CN107190319A - A kind of preparation method and application of few layer molybdenum trioxide two-dimensional atomic crystal nanometer sheet - Google Patents
A kind of preparation method and application of few layer molybdenum trioxide two-dimensional atomic crystal nanometer sheet Download PDFInfo
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Abstract
The invention belongs to technical field of nano material, a kind of preparation method of few layer molybdenum trioxide two-dimensional atomic crystal nanometer sheet is disclosed.This method includes step in detail below：(1) molybdenum trioxide powder is formed into molybdenum trioxide crystal by recrystallization.(2) molybdenum trioxide crystal is pasted on adhesive tape.(3) it is sturdy by tape-stripping on flat substrate, extruding bubble therein, then tear, part molybdenum trioxide crystal is close on substrate.(4) substrate for being stained with molybdenum trioxide is soaked in 8~20s in alkaline solution, takes out rapid drying, you can obtain the few layer molybdenum trioxide nanosheet of large area in substrate surface.Present invention incorporates mechanical stripping method and the advantage of solution intercalation method, the few layer molybdenum trioxide nanosheet of large area, and manufacture craft simple and fast can be obtained.The molybdenum trioxide crystal of preparation can be used for field of photoelectric devices.
Description
Technical field
The invention belongs to technical field of nano material, more particularly to a kind of mechanical stripping method, chemical etching method prepares few layer
The method of molybdenum trioxide two-dimensional atomic crystal nanometer sheet.
Background technology
Two-dimensional graphene has very excellent photoelectric characteristic, but its band gap is 0, and band gap is difficult to open, seriously
Constrain the application of material in the semiconductor device.Two-dimensional semiconductor oxide material have higher dielectric constant, band gap compared with
Wide and structure can regulate and control, therefore the preparation of its material and device are applied and rapidly paid close attention to.Alfa phase molybdenum trioxides have
Two-dimensional layered structure, a molecular layers thick is 0.7nm, and dielectric constant increases with size reduction.Material has about 3eV simultaneously
Broad-band gap, its band gap width can be regulated and controled by the introducing of defect or ion, and and then regulate and control its photoelectric characteristic, because
This scene effect device (Balendhran.S.et al. (2013) " Field Effect Biosensing Platform
Based on 2Dα-MoO3."ACS Nano 7(11):9753-9760.), photodetection (Wang Y.et al. (2017) "
Growth of Large-Scale,Large-Size,Few-Layeredα-MoO3on SiO2and Its Photoresponse
Mechanism."ACS Applied Materials&Interfaces 9(6):5543-5549.), phasmon heat treatment
(Song,G.et al.(2014)."Hydrophilic Molybdenum Oxide Nanomaterials with
Controlled Morphology and Strong Plasmonic Absorption for Photothermal
Ablation of Cancer Cells."ACS Applied Materials&Interfaces 6(6):3915-3922.),
Photocatalysis (Sreedhara.M.B, et al. (2013) " Synthesis, Characterization, and Properties
of Few-Layer MoO3."Chemistry–An Asian Journal 8(10):2430-2435.) etc. field have important
Application prospect.
Two-dimentional molybdenum trioxide atomic crystal (thickness is prepared at present<Method 10nm) has：1. mechanical stripping method
(Kalantar-zadeh.K.et al.(2010)."Synthesis of nanometre-thick MoO3sheets."
Nanoscale 2(3):429-433.).Advantage prepared by mechanical stripping method is that material crystalline quality is high, and defect is small.But by
It is weaker in mechanical strength in the layer of molybdenum oxide, it is difficult to method is by mechanically pulling off as graphene and prepares large area (long or wide 10 μ
More than m) few layer crystal body.And mechanical stripping method is extremely inefficient, thickness can not regulate and control, and can only find at random under the microscope,
Characteristic is difficult to further regulation and control.2. solution stripping method (Hanlon D.et al. (2014) " Production of
Molybdenum Trioxide Nanosheets by Liquid Exfoliation and Their Application in
High-Performance Supercapacitors."Chemistry of Materials 26(4):1751-1763.)；It is molten
The advantage of liquid stripping method is to prepare yield greatly, but molybdenum oxide can be easy to crush when etching, form length and width size small
In 1 micron of thin slice, it is adapted to the application of the chemical fields such as large-scale photocatalysis, but is not suitable as optoelectronic semiconductor device
Part.The fault in material prepared in addition is more, and characteristic is difficult to regulate and control.3. vapor deposition method.Vapor deposition method can prepare high-quality, big
Few layer film of area (length reaches more than grade).But need to be used as substrate using mica.(Molina-Mendoza
A.J.et al.(2016)."Centimeter-Scale Synthesis of Ultrathin Layered MoO3by van
der Waals Epitaxy."Chemistry of Materials 28(11):4042-4051.) due to mica and semiconductor
Technique is incompatible, it is necessary to further carry out defect that the transfer of material, not only complex process, and transfer process introduce and miscellaneous
Matter is difficult to control to.High-quality, large area (tens micron dimensions) can be prepared on silicon and silica by process modification
Few layer of molybdenum oxide crystal.But the warm area of growth is small, process control difficulty is big, and the consumption of the energy and the loss of material are larger,
Preparation time is longer, at the same the later stage material property regulation and control when material uneven (the Wang.Y.et al. of spatial character
(2017)."Growth of Large-Scale,Large-Size,Few-Layeredα-MoO3on SiO2and Its
Photoresponse Mechanism."ACS Applied Materials&Interfaces9(6):5543-5549), no
Beneficial to the extension of application.
The content of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, primary and foremost purpose of the invention is to provide a kind of few oxygen of layer three
Change the preparation method of molybdenum two-dimensional atomic crystal nanometer sheet.This method technical process is simple, with low cost.
Another object of the present invention is to provide a kind of few layer of molybdenum trioxide tow -dimensions atom crystalline substance prepared by the above method
Body, the defect of the crystal is controllable, can prepare the two-dimentional molybdenum trioxide atomic crystal of different conductive characteristics, can be applied to semiconductor light
The fields such as power conversion device, the preparation of two-dimension laminate device.
The present invention by molybdenum trioxide powder by being converted to monocrystal material, and the method for being by mechanically pulling off is transferred to arbitrarily can not be by
The substrate of etching alkaline solution, by etching alkaline solution, can obtain few layer three oxidation of the length and width yardstick at tens to hundreds of microns
Molybdenum two-dimensional atomic crystal.The advantage of this method combination mechanical stripping method and chemical etching method, the protection using substrate to boundary layer
Effect, to obtain few layer of molybdenum oxide crystal of a large amount of large area.
The purpose of the present invention is realized by following proposal：
A kind of preparation method of few layer molybdenum trioxide two-dimensional atomic crystal nanometer sheet, it includes step in detail below：
(1) take molybdenum trioxide powder is some to be placed in crucible, in non-reducing atmosphere, including dry air environment or/
Inert environments or low vacuum environment are heated to 580 DEG C~780 DEG C, and more than time 1h obtains MoO 3 monocrystal piece；
(2) MoO 3 monocrystal piece is taken to adhere on adhesive tape, by adhesive tape doubling, MoO 3 monocrystal piece is clipped in adhesive tape has
The centre of sticky side, is compacted and then tears, and MoO 3 monocrystal piece is divided into two.Repeat said process 3~10 times；
(3) substrate used is put into solvent and be cleaned by ultrasonic；
(4) adhesive tape with molybdenum trioxide is attached to substrate used, extrudes adhesive tape, remove the sky between adhesive tape and silicon chip
Gas, makes adhesive tape and substrate attach completely.Slowly adhesive tape is torn from substrate, the different molybdenum trioxide thin slice of a large amount of thickness due to
Electrostatic Absorption is transferred on substrate；
(5) substrate for being stained with molybdenum trioxide is soaked in alkaline solution, 8~20s of time, nitrogen is used rapidly after taking-up
Drying.
Molybdenum trioxide powder described in step (1) is micron or the amorphous or polycrystal powder of Nano grade.It is such as purified
Grade monocrystalline is crystallized to, this step is may skip.
Dry air described in step (1) is less than 90% air atmosphere for humidity.It is preferred that, humidity is less than 40%.
Described inert environments are N2Or Ar etc..Low vacuum environment is that pressure is higher than 10-4Pa vacuum environment.
The accumulation degree that acid extraction described in step (1) regards molybdenum trioxide is determined.Temperature it is too high or when
Between long will make the distillation loss of part molybdenum trioxide.Preferably 580 DEG C, more than time 1h.In the distillation of this temperature oxidation molybdenum
It is weaker, the longer time can be maintained molybdenum trioxide is fully converted to crystal and will not material loss.
Step (1) the heat treatment recrystallization technique is simple, but can be not limited to heat treatment, and other use chemical vapor
Sedimentation, physical vapor deposition etc. realizes that the method for the preparation of large single crystal can be used.
After molybdenum trioxide used need to reach that submillimeter level, monocrystalline chip size are determined for monocrystalline chip size in step (2)
The full-size of continuous atomic crystal.
Adhesive tape used is any sticking adhesive tape of tool in step (2), uses 3M adhesive tapes of low-residual etc. can be with
Keep substrate clean, it is not necessary to carry out follow-up cleaning.
Substrate described in step (3) is silica, silicon, ito glass or other are smooth and be not readily dissolved at room temperature strong
The material of alkali.
It is preferred that, the substrate described in step (3) is silica and silicon substrate.
Solvent described in step (3) is at least one of ethanol, acetone and deionized water.
Aqueous slkali described in step (5) includes the aqueous slkalis such as sodium hydroxide, potassium hydroxide.Using higher concentration, stronger
Alkali needed for soak time it is less, be more beneficial for being formed few layer of molybdenum oxide of large area.By control alkali concn, alkali power and
Soak time can obtain the molybdenum trioxide of different defects.
It is preferred that, 2M potassium hydroxide solutions are such as used, soak time is 8~10s, can obtain the atomic crystal of low defect.
The length of few layer of above-mentioned molybdenum trioxide two-dimensional atomic crystal is 50~100 μm, and thickness is less than 7nm；Nanometer sheet is
Less than ten layers；Its electric conductivity is soaked in the growth of the time of alkaline solution with substrate and strengthened.It can be applicable to photoelectric sensing, photoelectricity
The photoelectricity clothing arts such as the preparation of conversion, gas sensing and two-dimension laminate device.
The inventive method of this patent make use of two mechanism：
1. there is anisotropic etching to the etching of molybdenum trioxide using alkaline solution, to the etching of crystrallographic plane (010)
Speed is much smaller than other crystal faces.
2. there is strong interaction in the molybdenum trioxide crystal of mechanical stripping transfer, therefore block alkali with substrate interface
The infiltration of property solution, it is ensured that the atomic layer at interface is not etched in immersion process.
The present invention has the following advantages and beneficial effect relative to prior art：
(1) molybdenum trioxide two-dimensional atomic crystal size prepared by the present invention has the raising of 2 orders of magnitude compared to liquid phase method,
It is very good in the dispersiveness of substrate；Size is bigger compared with simple mechanical stripping method, more efficiently, and yield is increased substantially.
(2) technique is simple compared with chemical vapor deposition method, and less energy consumption, material consumption is few, and can prepare more
On the substrate of species, while the regulation and control of material photoelectric characteristic can be reached by controlling etch period to produce required defect.
Brief description of the drawings
Fig. 1 is preparation flow figure of the invention.
Fig. 2 is the scanning electron microscope diagram piece of the molybdenum trioxide two-dimensional atomic crystal prepared by embodiment 1, prepared by display
Sample length be 50~100 μm.
Fig. 3 is the atomic force microscope images of the molybdenum trioxide two-dimensional atomic crystal prepared by embodiment 1.
Fig. 4 is molybdenum trioxide edge contour curve in Fig. 3, and display thickness is 3.96nm.
Fig. 5 is the comparison diagram of few layer molybdenum trioxide and body material Raman spectrum.Wherein " * " corresponding peak is the Si of substrate
Peak.The corresponding peak of "○" is the Raman vibration peak of molybdenum oxide, respectively 819cm-1O-Mo2Stretching vibration and 670cm-1O-
Mo3Stretching vibration.
Fig. 6 is the transmission electron microscope image of few layer molybdenum trioxide, can calculate (100) interplanar distance for 0.356nm and
(001) interplanar distance is 0.402nm.
Fig. 7 prepares gold electrode at nanometer sheet two ends using micro-processing technology and prepares two ends end-apparatus part, and measurement obtains different leachings
The voltage-current characteristic curve of the molybdenum trioxide atomic crystal of bubble time.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited
In this.Molybdenum trioxide powder used in following instance is purchased from Aladdin company.
Embodiment 1
(1) molybdenum trioxide powder (purity 99.9%) 1g of purchase is taken to be placed in the wide 2cm of long 5cm square ceramic crucible.
Crucible is positioned in tube furnace, two ends are not closed, air humidity is 40%.Crucible is heated to 580 DEG C, 1h is maintained, obtained
MoO 3 monocrystal piece.
(2) choose MoO 3 monocrystal piece and be positioned over 3M adhesive tapes and have sticking one side, it is multiple with rubber by adhesive tape doubling
The extrusion friction adhesive tape back side, tears in the same direction, it can be seen that part MoO 3 monocrystal piece is separated adhesive to another
On outer half adhesive tape.Process 5 times or so in repetition.
(3) silicon chip that surface there are 300nm silicon dioxide layers is cut into 1 × 1cm2Small pieces are placed the substrate into as substrate
Each ultrasonic 10min of alcohol, acetone, deionized water is sequentially passed through in clean beaker.Washed substrate is taken out, is blown with nitrogen gun
It is dry.
(4) tape-stripping of molybdenum trioxide will be stained with to ready silicon dioxide layer.The hard thing such as ruler gently scrapes table
Face, removes the air between adhesive tape and silicon chip, adhesive tape and substrate is attached completely.Slowly adhesive tape is torn from substrate,
It can be seen that a large amount of different molybdenum trioxide thin slices of thickness are transferred on substrate due to Electrostatic Absorption.
(5) compound concentration is 2M potassium hydroxide solution, and the titanium dioxide silicon chip for being stained with molybdenum trioxide is vertically soaked completely
Bubble enters in potassium hydroxide solution, and hold time 8s, takes out blow away remained on surface drop with elevated pressure nitrogen air gun rapidly afterwards.
(6) the scanning electron microscope diagram piece of few layer of molybdenum trioxide two-dimensional atomic crystal prepared by Fig. 2 displays.Due to pure
Molybdenum trioxide electric conductivity is poor, and black is presented in figure.Fig. 2 shows that multi-disc molybdenum trioxide chip size generally reaches tens microns
Length, can partly reach microns up to a hundred.Fig. 3 and Fig. 4 carry out pattern imaging to middle oxidation molybdenum sheet respectively, and test obtains thickness
Spend for 3.96nm, 5~6 layers of molecular layers thick, for few layer of atomic crystal.Fig. 5 Raman spectrum show the molybdenum trioxide of few layer by
In the reduction of thickness, resonance Raman peak-to-peak signal substantially weakens, and peak width increase.The Raman line of few layer can be observed clearly
819cm-1O-Mo2Stretching vibration and 670cm-1O-Mo3Stretching vibration, can confirm that as molybdenum trioxide.Fig. 6 high-resolution is saturating
Penetrate electron micrograph and show that molybdenum trioxide is looked unfamiliar length along (100) face and (001), interplanar distance be respectively 0.356nm and
0.402nm, the lattice that display molybdenum trioxide is has been distorted, and illustrates that this method can influence lattice structure, and then to regulate and control
The conductive characteristic of material.Prepare photoelectric device.
Embodiment 2
(1) molybdenum trioxide powder (purity 99.9%) 1g of purchase is taken to be placed in the wide 2cm of long 5cm square ceramic crucible.
Crucible is positioned in tube furnace, two ends are not closed, air humidity~40%.Crucible is heated to 580 DEG C, 1h is maintained, obtained
MoO 3 monocrystal piece.
(2) choose MoO 3 monocrystal piece and be positioned over 3M adhesive tapes and have sticking one side, it is multiple with rubber by adhesive tape doubling
The extrusion friction adhesive tape back side, tears in the same direction, it can be seen that part MoO 3 monocrystal piece is separated adhesive to another
On outer half adhesive tape.Process 5 times or so in repetition.
(3) silicon chip that surface there are 300nm silicon dioxide layers is cut into 1 × 1cm2Small pieces are placed the substrate into as substrate
Each ultrasonic 10min of alcohol, acetone, deionized water is sequentially passed through in clean beaker.Washed substrate is taken out, is dried up with nitrogen gun
It is standby.
(4) tape-stripping of molybdenum trioxide will be stained with to ready silicon dioxide layer.The hard thing such as ruler gently scrapes table
Face, removes the air between adhesive tape and silicon chip, adhesive tape and substrate is attached completely.Slowly adhesive tape is torn from substrate,
It can be seen that a large amount of different molybdenum trioxide thin slices of thickness are transferred on substrate due to Electrostatic Absorption.
(5) compound concentration is 2M potassium hydroxide solution, and the titanium dioxide silicon chip for being stained with molybdenum trioxide is vertically soaked completely
Bubble enters in potassium hydroxide solution, and hold time 20s, takes out blow away remained on surface drop with elevated pressure nitrogen air gun rapidly afterwards.
(6) immersion 20s molybdenum trioxide atomic crystal remains in that flaky nanometer structure.Fig. 7 compared for soak time
8s and 20s volt-ampere characteristic curve.There it can be seen that applying the electric current of 1V voltages only to sample when soak time is shorter
For nA magnitudes, resistance is higher.Electric current adds 1 magnitude after soak time increase.Table can confirm that by AFM
Defect in nano particle pattern, display crystal, which occurs, in face to be increased so that resistance reduction.Therefore by controlling soak time, it can control
The surface topography and electrology characteristic of nanometer sheet processed.The molybdenum trioxide nanosheet of preparation can prepare photoelectric device.
Embodiment 3
(1) molybdenum trioxide powder (purity 99.9%) 1g of purchase is taken to be placed in the wide 2cm of long 5cm square ceramic crucible.
Crucible is positioned in tube furnace, two ends are not closed, air humidity is 40%.Crucible is heated to 580 DEG C, 1h is maintained, obtained
MoO 3 monocrystal piece.
(2) choose MoO 3 monocrystal piece and be positioned over 3M adhesive tapes and have sticking one side, it is multiple with rubber by adhesive tape doubling
The extrusion friction adhesive tape back side, tears in the same direction, it can be seen that part MoO 3 monocrystal piece is separated adhesive to another
On outer half adhesive tape.Process 5 times or so in repetition.
(3) conductive pure silicon piece is cut into 1 × 1cm2Small pieces are placed the substrate into clean beaker successively as substrate
By alcohol, acetone, each ultrasonic 10min of deionized water.Washed substrate is taken out, is dried up with nitrogen gun.
(4) tape-stripping of molybdenum trioxide will be stained with to ready silicon chip.The hard thing such as ruler gently scrapes surface, removes
Air between adhesive tape and silicon chip, makes adhesive tape and substrate attach completely.Slowly adhesive tape is torn from substrate, it can be seen that big
The different molybdenum trioxide thin slice of amount thickness is transferred on substrate due to Electrostatic Absorption.
(5) compound concentration is 2M potassium hydroxide solution, and the silicon chip for being stained with molybdenum trioxide is vertically completely soaked into entrance
In potassium hydroxide solution, hold time 8s, takes out blow away remained on surface drop with elevated pressure nitrogen air gun rapidly afterwards.
(6) obtain molybdenum trioxide nanosheet with silica surface prepare molybdenum trioxide nanosheet surface topography and
Electrology characteristic is identical.Compared to silicon dioxide substrates, silicon is conductive substrates, therefore can directly prepare vertical semiconductor devices.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of few layer molybdenum trioxide two-dimensional atomic crystal nanometer sheet, it is characterised in that including walking in detail below
Suddenly：
(1) molybdenum trioxide powder is taken, heating obtains the MoO 3 monocrystal piece of submillimeter above length in non-reducing atmosphere；
(2) MoO 3 monocrystal piece transfer process：Take MoO 3 monocrystal piece to be pasted on adhesive tape, adhesive tape doubling is made three for several times
Molybdenum oxide crystal is uniformly distributed on adhesive tape, by tape-stripping in flat substrate surface and then stripping, makes molybdenum trioxide crystal equal
Even clings on substrate；
(3) substrate for being stained with molybdenum trioxide crystal is soaked in a period of time in alkaline solution, takes out and dry up rapidly.
2. preparation method according to claim 1, it is characterised in that：
Heating-up temperature described in step (1) is 580 DEG C~780 DEG C.
3. preparation method according to claim 1, it is characterised in that：
Atmosphere described in step (1) includes dry air or inert gas or low vacuum environment.
4. preparation method according to claim 1, it is characterised in that：
Substrate described in step (2) is SiO2, Si, ito glass.
5. preparation method according to claim 1, it is characterised in that：
MoO 3 monocrystal piece transfer process described in step (2) is to use impressing mode.
6. preparation method according to claim 1, it is characterised in that：
Alkaline solution described in step (3) is sodium hydroxide, potassium hydroxide.
7. preparation method according to claim 1, it is characterised in that：
Soak time described in step (3) is 8~20s.
8. the few layer of molybdenum trioxide two-dimensional atomic crystal that a kind of method according to any one of claim 1~7 is prepared
Nanometer sheet.
9. few layer molybdenum trioxide two-dimensional atomic crystal nanometer sheet according to claim 8, it is characterised in that：Above-mentioned crystal
Length is 50~100 μm, and thickness is less than 7nm；Nanometer sheet is less than ten layers；Its electric conductivity with substrate be soaked in alkaline solution when
Between growth and strengthen.
10. few layer of molybdenum trioxide two-dimensional atomic crystal nanometer sheet according to claim 8 or claim 9 should field of photoelectric devices
With.
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| CN108611684A (en) * | 2018-04-27 | 2018-10-02 | 清华-伯克利深圳学院筹备办公室 | A kind of controllable thining method of Transition-metal dichalcogenide two-dimensional atomic crystal |
| CN109368627A (en) * | 2018-11-13 | 2019-02-22 | 清华大学 | The method of two-dimension nano materials directional assembly |
| CN109580615A (en) * | 2018-11-13 | 2019-04-05 | 清华大学 | Determine the method for few layer two-dimension nano materials crystal orientation |
| CN109928427A (en) * | 2019-03-21 | 2019-06-25 | 暨南大学 | A kind of double ion intercalation molybdenum oxide nanometer sheet, hetero-junctions and preparation method thereof |
| CN110098267A (en) * | 2019-04-09 | 2019-08-06 | 深圳激子科技有限公司 | A kind of graphene mid-infrared light detector and preparation method thereof based on the enhancing of phonon excimer |
| CN113186590A (en) * | 2020-01-14 | 2021-07-30 | 中国科学院物理研究所 | Preparation method of centimeter-level molybdenum trioxide single crystal |
| CN115287743A (en) * | 2022-08-16 | 2022-11-04 | 北京航空航天大学 | Two-dimensional material synthesis method, two-dimensional material and application thereof |
-
2017
- 2017-05-17 CN CN201710350244.6A patent/CN107190319A/en active Pending
Non-Patent Citations (4)
| Title |
|---|
| H. C. ZENG: "Chemical Etching of Molybdenum Trioxide: A New Tailor-Made Synthesis of MoO3 Catalysts", 《INORG. CHEM.》 * |
| KOUROSH KALANTAR-ZADEH ET AL.: "Synthesis of nanometre-thick MoO3 sheets", 《NANOSCALE》 * |
| S. K. DEB: "Physical properties of a transition metal oxide: optical and photoelectric properties of single crystal and thin film molybdenum trioxide", 《PROC.ROY.SOC.A》 * |
| YU WANG ET AL.: "Growth of Large-Scale, Large-Size, Few-Layered α‑MoO3 on SiO2 and Its Photoresponse Mechanism", 《ACS APPL. MATER. INTERFACES》 * |
Cited By (11)
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| CN108502620A (en) * | 2018-03-15 | 2018-09-07 | 东南大学 | A kind of folding system and its application method of two-dimensional material |
| CN108502620B (en) * | 2018-03-15 | 2019-08-27 | 东南大学 | A kind of folding system and its application method of two-dimensional material |
| CN108611684A (en) * | 2018-04-27 | 2018-10-02 | 清华-伯克利深圳学院筹备办公室 | A kind of controllable thining method of Transition-metal dichalcogenide two-dimensional atomic crystal |
| CN109368627A (en) * | 2018-11-13 | 2019-02-22 | 清华大学 | The method of two-dimension nano materials directional assembly |
| CN109580615A (en) * | 2018-11-13 | 2019-04-05 | 清华大学 | Determine the method for few layer two-dimension nano materials crystal orientation |
| CN109928427A (en) * | 2019-03-21 | 2019-06-25 | 暨南大学 | A kind of double ion intercalation molybdenum oxide nanometer sheet, hetero-junctions and preparation method thereof |
| CN110098267A (en) * | 2019-04-09 | 2019-08-06 | 深圳激子科技有限公司 | A kind of graphene mid-infrared light detector and preparation method thereof based on the enhancing of phonon excimer |
| CN113186590A (en) * | 2020-01-14 | 2021-07-30 | 中国科学院物理研究所 | Preparation method of centimeter-level molybdenum trioxide single crystal |
| CN113186590B (en) * | 2020-01-14 | 2023-03-21 | 中国科学院物理研究所 | Preparation method of centimeter-level molybdenum trioxide single crystal |
| CN115287743A (en) * | 2022-08-16 | 2022-11-04 | 北京航空航天大学 | Two-dimensional material synthesis method, two-dimensional material and application thereof |
| CN115287743B (en) * | 2022-08-16 | 2023-12-22 | 北京航空航天大学 | Two-dimensional material synthesis method, two-dimensional material and application thereof |
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