CN110373636A - A kind of preparation method of molybdenum silicide transistion metal compound thin-film material - Google Patents
A kind of preparation method of molybdenum silicide transistion metal compound thin-film material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
Abstract
The present invention relates to a kind of preparation methods of molybdenum silicide transistion metal compound thin-film material, it is characterized by: under vacuum conditions, with the metal molybdenum target material of high-energy electron beam heating high-purity, metal molybdenum target material is set to gasify, surface of silicon of the molybdenum vapor deposition of evaporation in high-purity, the annealing for finally carrying out 350~900 DEG C in air, can form silication molybdenum film;The preparation method of the molybdenum silicide transistion metal compound thin-film material is that upper one layer of metal molybdenum directly is deposited in surface of silicon, and method is easy, process is convenient, and film deposition thickness is controllable, and quality of forming film is good, Elemental redistribution is uniform, and annealed processing has obtained molybdenum silicide transition metal oxide film;The advantages that film of used magnetically controlled sputter method preparation compared with the prior art, has purity is high, and high-quality, annealing temperature is low, reproducible.
Description
Technical field
The present invention relates to the technical fields of the preparation and representation of material, and in particular to a kind of molybdenum silicide transistion metal compound
The preparation method of thin-film material.
Background technique
Molybdenum disilicide since the atomic radius of silicon atom is larger, therefore can't be gold as a kind of transistion metal compound
Belong to the interstitial atom in dot matrix, therefore also referred to as " fill compound ".This special structure, causes it to possess special object
Physicochemical property makes the fusing point of this compound and hardness greatly exceed its basis material.Its superior physical property, it is such as molten
Point is high, and density is low, and hardness is big, and resistivity is low, and thermal expansion coefficient is small, and high temperature properties are stablized, and electrical and thermal conductivity is good, has under high temperature
The features such as inoxidizability and corrosion resistance.Molybden silicide material is fully applicable to the multiple fields such as aerospace, the energy, military affairs,
Often it is used to manufacture high temperature exothermic element, turbo blade, combustion chamber, high temperature protection coating material and Wear-resistant corrosion-resistant material etc..
Exploration in terms of high-temperature stability makes some progress.The characteristic research of two-dimentional molybdenum silicide thin-film material and application are also very
There is prospect.
With gradualling mature for semiconductor technology, molybdenum silicide is increasingly closer in conjunction with semiconductor technology.Due to silication
There is molybdenum film material excellent electric conductivity therefore would be possible to replace Al, Cu and polysilicon super as a new generation deep-submicron 3D
The lead of large scale integrated circuit (3DVLSI) and outer connecting material.Meanwhile molybdenum silicide quartz mask plate is as a kind of novel
Photomask blank is superior to conventional chromium exposure mask in terms of chemical durability and dry etching characteristic.Amorphous state silication molybdenum film is made super
Lead single-photon detector SSPD etc..General integrated circuit will carry out 1000 DEG C or more of high-temperature process, resistance to height in the fabrication process
The MoSi of temperature characteristics2It is one of the ideal material for making integrated circuit gate.So to molybdenum silicide thin-film material and semiconductor work
The research and discovery that skill is integrated has far reaching significance.
Summary of the invention
It is an object of the present invention to provide a kind of preparation methods of molybdenum silicide transistion metal compound thin-film material, in vacuum condition
Under, with the metal molybdenum target material of high-energy electron beam heating high-purity, so that metal molybdenum target material is gasified, the molybdenum vapor deposition of evaporation is high-purity
The surface of silicon of degree finally carries out 350~900 DEG C of annealing in air, can form silication molybdenum film.
The detailed process of above-mentioned molybdenum silicide transistion metal compound thin-film material preparation method is:
S1, the high purity silicon substrate cleaned is placed in apparatus for electron beam evaporation, the metal molybdenum target material of high-purity is put into copper
In crucible;
S2, vacuumize process is carried out to cavity, its vacuum degree is made to be down to 1 × 10-3Pa is hereinafter, simultaneously using resistance wire to high-purity
Degree silicon substrate is heated to 300 DEG C and maintains constant temperature;
S3, metal molybdenum target material is melted in advance using electron gun launching electronics beam;
Plasma processing is carried out after S4, pre- melt beam, this effect is generated when being the intracavitary residual gas of cleaning and melting in advance
Useless molybdenum steam;
S5, setting coating process parameter, start plated film;
S6, the annealing that the sample being prepared is carried out to 350~900 DEG C in air, can form silication molybdenum film.
The metal molybdenum target material of the high-purity, the purity of high purity silicon substrate are 99.95% or more.
The high purity silicon substrate is single-sided polishing Si (100) single-chip, resistivity 10kcm.
The area of the high purity silicon substrate is 4 × 4cm2。
The high purity silicon substrate detailed process cleaned is: silicon substrate is put into equipped with the concentrated sulfuric acid and hydrogen peroxide ratio
In the mixed solution of 3:1, to be heated to 120 DEG C of boilings on high temperature furnace, the duration is 8 minutes.Then respectively in acetone, nothing
It is cleaned by ultrasonic 15 minutes in water-ethanol and deionized water.
The concentrated sulfuric acid concentration is 96%, hydrogen peroxide concentration 30%.
The metal molybdenum target material is 75~100cm at a distance from silicon substrate.
The operating voltage of the electron gun is 7.8~8.2kv, and electric current is 390~410mA.
Beneficial effects of the present invention: the preparation side of this molybdenum silicide transistion metal compound thin-film material provided by the invention
Method is that upper one layer of metal molybdenum directly is deposited in surface of silicon, and then annealed processing forms silication molybdenum film.Preparation method is held
Easily, process is convenient, and film deposition thickness is controllable, and quality of forming film is good, and Elemental redistribution is uniform;Used magnetic compared with the prior art
The advantages that silication molybdenum film for controlling sputtering method preparation, with purity is high, high-quality, annealing temperature is low, reproducible;It is prepared
It is integrated that the molybdenum silicide transistion metal compound thin-film material of acquisition can be used for making the raw material of heat-resisting material, especially semiconductor
Grid material needed for meeting transistor high-temperature processing technology in circuit technology.
The present invention is described in further details below with reference to attached drawing.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of the molybdenum silicide transistion metal compound film prepared.
Fig. 2 is the Raman spectrogram of the molybdenum silicide transistion metal compound film prepared.
Fig. 3 is the scanning electron microscope diagram one of the molybdenum silicide transistion metal compound film prepared.
Fig. 4 is the scanning electron microscope diagram two of the molybdenum silicide transistion metal compound film prepared.
Fig. 5 is the scanning electron microscope diagram three of the molybdenum silicide transistion metal compound film prepared.
Fig. 6 is the scanning electron microscope diagram four of the molybdenum silicide transistion metal compound film prepared.
Fig. 7 is the scanning electron microscope diagram five of the molybdenum silicide transistion metal compound film prepared.
Fig. 8 is the scanning electron microscope diagram one of the molybdenum silicide transistion metal compound film cross section prepared.
Fig. 9 is the scanning electron microscope diagram two of the molybdenum silicide transistion metal compound film cross section prepared.
Figure 10 is the scanning electron microscope diagram three of the molybdenum silicide transistion metal compound film cross section prepared.
Figure 11 is the scanning electron microscope diagram four of the molybdenum silicide transistion metal compound film cross section prepared.
Figure 12 is the scanning electron microscope diagram five of the molybdenum silicide transistion metal compound film cross section prepared.
Specific embodiment
Reach the technical means and efficacy that predetermined purpose is taken for the present invention is further explained, below in conjunction with attached drawing and reality
Example is applied to a specific embodiment of the invention, structure feature and its effect, detailed description are as follows.
Embodiment 1
A kind of preparation method such as Fig. 1~Figure 12 molybdenum silicide transistion metal compound thin-film material is present embodiments provided, true
Under empty condition, with the metal molybdenum target material of high-energy electron beam heating high-purity, metal molybdenum target material is set to gasify, the molybdenum vapor deposition of evaporation
In the surface of silicon of high-purity, 350~900 DEG C of annealing is finally carried out in air, can form silication molybdenum film.
The preparation method of the molybdenum silicide transistion metal compound thin-film material prepares the detailed process of silication molybdenum film
It is:
S1, the high purity silicon substrate cleaned is placed in apparatus for electron beam evaporation, the metal molybdenum target material of high-purity is put into copper
In crucible;
S2, vacuumize process is carried out to cavity, its vacuum degree is made to be down to 1 × 10-3Pa is hereinafter, simultaneously using resistance wire to high-purity
Degree silicon substrate is heated to 300 DEG C and maintains constant temperature, and stress factor causes film quality poor when reducing plated film;
S3, metal molybdenum target material is melted using electron gun launching electronics beam in advance, makes pre- to melt metal surface uniform ground, Ke Yiti
It is high more evenly and more stable boil-off gas;
Plasma processing is carried out after S4, pre- melt beam, this effect is generated when being the intracavitary residual gas of cleaning and melting in advance
Useless molybdenum steam;
S5, setting coating process parameter control the evaporation rate of molybdenum steam and use crystal oscillator monitoring film deposition thickness, start
Plated film;Detailed process is: by adjusting the size of electron beam current density to control the rate of molybdenum steam raising, in cavity
There is a kind of crystal-vibration-chip to can detecte the deposition thickness of plated film, when its deposition thickness reaches set film thickness, deposition
It is automatically stopped;Having around silicon substrate can play the role of heating substrate after one week resistance wire of vacuum cavity, galvanization;
In evaporation process, the temperature of silicon substrate is maintained 300 DEG C using the method for upper baking, to reduce membrane stress, improves film forming
Quality.
S6, the annealing that the sample being prepared is carried out to 350~900 DEG C in air, it is thin can to form molybdenum silicide
Film;It anneals in air, metal molybdenum and silicon substrate phase counterdiffusion can be promoted, form molybdenum silicide;In addition, the oxygen in air also can
Oxidation reaction occurs with metal molybdenum film or the silicon atom for being diffused into molybdenum film, forms molybdenum trioxide and silica.Three oxygen
Changing molybdenum can form at low temperature, in 500 DEG C of beginning steam raisings.And silica is about initially formed at 600 degree, dioxy
SiClx film forming is mainly formed in film surface, finer and close, oxygen can be prevented further to penetrate into film, thus prevents three
This process of the formation and steam raising of molybdenum oxide.And molybdenum silicide is increased to 1400 degree with annealing temperature, all exists always.Thus
We select 350~900 degree to make annealing treatment sample, and main purpose is to observe film to consolidate with what annealing temperature variation occurred
Phase reaction.As for annealing time, we select 1 hour, primarily to film solid phase reaction can be carried out sufficiently.
Further, the metal molybdenum target material of the high-purity, the purity of high purity silicon substrate are 99.95% or more.
Further, the high purity silicon substrate is single-sided polishing Si (100) single-chip, resistivity 10kcm.
Further, the area of the high purity silicon substrate is 4 × 4cm2。
The high purity silicon substrate detailed process cleaned is: by 4 × 4cm2The silicon substrate of size is put into equipped with concentration
It is 30% hydrogen peroxide for 96% concentrated sulfuric acid and concentration, ratio is that 120 DEG C of boilings are heated on high temperature furnace in the mixed solution of 3:1,
Duration is 8 minutes.Then it is cleaned by ultrasonic 15 minutes in acetone, dehydrated alcohol and deionized water respectively.
The metal molybdenum target material is 75~100cm at a distance from silicon substrate.Metal molybdenum target material is at a distance from electron gun filament
For 20~30mm;Since electron beam heats molybdenum, silicon substrate apart from metal molybdenum target material it is too close in the case where, the molybdenum that has just been evaporated
For steam since rate is too fast, rate of film build is more difficult to control, may will affect quality of forming film and the uniformity.In addition, some are evaporated
Material is even due to uneven heating, it may occur that the phenomenon that explosion collapses, the evaporation material collapsed splashes on substrate, will affect quality of forming film.
When substrate and evaporation material distance are between 75~100cm, at this point, the opposing gas of the climbing speed of molybdenum steam and molybdenum steam
Density can more evenly can play the role of the growth of film advantageous.
The operating voltage of the electron gun is 7.8~8.2kv, and electric current is 390~410mA, can maintain deposition speed at this time
Rate is 0.06nm/s or so;Deposition rate can have certain influence to the growth pattern of film.If film thickness is larger, using elder generation
Small speed, rear big speed may improve film quality;But if thickness is smaller (30 nanometers), film is influenced with regard to very little.
Embodiment 2
Using electron beam evaporation method, the metal molybdenum powder that purity is 99.95% is mounted in graphite crucible, it will be through surface cleaning processing
The silicon substrate crossed is fixed on pedestal, keeps underlayer temperature at 300 DEG C, and control electron gun filament size of current is 400mA, deposition
Rate is 0.06nm/s, make to deposit metal molybdenum film on a silicon substrate with a thickness of 30nm.
Embodiment 3
In the present embodiment, annealing is carried out in 350 DEG C of air atmosphere 1 hour, heating rate is set in annealing process as 5
DEG C/min, 10 minutes are kept the temperature when temperature reaches 300 DEG C, with furnace Temperature fall.
Embodiment 4
In the present embodiment, annealing is carried out in 500 DEG C of air atmosphere 1 hour, heating rate is set in annealing process as 5
DEG C/min, 10 minutes are kept the temperature when temperature reaches 300 DEG C, with furnace Temperature fall.
Embodiment 5
In the present embodiment, annealing is carried out in 600 DEG C of air atmosphere 1 hour, heating rate is set in annealing process as 5
DEG C/min, 10 minutes are kept the temperature when temperature reaches 300 DEG C, with furnace Temperature fall.
Embodiment 6
In the present embodiment, annealing is carried out in 700 DEG C of air atmosphere 1 hour, heating rate is set in annealing process as 5
DEG C/min, 10 minutes are kept the temperature when temperature reaches 300 DEG C, with furnace Temperature fall.
Embodiment 7
In the present embodiment, annealing is carried out in 900 DEG C of air atmosphere 1 hour, heating rate is set in annealing process as 5
DEG C/min, 10 minutes are kept the temperature when temperature reaches 300 DEG C, then with furnace Temperature fall.
Embodiment 8
Using X-ray diffractometer, Raman spectrum analysis instrument, the silication molybdenum film that scanning electron microscope prepares embodiment 2 ~ 6
It is analyzed, characterization result is shown in Fig. 1~Figure 12.Fig. 1 is oriented to the results show that being prepared under lower annealing temperature
(202) MoSi2Film, with gradually rising for annealing temperature, diffraction maximum is gradually decreased.Fig. 2 is the results show that be located at 521cm-1
And 950cm-1The absorption peak at place represents the peak Si, and annealing temperature is at 600 DEG C or more, MoO3Caused vibration peak disappears, this be by
In two-dimensional film structure MoO3Boiling point reduce, lead to MoO3The steam raising in 500 DEG C of annealing, has left film.Fig. 3~Fig. 7
The results show that film porosity becomes smaller with the raising of annealing temperature, consistency improves.This may be due to MoO3Gasification
Evaporation Phenomenon is just will form under 500 DEG C of annealing temperatures, and with the raising of annealing temperature, sample surfaces can gradually form one layer
Fine and close silicon dioxide layer of protection, the protective layer can prevent extraneous oxygen from penetrating into film, form MoO3, thus MoO3Evaporation tails off, hole
Gap becomes smaller.For Fig. 8~Figure 12 the results show that when annealing temperature is 500 DEG C, molybdenum element, which absorbs a large amount of oxygen element, causes film to become
Thickness, with the raising of annealing temperature, deep layer molybdenum element is more readily permeable into silicon layer, and the silicon dioxide layer of protection generated completely cuts off
The thickening phenomenon that the entrance of oxygen causes film slight.Electron beam evaporation method prepares silication molybdenum film, is banged using high energy electron rifle
Metal targets are hit, makes metal molybdenum steam raising, is deposited on surface of silicon.Compared to magnetically controlled sputter method, the particle obtained
It is smaller and more evenly.By accurately controlling the deposition rate of molybdenum steam to optimize the growth pattern of film, film quality is promoted.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (9)
1. a kind of preparation method of molybdenum silicide transistion metal compound thin-film material, it is characterised in that: under vacuum conditions, with height
Can electron beam heated high-purity metal molybdenum target material, so that metal molybdenum target material is gasified, the silicon of the molybdenum vapor deposition of evaporation in high-purity
Substrate surface finally carries out 350~900 DEG C of annealing in air, can form silication molybdenum film.
2. the preparation method of molybdenum silicide transistion metal compound thin-film material as described in claim 1, which is characterized in that preparation
The detailed process of silication molybdenum film is:
S1, the high purity silicon substrate cleaned is placed in apparatus for electron beam evaporation, the metal molybdenum target material of high-purity is put into copper
In crucible;
S2, vacuumize process is carried out to cavity, its vacuum degree is made to be down to 1 × 10-3Pa is hereinafter, simultaneously using resistance wire to high-purity
Silicon substrate is heated to 300 DEG C and maintains constant temperature;
S3, metal molybdenum target material is melted in advance using electron gun launching electronics beam;
Plasma processing is carried out after S4, pre- melt beam, this effect is generated when being the intracavitary residual gas of cleaning and melting in advance
Useless molybdenum steam;
S5, setting coating process parameter, start plated film;
S6, the annealing that the sample being prepared is carried out to 350~900 DEG C in air, can form silication molybdenum film.
3. the preparation method of molybdenum silicide transistion metal compound thin-film material as claimed in claim 2, it is characterised in that: described
The metal molybdenum target material of high-purity, the purity of high purity silicon substrate are 99.95% or more.
4. the preparation method of molybdenum silicide transistion metal compound thin-film material as claimed in claim 2, it is characterised in that: described
High purity silicon substrate is single-sided polishing Si (100) single-chip, resistivity 10kcm.
5. the preparation method of molybdenum silicide transistion metal compound thin-film material as claimed in claim 2, it is characterised in that: described
The area of high purity silicon substrate is 4 × 4cm2。
6. the preparation method of molybdenum silicide transistion metal compound thin-film material as claimed in claim 2, it is characterised in that: described
The high purity silicon substrate detailed process cleaned is: silicon substrate is put into the mixing for being 3:1 equipped with the concentrated sulfuric acid and hydrogen peroxide ratio
In solution, 120 DEG C of boilings are heated on high temperature furnace, the duration is 8 minutes;Then it respectively in acetone, dehydrated alcohol and goes
It is cleaned by ultrasonic 15 minutes in ionized water.
7. the preparation method of molybdenum silicide transistion metal compound thin-film material as claimed in claim 6, it is characterised in that: described
Concentrated sulfuric acid concentration is 96%, hydrogen peroxide concentration 30%.
8. the preparation method of molybdenum silicide transistion metal compound thin-film material as claimed in claim 2, it is characterised in that: described
Metal molybdenum target material is 75~100cm at a distance from silicon substrate.
9. the preparation method of molybdenum silicide transistion metal compound thin-film material as claimed in claim 2, it is characterised in that: described
The operating voltage of electron gun is 7.8~8.2kv, and electric current is 390~410mA.
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CN112798116A (en) * | 2021-01-13 | 2021-05-14 | 南京大学 | Intermediate infrared superconducting nanowire single photon detector |
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Cited By (3)
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CN111270207A (en) * | 2020-02-17 | 2020-06-12 | 西安邮电大学 | Preparation method of high-entropy alloy thin film material with layered structure |
CN112798116A (en) * | 2021-01-13 | 2021-05-14 | 南京大学 | Intermediate infrared superconducting nanowire single photon detector |
CN112798116B (en) * | 2021-01-13 | 2022-03-18 | 南京大学 | Intermediate infrared superconducting nanowire single photon detector |
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