CN105810569A - Tungsten sulphide film and preparation method thereof - Google Patents
Tungsten sulphide film and preparation method thereof Download PDFInfo
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- CN105810569A CN105810569A CN201610182002.6A CN201610182002A CN105810569A CN 105810569 A CN105810569 A CN 105810569A CN 201610182002 A CN201610182002 A CN 201610182002A CN 105810569 A CN105810569 A CN 105810569A
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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
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02373—Group 14 semiconducting materials
- H01L21/02381—Silicon, silicon germanium, germanium
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- 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
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- 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
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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Abstract
The invention belongs to the technical field of inorganic nano-film materials, and provides a preparation method of a tungsten sulphide film. The preparation method comprises the following steps of: plating a W layer, the thickness of which is one atom, on a silicon substrate; plating a S layer, the thickness of which is one atom, on the W layer; and plating another W layer, the thickness of which is one atom, on the S layer so as to obtain a WS2 film, wherein the WS2 film is a W-S-W layered single-layer film. The invention further provides the tungsten sulphide film, which is prepared by the preparation method. By means of the method disclosed by the invention, large-area preparation of the WS2 film can be realized; furthermore, the quality of the prepared WS2 film is obviously improved; and the electrical property of the WS2 film is greatly improved.
Description
Technical field
The invention belongs to inorganic nano technology field of membrane materials, particularly relate to a kind of tungsten sulfide thin film and preparation thereof
Method.
Background technology
Tungsten sulfide (WS2) thin film is much like with molybdenum sulfide thin film in structure and performance, tungsten sulfide thin film is also
There is a regulatable band gap.Bulk crystals WS2Band gap be 1.3eV, its electron transition mode is indirect
Transition;When thickness is monolayer, WS2Band gap can reach 2.1eV, and its electron transition mode changes
For direct transition.Therefore, WS2The structure of thin film uniqueness and excellent physical property and adjustable energy carry
Gap so that it is in field of electronic devices especially before electricity, optics, semiconductor applications have particularly significant application
The two-dimension nano materials of scape.Tungsten disulfide thin film is due to its special optically and electrically performance so that it is at light
The application of electronic applications is very wide, be widely used in manufacturing field-effect transistor, sensor, light emitting diode,
Large bulk capacitance memorizer and electrode of lithium cell.Simultaneously because its special crystal structure, they are also by extensively
For being catalyzed, the field such as antifriction.Although WS2Thin film has the biggest application potential, but in prior art
Grow monolayer WS2Thin film, its product area is minimum, and compactness is relatively poor, and sulfur room is more, causes
The poor-performing of thin film prepared therefrom.
Summary of the invention
For solving above-mentioned technical problem, the invention provides the preparation method of a kind of tungsten sulfide thin film, it is intended to obtain
A kind of must preferably prepare large-area high-quality WS2The method of thin film, makes up WS2Thin film is in technique preparation side
Deficiency in method.
The present invention is achieved in that the preparation method of a kind of tungsten sulfide thin film, comprises the following steps:
Step one: plate the W layer that a layer thickness is an atom on a silicon substrate;
Step 2: plate the S layer that a layer thickness is an atom on described W layer;
Step 3: plate the W layer that another layer thickness is an atom on described S layer, it is thus achieved that WS2Thin
Film;
Described WS2Thin film is the single thin film of W-S-W layer structure.
Further, the material of described silicon substrate is SiO2。
Further, described silicon substrate is the most first carried out, and described cleaning process is: serve as a contrast silicon
The end, carries out the ultrasonic immersion of acetone successively, deionized water cleans, hydrogen peroxide and concentrated sulphuric acid mixed liquor clean and go from
Sub-water cleans.
Further, in the ultrasonic immersion of described acetone, the mass ratio of acetone used and described silicon substrate is 20:1.
Further, the frequency of the ultrasonic immersion of described acetone is 28kHz, and power is 150W;Scavenging period is
10~25min.
Further, described hydrogen peroxide with concentrated sulphuric acid mixed liquor cleaning process is: described silicon substrate is put into institute
State immersion 2h-3h in mixed liquor.
Further, described hydrogen peroxide with concentrated sulphuric acid Compound mixed solution process is: added by 30% hydrogen peroxide solution
Entering in 98% concentrated sulphuric acid, stirring, solution obtains mixed liquor after cooling down completely;Described hydrogen peroxide solution and dense sulfur
Acid solution volume ratio is 1:3.
Further, the technology used plating last layer W atomic layer in described step one and step 3 includes ALD
One in technology (technique for atomic layer deposition), pulsed laser deposition technique and magnetron sputtering technique.
Further, in described step 2, method therefor is CVD (chemical vapour deposition technique).
Present invention also offers a kind of tungsten sulfide thin film, the preparation method described in employing is made.
Further, described thin film is a monoblock continuous, and area is 1-3 square centimeter.
The present invention compared with prior art, has the beneficial effects that: the present invention uses ALD skill the most on a silicon substrate
Art plating last layer W atomic layer, then uses CVD to grow one layer of S atom layer on its W atomic layer,
Re-use ALD technique plating last layer W atomic layer, thus grow the monolayer WS of W-S-W layer structure2
Thin film.By the method for the present invention, WS can be realized2Prepared by the large area of thin film;And the WS of preparation2Thin film
Compactness is good, sulfur room is few, and this makes its quality significantly improve, and then significantly improves WS2Thin film
Electric property.
Accompanying drawing explanation
Fig. 1 is the ALD fundamental reaction circulation schematic diagram in the present invention.
Fig. 2 is the process flow diagram of technical solution of the present invention.
Fig. 3 is the test result of optical microscope and Raman spectrometer;Wherein Fig. 3 (a) Raman test result,
Fig. 3 (b) is PL test result.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and reality
Execute example, the present invention is further elaborated.Only should be appreciated that specific embodiment described herein
Only in order to explain the present invention, it is not intended to limit the present invention.
Chemical vapour deposition technique (CVD): refer to anti-containing the gaseous reactant or liquid constituting thin film element
Steam and reaction other gas required of answering agent introduce reative cell, generate thin at substrate surface generation chemical reaction
The process of film.
Technique for atomic layer deposition (ALD): be that material can be plated layer by layer by one with monatomic form membrane
Method at substrate surface.The basic process of technique for atomic layer deposition is vaporous precursors pulse alternately to be led to
Enter reaction chamber, chemical absorption of surface reaction occurs on the deposition substrate, and then forms thin film.Ald
Similarity is had with common chemical deposition.
Pulsed laser deposition technique (PLD): be that one utilizes laser to bombard object, then will bombardment
Species precipitate out on different substrates, is precipitated or a kind of means of thin film.
Magnetron sputtering technique: electronics occurs with ar atmo during accelerating to fly to substrate under the effect of electric field
Collision, ionizes out substantial amounts of argon ion and electronics, and electronics flies to substrate.Argon ion adds under the effect of electric field
Speed bombardment target, sputters substantial amounts of target atom, is deposited on substrate in neutral target atom (or molecule)
Upper film forming.
Preparing tungsten sulfide thin film according to technical scheme, process is as follows:
First SiO is prepared2Silicon substrate, and prepare acetone, deionized water, hydrogen peroxide and concentrated sulphuric acid mixed liquor pair
It is carried out.Specifically, hydrogen peroxide with the process for preparation of concentrated sulphuric acid mixed liquor is: by water-soluble for 30% dioxygen
Liquid joins in 98% concentrated sulphuric acid, stirring, and solution obtains mixed liquor after cooling down completely;Described hydrogen peroxide solution with
Concentrated sulfuric acid solution volume ratio is 1:3.
To SiO2Silicon substrate carries out the ultrasonic immersion of acetone successively, deionized water cleans, hydrogen peroxide mixes with concentrated sulphuric acid
Close liquid to clean and deionized water cleaning.Specifically, first with acetone ultrasonic cleaning 20min, wherein acetone used
It is 20:1 with the mass ratio of described silicon substrate;The frequency of the ultrasonic immersion of acetone is 28kHz, and power is 150W;
Then clean up with deionized water;It is then placed in hydrogen peroxide and soaks 2h-3h, so in concentrated sulphuric acid mixed liquor
Clean up with deionized water afterwards.
Preparing tungsten sulfide thin film, specific operation process is as follows:
Step one, uses ALD technique to plate last layer W atomic layer on a silicon substrate:
This process uses ALD technique to carry out, and ALD technique is not a continuous print technical process, but
It is made up of a series of half-reaction.Fig. 1 is that ALD fundamental reaction circulates schematic diagram, and its each unit is followed
Ring is generally divided into four steps: first, is passed through precursor A steam pulse to reaction chamber, at the substrate surface exposed
There is Chemisorption;Then pass to purge gas (usually noble gas, such as high pure nitrogen or argon),
Take precursor A steam not to be adsorbed and byproduct of reaction out of reaction chamber;Then precursor B steam it is passed through
, there is surface chemical reaction with the A of surface adsorption in pulse;Finally again it is passed through purge gas, by unnecessary
B steam and byproduct of reaction take reaction chamber out of, the most often carry out a circulation, and substrate surface deposits one layer
Monoatomic layer.L in Fig. 1 is presoma dentate.Specifically, in conjunction with Fig. 1, A steam, B steam
Being the reacting gas in ALD growth course, growing tungsten atom layer A steam during corresponding basis is WF6, B
Steam Si2H6。
For growing tungsten atom layer during basis, this reaction is that extreme based on Si-F key is stable, thus occurs
Typical exothermic reaction, complete chemical reaction is WF6+Si2H6→W+SiF3H+2H2.This chemical process
Molar reactive enthalpy change Δ H=-181kcal/mol.Tungsten hexafluoride and Disilicoethane reaction obtained unusual light,
Pure tungsten film, the often circulation of grown at low temperature speed approximate ideal is 1 molecular layer (often circulating 0.25nm),
And thickness is proportional with period.Illustrate to there occurs between two kinds of presomas completely surface reaction it was confirmed
Two saturated generations from restriction half-reaction, i.e.
W-SiHF*2+WF6(g)→W-WF*5+SiHF3(g)
W-WF*5+Si2H6(g)→WW-SiHF*2+2H2(g)+SiHF3。
Overall reaction is: WF6(g)+Si2H6(g)→W+SiHF3+2H2(g)
W film in present invention work be the model using Finland Beneq Corp. to produce be BENEQ TFS
Prepared by 200-124 atomic deposition device, technological process is as follows:
(1) opening N2, power air pressure is set as that by force 0.5Mpa, carrier gas pressure set are 0.14Mpa;
(2) control chamber is turned on the power;
(3) mechanical pump is opened;
(4) control software is opened;
(5) design temperature is 60 DEG C;
(6) reach about 60 DEG C when reaction chamber temperature, click on vent button, to interacvity air-filling, then uncap
Put into silicon chip, close;
(7) evacuation is continued, until intracavity pressure is steady;
(8) reaction temperature is set: 300 DEG C;
(9) precursor gas pressure is set:
WF6(g): 6.5 × 10-8pa
Si2H6(g): 2.2 × 10-9pa
(10) reaction formula is set: grow the W film of 0.25nm;
(11) reaction terminates to take out sample, closes hull closure.
Step 2, plating last layer S atom layer on described W atomic layer:
This process uses CVD to carry out, and the experiment condition of this technique of the present invention is: with sulfur powder (0.1g) be
Sulfur source, high-purity argon gas is current-carrying gas (flow is 15sccm), and temperature is 300 DEG C, is incubated 2min,
Deposition is had to have preparation WS on the titanium dioxide silicon chip of W atomic layer2Thin film.
Step 3, plates another layer of W atomic layer, it is thus achieved that WS on described S atom layer2Thin film:
This process is also to use ALD technique to carry out, and specific operation process and principle are identical with step one.
Concrete thin film growth process schematic diagram is as shown in Figure 2.By the method for the present invention, WS can be realized2
Prepared by the large area of thin film;The WS of preparation2Thin film is the single thin film of W-S-W layer structure, compactness
Good, sulfur room is few, not only increases WS2The quality of thin film, decreases WS simultaneously2The fault in material of thin film,
And then significantly improve WS2The electric property of thin film.
The product obtained for the process conditions of present invention proposition is WS2Thin film.Raman spectrum (raman) and
PL (luminescence generated by light) technology is the important means of research tungsten sulfide thin film, and we will use laser Raman spectroscopy
Instrument characterizes, and that can see in Raman spectrogram has two Raman-active vibrational peaks, is belonging respectively to curing
The E of tungsten1 2gAnd A1gVibration mode, the Raman frequency shift of its correspondence is respectively 355.6cm-1And 418.3cm-1。
According to the experimental verification of document, monolayer WS2E1 2gThe Raman frequency shift of vibration mode is 356cm-1, A1g
The Raman frequency shift of vibration mode is 417.5cm-1People is along with the increase of the number of plies, E1 2gVibration slow down (occur red shift,
Frequency displacement diminishes) and A1g(there is blue shift, frequency displacement increases) in vibration aggravation, the E of tungsten disulfide body phase material1 2gWith
A1gVibration mode Raman frequency shift is respectively 355.5cm-1And 420.5cm-1.The different layers provided with document
Number tungsten disulfide E1 2gAnd A1gThe position of vibration mode characteristic peak compares, the Raman collection of illustrative plates of institute's test sample product with
Monolayer WS2Collection of illustrative plates consistent.
We also use laser Raman spectrometer that sample thin film carries out fluorescent scanning (PL mapping) simultaneously,
Crystal film luminosity difference according to different-thickness characterizes film shape and thickness, when thickness is monolayer
Time, WS2Band gap can reach 2.1eV, experiment prove the present invention prepared be monolayer WS2.FIG. 3 below
It is the test result of optical microscope and Raman spectrometer, wherein Fig. 3 (a) Raman test result;Fig. 3 (b) is
PL (luminescence generated by light) test result.
By Raman spectrogram and PL spectrogram it can be seen that the present invention propose process conditions obtained by product
Product are WS really2Single thin film, and quality is the best.It addition, in addition to ALD growth W atomic layer, bag
Include a series of additive method, equally may be used as pulsed laser deposition technique and magnetron sputtering technique grow W atomic layer
To implement the present invention.
By measuring us, WS prepared by the present invention2Thin film is continuous print one monolithic films, and area is
1-3 square centimeter.Present invention achieves WS2Prepared by the large area of thin film;And the WS of preparation2The matter of thin film
Amount significantly improves, and also significantly improves WS2The electric property of thin film.
In the application of tungsten sulfide thin film, when two dimension transition metal two chalcogenide is become single from block
During layer, the energy band band gap of electronics also become direct band gap from direct band gap, and its optical property occurs accordingly simultaneously
Change, the change of a series of optical properties such as such as luminescence generated by light, electroluminescent, photovoltaic effect can be produced.
The heliosensitivity several times higher than Graphene of two dimension transition metal dichalcogenide, simultaneously because energy gap problem,
Electron mobility is less than Graphene, and response is also the most corresponding less fast, therefore can be used to make high-performance
Optical pickocff, the device such as Photoelectrical detector.It is reported, by monolayer MoS2The flexible LED that thin film is made
Device has occurred, and has good optical property, therefore WS2Thin film is also widely used.Separately
Outward, class Graphene transition metal dichalcogenide all has in terms of the many such as mechanics, optics, electricity, electrochemistry
Certain feature, the lamellar structure of class Graphene makes it have bigger specific surface area, and unit are is external
The acceptance that boundary stimulates is also the most more.As a kind of semi-conducting material, WS2Class Graphene transition metal curing
Substantially, it is fast that the high electron mobility that the multi-layer sheet structure of itself brings can make it respond again in the switch response of sundries part
Speed;The activity of material surface is high, it is simple to its modifying surface is strengthened sensitivity and detection range.This
Series of advantages allows WS2Sensor become a kind of highly sensitive, response rapidly, the wide sensor of suitable environment,
There is the application prospect of brilliance.The technical scheme that the present invention provides, for WS2The application of thin film provides another
Wide prospect.
Below in conjunction with specific embodiment, technical scheme is described further.
Embodiment 1
Prepare SiO2Silicon substrate, and prepare acetone, it is entered by deionized water, hydrogen peroxide with concentrated sulphuric acid mixed liquor
Row cleans.Specifically, hydrogen peroxide with the process for preparation of concentrated sulphuric acid mixed liquor is: added by 30% hydrogen peroxide solution
Entering in 98% concentrated sulphuric acid, stirring, solution obtains mixed liquor after cooling down completely;Described hydrogen peroxide solution and dense sulfur
Acid solution volume ratio is 1:3.
To SiO2Silicon substrate carries out the ultrasonic immersion of acetone successively, deionized water cleans, hydrogen peroxide mixes with concentrated sulphuric acid
Close liquid to clean and deionized water cleaning.Specifically, first with acetone ultrasonic cleaning 20min, wherein acetone used
It is 20:1 with the mass ratio of described silicon substrate;The frequency of the ultrasonic immersion of acetone is 28kHz, and power is 150W;
Then clean up with deionized water;It is then placed in hydrogen peroxide and soaks 3h in concentrated sulphuric acid mixed liquor, then use
Deionized water cleans up.
Preparing tungsten sulfide thin film, specific operation process is as follows:
Step one, uses ALD technique to plate last layer W atomic layer on a silicon substrate;
Step 2, plating last layer S atom layer on described W atomic layer:
With 0.1g sulfur powder for sulfur source, high-purity argon gas is current-carrying gas (flow is 15sccm), and temperature is 300 DEG C,
Insulation 2min, has preparation WS on the titanium dioxide silicon chip of W atomic layer there being deposition2Thin film.
Step 3, plates another layer of W atomic layer, it is thus achieved that WS on described S atom layer2Thin film.
By measuring, WS prepared by the present embodiment2Thin film is continuous print one monolithic films, and area is 2
Square centimeter.
Embodiment 2
Prepare SiO2Silicon substrate, and prepare acetone, it is entered by deionized water, hydrogen peroxide with concentrated sulphuric acid mixed liquor
Row cleans.Specifically, hydrogen peroxide with the process for preparation of concentrated sulphuric acid mixed liquor is: added by 30% hydrogen peroxide solution
Entering in 98% concentrated sulphuric acid, stirring, solution obtains mixed liquor after cooling down completely;Described hydrogen peroxide solution and dense sulfur
Acid solution volume ratio is 1:3.
To SiO2Silicon substrate carries out the ultrasonic immersion of acetone successively, deionized water cleans, hydrogen peroxide mixes with concentrated sulphuric acid
Close liquid to clean and deionized water cleaning.Specifically, first with acetone ultrasonic cleaning 15min, wherein acetone used
It is 20:1 with the mass ratio of described silicon substrate;The frequency of the ultrasonic immersion of acetone is 28kHz, and power is 150W;
Then clean up with deionized water;It is then placed in hydrogen peroxide and soaks 3h in concentrated sulphuric acid mixed liquor, then use
Deionized water cleans up.
Preparing tungsten sulfide thin film, specific operation process is as follows:
Step one, uses ALD technique to plate last layer W atomic layer on a silicon substrate;
Step 2, plating last layer S atom layer on described W atomic layer:
With 0.1g sulfur powder for sulfur source, high-purity argon gas is current-carrying gas (flow is 15sccm), and temperature is 300 DEG C,
Insulation 2min, has preparation WS on the titanium dioxide silicon chip of W atomic layer there being deposition2Thin film.
Step 3, plates another layer of W atomic layer, it is thus achieved that WS on described S atom layer2Thin film.
By measuring, WS prepared by the present embodiment2Thin film is continuous print one monolithic films, and area is 1
Square centimeter.
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 (10)
1. the preparation method of a tungsten sulfide thin film, it is characterised in that comprise the following steps:
Step one: plate the W layer that a layer thickness is an atom on a silicon substrate;
Step 2: plate the S layer that a layer thickness is an atom on described W layer;
Step 3: plate the W layer that another layer thickness is an atom on described S layer, it is thus achieved that WS2Thin
Film;
Described WS2Thin film is the single thin film of W-S-W layer structure.
2. preparation method as claimed in claim 1, it is characterised in that the material of described silicon substrate is SiO2。
3. preparation method as claimed in claim 1, it is characterised in that described silicon substrate is before the use first
Being carried out, described cleaning process is: silicon substrate is carried out successively the ultrasonic immersion of acetone, deionized water clean,
Hydrogen peroxide cleans with concentrated sulphuric acid mixed liquor and deionized water cleans.
4. preparation method as claimed in claim 3, it is characterised in that used in the ultrasonic immersion of described acetone
Acetone is 20:1 with the mass ratio of described silicon substrate;The frequency of the ultrasonic immersion of described acetone is 28kHz, power
For 150W;Scavenging period is 10~25min.
5. preparation method as claimed in claim 3, it is characterised in that described hydrogen peroxide mixes with concentrated sulphuric acid
Liquid cleaning process is: described silicon substrate is put into immersion 2-3h in described mixed liquor.
6. preparation method as claimed in claim 3, it is characterised in that described hydrogen peroxide mixes with concentrated sulphuric acid
Liquid process for preparation is: joined by 30% hydrogen peroxide solution in 98% concentrated sulphuric acid, and stirring, solution cools down completely
After mixed liquor;Described hydrogen peroxide solution and concentrated sulfuric acid solution volume ratio are 1:3.
7. preparation method as claimed in claim 1, it is characterised in that plate in described step one and step 3
Technology used by upper W layer includes in ALD technique, pulsed laser deposition technique and magnetron sputtering technique
Kind.
8. preparation method as claimed in claim 1, it is characterised in that in described step 2, method therefor is
CVD.
9. a tungsten sulfide thin film, it is characterised in that use the preparation method system described in claim 1~8
Become.
10. tungsten sulfide thin film as claimed in claim 9, it is characterised in that described thin film is that a monoblock connects
Ideotype, area is 1-3 square centimeter.
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Cited By (4)
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WO2017166028A1 (en) * | 2016-03-28 | 2017-10-05 | 深圳大学 | Tungsten sulfide film and preparation method therefor |
CN110607516A (en) * | 2019-10-24 | 2019-12-24 | 云南师范大学 | Preparation method of single-layer or double-layer tungsten disulfide film |
CN113532273A (en) * | 2021-07-09 | 2021-10-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Based on multilayer WS2High-sensitivity position detector of/Si structure |
CN114958036A (en) * | 2022-06-30 | 2022-08-30 | 厦门韫茂科技有限公司 | Pearlescent pigment and preparation method thereof |
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CN104561937A (en) * | 2015-01-05 | 2015-04-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing WS2 film having solid lubrication function by means of atomic layer deposition |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2017166028A1 (en) * | 2016-03-28 | 2017-10-05 | 深圳大学 | Tungsten sulfide film and preparation method therefor |
CN110607516A (en) * | 2019-10-24 | 2019-12-24 | 云南师范大学 | Preparation method of single-layer or double-layer tungsten disulfide film |
CN110607516B (en) * | 2019-10-24 | 2021-06-29 | 云南师范大学 | Preparation method of single-layer or double-layer tungsten disulfide film |
CN113532273A (en) * | 2021-07-09 | 2021-10-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Based on multilayer WS2High-sensitivity position detector of/Si structure |
CN114958036A (en) * | 2022-06-30 | 2022-08-30 | 厦门韫茂科技有限公司 | Pearlescent pigment and preparation method thereof |
CN114958036B (en) * | 2022-06-30 | 2023-12-01 | 丰田自动车株式会社 | Pearlescent pigment and preparation method thereof |
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