 is a graph showing the structure and Id-Vg characteristics of a thin film transistor using the molybdenum disulfide thin film of Examples 1 to 3 of the present invention as a channel layer.
9 is a graph showing electron mobility of thin film transistors using the molybdenum disulfide thin films of Examples 1 to 3 as a channel layer.
While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail. It should be understood, however, that the invention is not intended to be limited to the particular embodiments, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Hereinafter, a preferred embodiment of the present invention will be described in detail with reference to the accompanying drawings. Wherein like reference numerals refer to like elements throughout.
A method of manufacturing a molybdenum disulfide thin film according to an embodiment of the present invention includes: exposing an insulating substrate to an oxygen plasma; And forming a molybdenum disulfide thin film on the insulating substrate by reacting molybdenum and sulfur. The thickness of the molybdenum disulfide thin film can be controlled by controlling the oxygen plasma exposure time of the insulating substrate . As the plasma exposure time increases, the thickness of the molybdenum disulfide thin film may increase. This is because as the plasma exposure time becomes longer, the amount of plasma that can react with the surface of the insulating substrate increases.
In one embodiment, the molybdenum disulfide thin film may be formed in the thin film forming step when the oxygen plasma exposure time is less than 120 seconds, and the plasma processing time of the plasma step is 120 seconds or more and 300 seconds , Two layers of the molybdenum disulfide thin film may be formed in the thin film forming step and three layers of the molybdenum disulfide thin film may be formed in the thin film forming step when the plasma processing time of the plasma step is 300 seconds or more.
According to another embodiment of the present invention, there is provided a method of manufacturing a molybdenum disulfide thin film comprising: exposing an insulating substrate to an oxygen plasma; And forming a molybdenum disulfide thin film on the substrate by reacting molybdenum and sulfur, wherein the pressure in the chamber, the power applied to the oxygen plasma, and the oxygen plasma are injected to produce the oxygen plasma The thickness of the molybdenum disulfide thin film can be controlled by controlling at least one of the flow rate of the oxygen gas and the flow rate of the oxygen gas. In one embodiment, as the power applied to the plasma increases, the thickness of the molybdenum disulfide thin film may increase. As the power applied to the plasma increases, the amount of plasma generated increases, and as the amount of plasma at the exposed surface of the insulating substrate increases, the reactivity of the surface of the insulating substrate increases. As the flow rate of the oxygen gas is lower, oxygen plasma is not scattered by the oxygen gas, so that higher reactivity can be given to the insulating substrate. The lower the pressure in the chamber is, the more scattering of the oxygen plasma in the chamber does not occur and the higher reactivity can be given to the insulating substrate.
In one embodiment, the insulating substrate may include at least one of SiO 2 / Si, sapphire, and quartz, but the material is not limited as long as the substrate can be used for chemical vapor deposition. In one embodiment for use in a thin film transistor, a SiO 2 / Si substrate can be used.
In one embodiment, the molybdenum disulfide thin film may be composed of three or less molecular layers. For example, the molybdenum disulfide thin film formed on the insulating substrate may be a single layer, a double layer, or a three layer.
The molybdenum and sulfur may be used in various molybdenum sources and sulfur sources, and in one embodiment, molybdenum trioxide powder and sulfur powder may be used.
In one embodiment, the step of forming the molybdenum disulfide thin film may include a chemical vapor deposition (CVD) process using a molybdenum source and a sulfur source. In one embodiment, the chemical vapor deposition may be performed in a chamber of a chemical vapor deposition apparatus. For example, the molybdenum source and the sulfur source may be transported in the chamber through a carrier gas, and then reacted through heat treatment, followed by forming a molybdenum disulfide thin film on the insulating substrate. In one embodiment, the carrier gas may be an inert gas and may be, for example, argon (Ar).
The thin film transistor according to another embodiment of the present invention may use the molybdenum disulfide thin film produced by any one of the above embodiments as a channel layer.
BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a diagram illustrating steps of a method for producing a molybdenum disulfide thin film according to Examples 1 to 3 of the present invention. FIG.
≪ Example 1 >
Referring to FIG. 1, a substrate for preparing a molybdenum disulfide thin film according to Example 1 of the present invention was prepared. The substrate was the same size as 2 cm x 2 cm, and a substrate made of a 285 nm thick silicon dioxide insulating layer and a silicon layer was prepared. The substrate was washed with acetone, isopropyl alcohol (IPA) and deionized water. Subsequently, the cleaned substrate was placed in a plasma chamber and subjected to a plasma treatment in an oxygen atmosphere for 90 seconds by a capacitive coupled plasma (CCP) method. Plasma processing conditions are as follows. The substrate subjected to the plasma treatment for 90 seconds was used for producing the monolayer molybdenum disulfide thin film of Example 1. [
In order to form a molybdenum disulfide thin film on the plasma-treated substrate, a chemical vapor deposition (CVD) process was used. The chemical vapor deposition process was performed in a chemical vapor deposition apparatus using a 10 cm quartz tube as a chamber.
2 is a view showing a side view of a chemical vapor deposition apparatus for
Referring to FIG. 2, in order to manufacture the molybdenum disulfide thin film of the present invention, the
≪ Example 2 >
Example 2 is a two-layer molybdenum disulfide thin film. In order to produce the molybdenum disulfide thin film of Example 2, only the plasma treatment time in the plasma process conditions of Example 1 was changed as shown in the following table. The remaining process conditions are the same as the process conditions in Example 1, and redundant descriptions are omitted.
≪ Example 3 >
Example 3 is a three-layer molybdenum disulfide thin film. In order to produce the molybdenum disulfide thin film of Example 3, only the plasma treatment time in the plasma process conditions of Example 1 was changed as shown in the following table. The remaining process conditions are the same as the process conditions in Example 1, and redundant descriptions are omitted.
≪ Analysis of Optical Microscope and Atomic Force Microscope Photographing Results of Examples 1 to 3 >
FIGS. 3A to 3C are photographs of the molybdenum disulfide thin films of Examples 1 to 3 of the present invention, respectively, taken by an optical microscope. FIG. FIG. 3A shows an optical microscope image of Example 1, FIG. 3B shows Example 2, and FIG. 3C shows Example 3. FIGS. 3D to 3F are photographs of the molybdenum disulfide thin films of Examples 1 to 3, taken with an atomic force microscope.
Referring to FIGS. 3A to 3C, it can be seen that colors are different between the thin films. The colors shown in the optical microscope photographs are due to the difference in refractive index between the silicon layer of the substrate on which the molybdenum disulfide thin film is deposited and the molybdenum disulfide thin film, and since the colors of FIGS. 3A to 3C are all different, And the thickness of the molybdenum disulfide thin films are different from each other. In addition, it can be seen that the thicknesses of the molybdenum disulfide thin films produced are uniform since the image colors of Examples 1 to 3 are all uniform.
Referring to FIGS. 3D to 3E, in FIG. 3D, the thickness of the molybdenum disulfide thin film was measured to be 0.65 nm, and in FIG. 3E, the thickness of the molybdenum disulfide thin film was measured to be 1.4 nm. In the case of FIG. 3F, the thickness of the molybdenum disulfide thin film was measured to be 2.2 nm. As a result, it can be seen that Example 1 formed a single layer of molybdenum disulfide thin film, Example 2 comprised two layers of molybdenum disulfide thin film, and Example 3 formed three layers of molybdenum disulfide thin film.
≪ Results of Raman Spectra Measurement of Examples 1 to 3>
4 is a graph showing the results of Raman spectrum measurement of a single layer, two layers and three layers of a molybdenum disulfide thin film. 4 (a) is a molybdenum disulfide thin film, (b) is a molybdenum disulfide thin film, and (c) is a molybdenum disulfide thin film. In Fig. 4, the E mode and the A mode represent the intrinsic Raman spectrum of molybdenum disulfide. Also, as the thickness of the thin film increases, the Raman shift of the E mode decreases and the Raman shift of the A mode increases.
5 is a graph showing the average values of Raman shift differences of A mode and E mode in the area of
Referring to FIGS. 4 and 5, it can be seen that Raman shifts in the E mode are reduced and Raman shifts in the A mode are increased in the first to third embodiments. The difference between the Raman shift values of the A mode and the E mode is 19.6 to 20.6 cm -1 in Example 1, 98.3 to 22.3 to 22.9 cm -1 in Example 2, 98.2% in Example 3, 23.2 To 24 cm < -1 >. Actually, referring to FIG. 4, the single layer of the molybdenum disulfide thin film has 20 cm -1, the two layers have 22.6 cm -1, and the three layers have 23.7-1. In Example 1, the single layer of molybdenum disulfide thin film, It was confirmed that the thin film had two layers and Example 3 had the molybdenum disulfide thin film three layers. As a result, it can be seen that the longer the time of treating the oxygen plasma with the substrate, the more the thickness of the molybdenum disulfide thin film, that is, the number of layers is increased.
≪ Results of Transmission Electron Microscope Measurement of Examples 1 to 3 >
In order to confirm the number of the thin film layers of Examples 1 to 3 of the present invention, a thin film was photographed by a transmission electron microscope. To this end, the thin films of Examples 1 to 3 were separated, transferred to a grid for measuring an electron transmission microscope, and photographed.
FIG. 6 is a diagram showing transmission electron microscope images and SAED (Selective Area Electron Diffraction) patterns for crystal structure analysis of Examples 1 to 3 of the present invention. FIG.
FIG. 7 is a diagram showing a transmission electron microscope measurement image of the folded regions of the thin films of Examples 1 to 3 of the present invention. FIG.
Referring to FIG. 6, the SAED pattern in the image (a) of Example 1 has a hexagonal crystal structure in which each of six atoms has one hexagonal structure. Thus, it can be confirmed that the molybdenum disulfide thin film of Example 1 is composed of a single layer. In addition, the SAED pattern in the image (b) of Example 2 is composed of a crystal structure having two sets of hexagonal structures. Thus, it can be seen that the molybdenum disulfide thin film of Example 2 has two layers of hexagonal thin films. Finally, the SAED pattern in the image (c) of Example 3 consists of three sets of hexagonal crystal structures. Thus, it can be seen that the molybdenum disulfide thin film of Example 3 is composed of three hexagonal thin films. Also, it can be seen that the SAED patterns of Examples 2 and 3 were photographed with Moire patterns formed by overlapping crystal structures of two or three layers.
Referring to FIG. 7, in the image (a) of Example 1, it can be seen that a single layer of molybdenum disulfide thin film having a thickness of 0.65 nm is formed in the folded region. In the image (b) of Example 2, it can be seen that the folded region is formed by overlapping two layers of molybdenum disulfide thin films having a thickness of 1.4 nm. Finally, in the image (c) of Example 3, it is confirmed that the folded region is formed by overlapping three layers of the molybdenum disulfide thin film having a thickness of 2.2 nm.
From the above results, it can be confirmed that the molybdenum disulfide thin film of Example 1 was formed as a single layer, that of Example 2 was formed as two layers, and that of Example 3 was formed.
<Analysis of Electrical Characteristics of Thin Film Transistors Using Thin Films of Examples 1 to 3>
Thin film transistors were fabricated to analyze the electrical characteristics of Examples 1 to 3. The gate was made of silicon and the insulating layer was made of 285 nm silicon dioxide. 5 nm thick titanium and 60 nm thick gold were used as the electrodes, and the molybdenum disulfide thin films of Examples 1 to 3 of the present invention were used as channel layers.
FIG. 8 is a diagram showing a structure of a thin film transistor using the molybdenum disulfide thin films of Examples 1 to 3 of the present invention as a channel layer and a graph measuring I d -V g characteristics. The blue line of the graph is the Id-Vg characteristic value of Example 1, the red line is the Id-Vg characteristic value of Example 2, and the green line is the Id-Vg characteristic value of Example 3. [
Referring to FIG. 8, it can be seen that the drain current (I d ) of the thin film
9 is a graph showing electron mobility of thin film transistors using the molybdenum disulfide thin films of Examples 1 to 3 as a channel layer. The blue region of the graph is the electron mobility measurement of Example 1, the red region is the Example 2, and the green region is the electron mobility measurement value of Example 3. [
Referring to FIG. 9, the mobility of the thin film transistor using Example 1 at room temperature is 3.6 cm 2 V -1 s -1 , the mobility of the thin film transistor using Example 2 is 8.2 cm 2 V -1 s -1 , The mobility of the thin film transistor using Example 3 was measured to be 15.6 cm 2 V -1 s -1 . As a result, it was confirmed that the electron mobility of the thin film transistor using the thin film was measured according to the thickness of the molybdenum disulfide thin film.
<The reason why the thickness of molybdenum disulfide thin film can be controlled by oxygen plasma pretreatment of insulating substrate>
The reason why the thickness control of the molybdenum disulfide thin film according to the embodiment of the present invention is controlled by the oxygen plasma pretreatment of the insulating substrate is twofold.
First, hydrophilization of an insulating substrate can be mentioned. When an oxygen plasma is exposed on an insulating substrate, OH radicals are generated by the plasma, and OH radicals are highly reactive substances. Since the OH radical is attached to the surface of the insulating substrate, the reactivity at the surface of the insulating substrate is increased, and the thickness of the molybdenum disulfide thin film is determined according to the amount of OH radical deposition. Therefore, the insulating substrate is exposed to the oxygen plasma to form a molybdenum disulfide thin film It is considered that the thickness can be adjusted.
Secondly, by exposing the surface of the insulating substrate to the plasma, more oxygen can be attached to the surface of the insulating substrate, and thereby the reactivity can be increased. For example, when a SiO 2 substrate is used as an insulating substrate, each of the two oxygen atoms is bonded to Si atoms with two bonds. When exposing the oxygen plasma on the SiO 2 substrate, one of the two bonding bonded to the oxygen atom falling by being brought into engagement with an oxygen plasma, is increased to three or four oxygen atoms are combined with Si, thereby SiO 2 It is considered that the reactivity of the substrate is increased and the thickness of the molybdenum disulfide thin film can be controlled.
While the invention has been shown and described with reference to certain preferred embodiments thereof, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims. Accordingly, the true scope of the present invention should be determined by the following claims.
Claims (6)
Reacting molybdenum and sulfur to form a molybdenum disulfide thin film on the substrate,
And adjusting the thickness of the molybdenum disulfide thin film by controlling the oxygen plasma exposure time of the insulating substrate,
Method for manufacturing molybdenum disulfide thin film.
Wherein the forming of the molybdenum disulfide thin film comprises:
And a chemical vapor deposition (CVD) process using a molybdenum source and a sulfur source.
Method for manufacturing molybdenum disulfide thin film.
Wherein the molybdenum disulfide thin film comprises three or less molecular layers.
If the oxygen plasma exposure time is less than 120 seconds, a molybdenum disulfide monolayer is formed in the thin film forming step,
When the plasma treatment time of the plasma step is 120 seconds or more and less than 300 seconds, two layers of molybdenum disulfide thin film are formed in the thin film forming step,
Wherein when the plasma treatment time of the plasma step is 300 seconds or more, three layers of molybdenum disulfide thin film are formed in the thin film forming step,
Method for manufacturing molybdenum disulfide thin film.
Reacting molybdenum and sulfur to form a molybdenum disulfide thin film on the substrate,
Adjusting a thickness of the molybdenum disulfide thin film by adjusting at least one of a pressure in the chamber, a power source applied to the oxygen plasma, and a flow rate of oxygen gas injected to generate the oxygen plasma,
Method for manufacturing molybdenum disulfide thin film.
Thin film transistor.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455675A (en) * | 2018-11-27 | 2019-03-12 | 北京科技大学 | A kind of preparation method in transition metal family sulfide nanometer sheet sulphur vacancy |
| CN110783179A (en) * | 2019-11-14 | 2020-02-11 | 苏州大学 | Preparation method of two-dimensional material field effect transistor |
| WO2024043625A1 (en) * | 2022-08-24 | 2024-02-29 | 경상국립대학교산학협력단 | Method for controlling surface characteristics and thickness of multilayer transition metal dichalcogenide thin film |
-
2015
- 2015-11-13 KR KR1020150160000A patent/KR20170056386A/en unknown
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455675A (en) * | 2018-11-27 | 2019-03-12 | 北京科技大学 | A kind of preparation method in transition metal family sulfide nanometer sheet sulphur vacancy |
| CN109455675B (en) * | 2018-11-27 | 2020-12-29 | 北京科技大学 | Preparation method of sulfur vacancy of transition metal sulfide nanosheet |
| CN110783179A (en) * | 2019-11-14 | 2020-02-11 | 苏州大学 | Preparation method of two-dimensional material field effect transistor |
| WO2024043625A1 (en) * | 2022-08-24 | 2024-02-29 | 경상국립대학교산학협력단 | Method for controlling surface characteristics and thickness of multilayer transition metal dichalcogenide thin film |
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