CN108428736A - One kind being based on n-VO2The heterojunction structure and preparation method of/p-NiO - Google Patents
One kind being based on n-VO2The heterojunction structure and preparation method of/p-NiO Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 69
- 239000010408 film Substances 0.000 claims abstract description 243
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 83
- 239000010935 stainless steel Substances 0.000 claims abstract description 83
- 239000000758 substrate Substances 0.000 claims abstract description 77
- 239000010409 thin film Substances 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 27
- 229910010037 TiAlN Inorganic materials 0.000 claims abstract description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 84
- 239000007789 gas Substances 0.000 claims description 77
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 58
- 239000001301 oxygen Substances 0.000 claims description 58
- 229910052760 oxygen Inorganic materials 0.000 claims description 58
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 54
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 42
- 229910052786 argon Inorganic materials 0.000 claims description 42
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 35
- 238000005546 reactive sputtering Methods 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000011787 zinc oxide Substances 0.000 claims description 27
- 239000004411 aluminium Substances 0.000 claims description 23
- 229910052782 aluminium Inorganic materials 0.000 claims description 23
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 23
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 claims description 17
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 claims description 17
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 16
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 12
- 229910000831 Steel Inorganic materials 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 239000010959 steel Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 3
- 238000009738 saturating Methods 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 230000002000 scavenging effect Effects 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 229910001882 dioxygen Inorganic materials 0.000 claims 1
- 239000013077 target material Substances 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 17
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000011241 protective layer Substances 0.000 abstract description 3
- 230000005693 optoelectronics Effects 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 9
- 238000000151 deposition Methods 0.000 description 7
- 230000008021 deposition Effects 0.000 description 7
- 239000000523 sample Substances 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 239000006101 laboratory sample Substances 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000011149 active material Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/26—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, elements provided for in two or more of the groups H01L29/16, H01L29/18, H01L29/20, H01L29/22, H01L29/24, e.g. alloys
- H01L29/267—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, elements provided for in two or more of the groups H01L29/16, H01L29/18, H01L29/20, H01L29/22, H01L29/24, e.g. alloys in different semiconductor regions, e.g. heterojunctions
-
- 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
- H01L21/02425—Conductive materials, e.g. metallic silicides
-
- 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
- H01L21/02483—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
-
- 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
- H01L21/02565—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
-
- 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
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Laminated Bodies (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The present invention relates to one kind being based on n VO2The heterojunction structure and preparation method of/p NiO includes TiAlN thin film, the first AZO transparent conductive film, VO successively from upper layer to lower layer2Film, p NiO films, the second AZO transparent conductive film and flexible stainless steel substrate.Wherein：P NiO films are buffer layer, and TiAlN thin film is protective layer, and the first AZO transparent conductive film and the second AZO transparent conductive film are used as conductive electrode and slow down layer.N VO of the present invention2/ P NiO heterojunction structures combine flexible stainless steel material and its technology of preparing, flexible high-power device can be prepared, the device has wide application in high-power optoelectronic switch, high-power cheap light storage device etc., solves the problems, such as that device power is low, long lifespan.
Description
Technical field
The invention belongs to the manufacturing technology field of reversible semiconductor to metal (SMT) first order transition coating, more particularly to one
Kind is based on n-VO2The heterojunction structure and preparation method of/p-NiO.
Background technology
Vanadium dioxide (VO2) the reversible semiconductor of temperature driving occurs under the critical-temperature (Tc) of 341K to metal
(SMT) first order transition, and along with the change of crystal symmetry.At a temperature of less than Tc, VO2In monocline crystalline phase (P21/
C) semiconductor form, the wherein energy gap of V atom pairs are 0.6eV.At a temperature of higher than Tc, VO2In tetragonal crystal system
(P42/mnm) metallic state, wherein the overlapping between fermi level and V3d bands eliminates above-mentioned band gap.This crystal symmetry
The suddenly change that transition with electron band structure is usually transmitted along with its resistivity and near-infrared.Therefore, VO2For a long time by
The critical material being considered in intellectual material relies on these unique performances, VO2Film has been widely studied.
It is well known that the electrical and optical properties of film of the selection of substrate to being grown have important influence.Due to it
Broad-band gap (3.39eV) and some other excellent performances, nickel oxide (NiO) are the important semi-conducting materials of a new generation.Especially
Ground, the advantages of due to it with higher reliability, longer service life and lower power consumption, currently based on the photoelectricity of NiO
Son and some new applications of microelectronic component.In solidstate electronics and photoelectronics and have no n-VO2/ p-NiO is combined different
Matter structure is used for as the novel device in solidstate electronics and photoelectronics.
In addition, the oxide with switching characteristic is integrated also to the emerging device based on photon chamber and active material table
Reveal huge potentiality.High power device flexibility in the prior art is poor, switching speed is low, driving power is big, driving circuit is multiple
Miscellaneous, switching frequency is low, but also there is a problem of that service life is low.
Invention content
In order to solve the deficiency in the prior art, the present invention provides a kind of based on n-VO2The heterojunction structure and system of/p-NiO
Preparation Method.
The purpose of the present invention is achieved through the following technical solutions：
One kind being based on n-VO2The heterojunction structure of/p-NiO is transparent including TiAlN thin film, the first AZO successively from upper layer to lower layer
Conductive film, VO2Film, p-NiO films, the second AZO transparent conductive film and flexible stainless steel substrate.
Further, the p-NiO films are buffer layer, and TiAlN thin film is protective layer, the first AZO transparent conductive film and the
Two AZO transparent conductive films are used as conductive electrode and slow down layer.
One kind being based on n-VO2The preparation method of the heterojunction structure of/p-NiO is sequentially prepared on flexible stainless steel substrate
Two AZO transparent conductive films, p-NiO films, VO2Film, the first AZO transparent conductive film and TiAlN thin film.
Further, the second AZO transparent conductive film is prepared, flexible stainless steel substrate is used into ethyl alcohol, deionized water successively
Ultrasonic cleaning is carried out, uses EtOH Sonicate scavenging period for 5 minutes, the 5 minutes deionized water ultrasonic cleaning time, using nitrogen
Air-blowing is dry to be sent into magnetron sputtering reative cell, 1.0 × 10-3It is anti-using argon gas and oxygen as mixed gas under conditions of Pa vacuum
Ying Yuan, argon gas and oxygen flow ratio 8:1-10：1, using Zinc oxide doped aluminium as target, the Zinc oxide doped aluminium target of reactive sputtering
Purity be 99.9%, preparation temperature be 200 DEG C~400 DEG C, preparation time be 60 minutes~80 minutes, obtain flexible stainless steel
The AZO transparent conductive film of substrate/second.
Further, p- is prepared in the AZO transparent conductive film of flexible stainless steel substrate/second using magnetron sputtering reative cell
NiO films, 1.0 × 10-3Under conditions of Pa vacuum, using oxygen as gas reaction source, oxygen flow be 80sccm~
120sccm, using nickel oxide as target, the purity of reactive sputtering nickel oxide target is 99.9%, and preparation temperature is 200 DEG C~400
DEG C, preparation time 30 minutes~180 minutes obtains flexible stainless steel substrate/second AZO transparent conductive film/p-NiO films.
Further, thin in flexible stainless steel substrate/second AZO transparent conductive film/p-NiO using magnetron sputtering reative cell
VO is prepared on membrane material2Thin-film material, 1.0 × 10-3Under conditions of Pa vacuum, VO is prepared2Thin-film material, with argon gas and oxygen
As mixed gas reaction source, argon gas and oxygen flow ratio 8:1-10：1, using vanadium dioxide as target, reactive sputtering vanadium dioxide
The purity of target is 99.9%, and preparation temperature is 100 DEG C~300 DEG C, and preparation time is -250 minutes 200 minutes, obtains flexibility
Stainless steel substrate/the second AZO transparent conductive film/p-NiO films/VO2Film.
Further, thin in flexible stainless steel substrate/second AZO transparent conductive film/p-NiO using magnetron sputtering reative cell
Film/VO2The first AZO transparent conductive film is prepared on film, using argon gas and oxygen as mixed gas reaction source, argon gas and oxygen
Flow-rate ratio 5:1~8:1, using Zinc oxide doped aluminium as target, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, system
Standby temperature is 100 DEG C~300 DEG C, and preparation time is 30 minutes~50 minutes, and it is transparent to obtain flexible stainless steel substrate/the 2nd AZO
Conductive film/p-NiO films/VO2The AZO transparent conductive film of film/first.
Further, thin in flexible stainless steel substrate/second AZO transparent conductive film/p-NiO using magnetron sputtering reative cell
Film/VO2TiN anti-corrosion protection coatings are prepared in the AZO transparent conductive film of film/first, with nitrogen as gas reaction source, nitrogen
Throughput is 30~80sccm, and using titanium nitride as target, the purity of reactive sputtering titanium nitride target is 99.99%, preparation temperature
It it is 100 DEG C~400 DEG C, preparation time is 20 minutes~30 minutes, and it is thin to obtain flexible stainless steel substrate/the 2nd AZO electrically conducting transparents
Film/p-NiO films/VO2Film/the first AZO transparent conductive film/TiAlN thin film.
Beneficial effects of the present invention：N-VO of the present invention2/ P-NiO heterojunction structures combine flexible stainless steel material as substrate,
The device for preparing high quality and low cost, using P-NiO films as buffer layer, on the one hand can alleviate flexible stainless steel with
VO2Adhesiveness between film controls VO on the other hand in order to adjust the partial pressure of oxygen of sputtering process2The resistivity of film is partly being led
Within the scope of body, using P-NiO films as buffer layer deposition in flexible stainless steel and VO2Between film, on the one hand it can alleviate
Flexible stainless steel and VO2The big problem of material lattice mismatch, can prepare the VO of high quality2Film, it is viscous so as to prepare
The VO that attached property is high, film forming area is big2Film, P-NiO films are at low cost as buffer layer, and environmentally friendly not generation environment is dirty
Dye.
The present invention uses conductive electrode of the AZO transparent conductive film as device, one side AZO transparent conductive film to have
The controllable resistor rate changed with partial pressure of oxygen in deposition process；Another aspect AZO transparent conductive film is as non-crystal transparent conductive oxygen
Compound is conductive to be increased substantially, resistivity can reduce, be easy to large area film forming, and AZO transparent conductive film also has
Higher deposition rate, low underlayer temperature and between flexible stainless steel have good substrate adhesion.
TiAlN thin film is finally deposited in the present invention, and one side TiAlN thin film hardness is big, and corrosion resistance is strong, efficiently solves device
Etching problem carries out protective effect to device, further improves the service life of device, another aspect TiAlN thin film and AZO are saturating
The degrees of fusion of bright conductive film is high, enhances n-VO2The stability of/P-NiO heterojunction structures.
The present invention is an important semiconductor using nickel oxide (NiO).Particularly, since it is with higher reliability,
Longer service life and lower power consumption and low-cost advantage, using VO2/ p-NiO/ flexibility stainless steel substrate hetero-junctions
N-type VO had both been utilized in structure2To the characteristic of metal (SMT) first order transition and p-NiO is utilized in the reversible semiconductor of temperature driving
Structural reliability, high-power, long-life, low power consumption and low-cost feature, in combination with flexible stainless steel substrate
Flexibility, in high-power optoelectronic switch, high-power cheap light storage device etc. has wide the device that three combines
Using solving the problems, such as low device power, short life and flexible poor.
Description of the drawings
Fig. 1 is n-VO of the present invention2The structural schematic diagram of the heterojunction structure of/p-NiO；
Fig. 2 is 1n-VO of the embodiment of the present invention2The atomic force microscope microscope figure of/P-NiO heterojunction structures；
Fig. 3 is 2n-VO of the embodiment of the present invention2The atomic force microscope microscope figure of/P-NiO heterojunction structures；
Fig. 4 is 3n-VO of the embodiment of the present invention2The atomic force microscope microscope figure of/P-NiO heterojunction structures；
Fig. 5 is 4n-VO of the embodiment of the present invention2The atomic force microscope microscope figure of/P-NiO heterojunction structures；
Fig. 6 is 1n-VO of the embodiment of the present invention2The electron microscope microscope figure of/P-NiO heterojunction structures；
Fig. 7 is 2n-VO of the embodiment of the present invention2The electron microscope microscope figure of/P-NiO heterojunction structures；
Fig. 8 is 3n-VO of the embodiment of the present invention2The electron microscope microscope figure of/P-NiO heterojunction structures.
Wherein:1, flexible stainless steel substrate, the 2, second AZO transparent conductive film, 3, p-NiO films, 4, VO2Film, 5,
First AZO transparent conductive film, 6, TiAlN thin film.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The model of laboratory sample test of the present invention atomic force microscope (AFM) used is the production of Agilent companies
Picoscan 2500.Film sample is tested and is analyzed under the test condition of normal room temperature, the test analysis of sample
Region is 2 μm of 2 μ m.
The model for the SEM used in sample test that the present invention utilizes is JSM-6360LV, is produced in Japan.Device parameter is
The accelerating potential of 0.5-30kV, the amplification factor that ten thousand times of 8-30, the secondary electron resolution ratio under conditions of high low vacuum are respectively
3nm and 4nm.
One kind being based on n-VO2The heterojunction structure of/p-NiO includes TiAlN thin film 6, the successively from upper layer to lower layer referring to Fig. 1
One AZO transparent conductive film 5, VO2Film 4, p-NiO films 3, the second AZO transparent conductive film 2 and flexible stainless steel substrate
1, wherein：The p-NiO films 3 are buffer layer, and TiAlN thin film 6 is protective layer, the first AZO transparent conductive film 5 and the 2nd AZO
Transparent conductive film 6 is used as conductive electrode and slows down layer.
One kind being based on n-VO2The preparation method of the heterojunction structure of/p-NiO：
Embodiment 1
1), ethyl alcohol, deionized water is used to carry out ultrasonic cleaning successively flexible stainless steel substrate, it is clear using EtOH Sonicate
It is 5 minutes to wash the time, and magnetron sputtering reative cell is sent into 5 minutes deionized water ultrasonic cleaning time, nitrogen drying, 1.0 ×
10-3Under conditions of Pa vacuum, deposition prepares AZO transparent conductive film on its flexible stainless steel；Its technological parameter condition is：With
Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, use Zinc oxide doped aluminium for target, instead
It is 99.9% to answer the purity of sputtering zinc oxide adulterated al target, and preparation temperature is 200 DEG C, and preparation time is 60 minutes, is obtained soft
The AZO transparent conductive film of property stainless steel substrate/second.
2), using magnetron sputtering reative cell it is above-mentioned 1) in obtained flexible stainless steel substrate/the 2nd AZO electrically conducting transparents it is thin
P-NiO thin-film materials are prepared on film, 1.0 × 10-3Under conditions of Pa vacuum, technological parameter condition is：Using oxygen as gas
Precursor reactant source, oxygen flow 80sccm use nickel oxide for target, and the purity of reactive sputtering nickel oxide target is
99.9%, preparation temperature is 200 DEG C, preparation time 30 minutes, obtain the AZO transparent conductive film of flexible stainless steel substrate/second/
P-NiO films.
3), using magnetron sputtering reative cell it is above-mentioned 2) in obtained flexible stainless steel substrate/the 2nd AZO electrically conducting transparents it is thin
VO is prepared on film/p-NiO thin-film materials2Thin-film material, 1.0 × 10-3Under conditions of Pa vacuum, technological parameter condition is：
Using argon gas and oxygen as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, using vanadium dioxide as target, reactive sputtering
The purity of vanadium dioxide target is 99.9%, and preparation temperature is 100 DEG C, and preparation time is 200 minutes, obtains flexible stainless base steel
Piece/the second AZO transparent conductive film/p-NiO thin-film materials/VO2Thin-film material.
4), continue using magnetron sputtering reative cell it is above-mentioned 3) in obtain flexible stainless steel substrate/the 2nd AZO is transparent leads
Conductive film/p-NiO thin-film materials/VO2The first AZO transparent conductive film is prepared on thin-film material, 1.0 × 10-3Pa vacuum
Under the conditions of, continue to prepare AZO transparent conductive film.Its technological parameter condition is：Using argon gas and oxygen as mixed gas reaction
Source, argon gas and oxygen flow ratio 5:1, using Zinc oxide doped aluminium as target, the purity of the Zinc oxide doped aluminium target of reactive sputtering is
99.9%, preparation temperature is 100 DEG C, and preparation time is 30 minutes, and it is thin to obtain flexible stainless second steel substrate/AZO electrically conducting transparents
Film/p-NiO thin-film materials/VO2The AZO transparent conductive film of thin-film material/first.
5), continue using magnetron sputtering reative cell it is above-mentioned 4) in obtain flexible stainless steel substrate/the 2nd AZO is transparent leads
Conductive film/p-NiO thin-film materials/VO2TiAlN thin film, technological parameter are prepared in the AZO transparent conductive film of thin-film material/first
Condition is：With nitrogen as gas reaction source, nitrogen flow 30sccm, using titanium nitride as target, reactive sputtering nitrogenizes titanium target
The purity of material is 99.99%, and underlayer temperature is 100 DEG C, and preparation time is 20 minutes, obtains the AZO of flexible stainless steel substrate/the 2nd
Transparent conductive film/p-NiO thin-film materials/VO2Thin-film material/the first AZO transparent conductive film/TiAlN thin film, obtains n-VO2/
P-NiO heterojunction structures laboratory sample 1.
Embodiment 2
1), ethyl alcohol, deionized water is used to carry out ultrasonic cleaning successively flexible stainless steel substrate, it is clear using EtOH Sonicate
It is 5 minutes to wash the time, and magnetron sputtering reative cell is sent into 5 minutes deionized water ultrasonic cleaning time, nitrogen drying, 1.0 ×
10-3Under conditions of Pa vacuum, deposition prepares AZO transparent conductive film on its flexible stainless steel；Its technological parameter condition is：With
Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 9:1, use Zinc oxide doped aluminium for target, instead
It is 99.9% to answer the purity of sputtering zinc oxide adulterated al target, and preparation temperature is 250 DEG C, and preparation time is 70 minutes, is obtained soft
The AZO transparent conductive film of property stainless steel substrate/second.
2), using magnetron sputtering reative cell it is above-mentioned 1) in obtained flexible stainless steel substrate/the 2nd AZO electrically conducting transparents it is thin
P-NiO thin-film materials are prepared on film, 1.0 × 10-3Under conditions of Pa vacuum, technological parameter condition is：Using oxygen as gas
Precursor reactant source, oxygen flow 90sccm use nickel oxide for target, and the purity of reactive sputtering nickel oxide target is
99.9%, preparation temperature is 250 DEG C, preparation time 60 minutes, obtain the AZO transparent conductive film of flexible stainless steel substrate/second/
P-NiO films.
3), using magnetron sputtering reative cell it is above-mentioned 2) in obtained flexible stainless steel substrate/the 2nd AZO electrically conducting transparents it is thin
VO is prepared on film/p-NiO films2Film, 1.0 × 10-3Under conditions of Pa vacuum, technological parameter condition is：With argon gas and
Oxygen is as mixed gas reaction source, argon gas and oxygen flow ratio 9:1, using vanadium dioxide as target, reactive sputtering vanadium dioxide
The purity of target is 99.9%, and preparation temperature is 250 DEG C, and preparation time is 220 minutes, obtains flexible stainless steel substrate/the second
AZO transparent conductive film/p-NiO films/VO2Film.
4), continue using magnetron sputtering reative cell it is above-mentioned 3) in obtain flexible stainless steel substrate/the 2nd AZO is transparent leads
Conductive film/p-NiO films/VO2The first AZO transparent conductive film is prepared on film, 1.0 × 10-3Under conditions of Pa vacuum, after
It is continuous to prepare AZO transparent conductive film.Its technological parameter condition is：Using argon gas and oxygen as mixed gas reaction source, argon gas and
Oxygen flow is than 6:1, using Zinc oxide doped aluminium as target, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, system
Standby temperature is 200 DEG C, and preparation time is 40 minutes, and it is thin to obtain flexible stainless steel substrate/second AZO transparent conductive film/p-NiO
Film/VO2The AZO transparent conductive film of film/first.
5), continue using magnetron sputtering reative cell it is above-mentioned 4) in obtain flexible stainless steel substrate/the 2nd AZO is transparent leads
Conductive film/p-NiO films/VO2TiAlN thin film is prepared in the AZO transparent conductive film of film/first, technological parameter condition is：With
Nitrogen is as gas reaction source, and nitrogen flow 50sccm, using titanium nitride as target, the purity of reactive sputtering titanium nitride target is
99.99%, underlayer temperature is 300 DEG C, and preparation time is 25 minutes, and it is thin to obtain flexible stainless steel substrate/the 2nd AZO electrically conducting transparents
Film/p-NiO films/VO2Film/the first AZO transparent conductive film/TiAlN thin film obtains the experiment of n-VO2/P-NiO heterojunction structures
Sample 2.
Embodiment 3
1), ethyl alcohol, deionized water is used to carry out ultrasonic cleaning successively flexible stainless steel substrate, it is clear using EtOH Sonicate
It is 5 minutes to wash the time, and magnetron sputtering reative cell is sent into 5 minutes deionized water ultrasonic cleaning time, nitrogen drying, 1.0 ×
10-3Under conditions of Pa vacuum, deposition prepares AZO transparent conductive film on its flexible stainless steel；Its technological parameter condition is：With
Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 10:1, use Zinc oxide doped aluminium for target, instead
It is 99.9% to answer the purity of sputtering zinc oxide adulterated al target, and preparation temperature is 300 DEG C, and preparation time is 80 minutes, is obtained soft
The AZO transparent conductive film of property stainless steel substrate/second.
2), using magnetron sputtering reative cell it is above-mentioned 1) in obtained flexible stainless steel substrate/the 2nd AZO electrically conducting transparents it is thin
P-NiO films are prepared on film, 1.0 × 10-3Under conditions of Pa vacuum, technological parameter condition is：It is anti-using oxygen as gas
Ying Yuan, oxygen flow 100sccm use nickel oxide for target, and the purity of reactive sputtering nickel oxide target is 99.9%, system
Standby temperature is 300 DEG C, and preparation time 90 minutes obtains flexible stainless steel substrate/second AZO transparent conductive film/p-NiO films
Material.
3), using magnetron sputtering reative cell it is above-mentioned 2) in obtained flexible stainless steel substrate/the 2nd AZO electrically conducting transparents it is thin
VO is prepared on film/p-NiO films2Film, 1.0 × 10-3Under conditions of Pa vacuum, technological parameter condition is：With argon gas and
Oxygen is as mixed gas reaction source, argon gas and oxygen flow ratio 10:1, using vanadium dioxide as target, reactive sputtering vanadium dioxide
The purity of target is 99.9%, and preparation temperature is 300 DEG C, and preparation time is 250 minutes, and it is saturating to obtain flexible stainless steel substrate/AZO
Bright conductive film/p-NiO films/VO2Film.
4), continue using magnetron sputtering reative cell it is above-mentioned 3) in obtain flexible stainless steel substrate/the 2nd AZO is transparent leads
Conductive film/p-NiO films/VO2The first AZO transparent conductive film is prepared on film, 1.0 × 10-3Under conditions of Pa vacuum, after
It is continuous to prepare AZO transparent conductive film.Its technological parameter condition is：Using argon gas and oxygen as mixed gas reaction source, argon gas and
Oxygen flow is than 8:1, using Zinc oxide doped aluminium as target, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, system
Standby temperature is 240 DEG C, and preparation time is 50 minutes, and it is thin to obtain flexible stainless steel substrate/second AZO transparent conductive film/p-NiO
Film/VO2The AZO transparent conductive film of film/first.
5), continue using magnetron sputtering reative cell it is above-mentioned 4) in obtain flexible stainless steel substrate/the 2nd AZO is transparent leads
Conductive film/p-NiO films/VO2TiAlN thin film is prepared in the AZO transparent conductive film of film/first, technological parameter condition is：With
Nitrogen is as gas reaction source, and nitrogen flow 70sccm, using titanium nitride as target, the purity of reactive sputtering titanium nitride target is
99.99%, underlayer temperature is 250 DEG C, and preparation time is 30 minutes, and it is thin to obtain flexible stainless steel substrate/the 2nd AZO electrically conducting transparents
Film/p-NiO films/VO2Film/the first AZO transparent conductive film/TiAlN thin film, obtains n-VO2/ P-NiO heterojunction structures test sample
Product 3.
Embodiment 4
1), ethyl alcohol, deionized water is used to carry out ultrasonic cleaning successively flexible stainless steel substrate, it is clear using EtOH Sonicate
It is 5 minutes to wash the time, and magnetron sputtering reative cell is sent into 5 minutes deionized water ultrasonic cleaning time, nitrogen drying, 1.0 ×
10-3Under conditions of Pa vacuum, deposition prepares AZO transparent conductive film on its flexible stainless steel；Its technological parameter condition is：With
Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, use Zinc oxide doped aluminium for target, instead
It is 99.9% to answer the purity of sputtering zinc oxide adulterated al target, and preparation temperature is 350 DEG C, and preparation time is 60 minutes, is obtained soft
The AZO transparent conductive film of property stainless steel substrate/second.
2), using magnetron sputtering reative cell it is above-mentioned 1) in obtained flexible stainless steel substrate/the 2nd AZO electrically conducting transparents it is thin
P-NiO films are prepared on film, 1.0 × 10-3Under conditions of Pa vacuum, technological parameter condition is：It is anti-using oxygen as gas
Ying Yuan, oxygen flow 110sccm use nickel oxide for target, and the purity of reactive sputtering nickel oxide target is 99.9%, system
Standby temperature is 350 DEG C, and it is thin to obtain flexible stainless steel substrate/second AZO transparent conductive film/p-NiO for preparation time 150 minutes
Film.
3), using magnetron sputtering reative cell it is above-mentioned 2) in obtained flexible stainless steel substrate/the 2nd AZO electrically conducting transparents it is thin
VO is prepared on film/p-NiO films2Film, 1.0 × 10-3Under conditions of Pa vacuum, technological parameter condition is：With argon gas and
Oxygen is as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, using vanadium dioxide as target, reactive sputtering vanadium dioxide
The purity of target is 99.9%, and preparation temperature is 300 DEG C, and preparation time is 200 minutes, obtains flexible stainless steel substrate/the second
AZO transparent conductive film/p-NiO films/VO2Film.
4), continue using magnetron sputtering reative cell it is above-mentioned 3) in obtain flexible stainless steel substrate/the 2nd AZO is transparent leads
Conductive film/p-NiO films/VO2The first AZO transparent conductive film is prepared on film, 1.0 × 10-3Under conditions of Pa vacuum, after
It is continuous to prepare AZO transparent conductive film.Its technological parameter condition is：Using argon gas and oxygen as mixed gas reaction source, argon gas and
Oxygen flow is than 5:1, using Zinc oxide doped aluminium as target, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, system
Standby temperature is 250 DEG C, and preparation time is 30 minutes, and it is thin to obtain flexible stainless steel substrate/second AZO transparent conductive film/p-NiO
Film/VO2The AZO transparent conductive film of film/first.
5), continue using magnetron sputtering reative cell it is above-mentioned 4) in obtain flexible stainless steel substrate/the 2nd AZO is transparent leads
Conductive film/p-NiO films/VO2TiAlN thin film is prepared in the AZO transparent conductive film of film/first, technological parameter condition is：With
Nitrogen is as gas reaction source, and nitrogen flow 65sccm, using titanium nitride as target, the purity of reactive sputtering titanium nitride target is
99.99%, underlayer temperature is 350 DEG C, and preparation time is 20 minutes, and it is thin to obtain flexible stainless steel substrate/the 2nd AZO electrically conducting transparents
Film/p-NiO films/VO2Film/the first AZO transparent conductive film/TiAlN thin film, obtains n-VO2/ P-NiO heterojunction structures test sample
Product 4.
Embodiment 5
1), ethyl alcohol, deionized water is used to carry out ultrasonic cleaning successively flexible stainless steel substrate, it is clear using EtOH Sonicate
It is 5 minutes to wash the time, and magnetron sputtering reative cell is sent into 5 minutes deionized water ultrasonic cleaning time, nitrogen drying, 1.0 ×
10-3Under conditions of Pa vacuum, deposition prepares AZO transparent conductive film on its flexible stainless steel；Its technological parameter condition is：With
Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, use Zinc oxide doped aluminium for target, instead
It is 99.9% to answer the purity of sputtering zinc oxide adulterated al target, and preparation temperature is 400 DEG C, and preparation time is 60 minutes, is obtained soft
The AZO transparent conductive film of property stainless steel substrate/second.
2), using magnetron sputtering reative cell it is above-mentioned 1) in obtained flexible stainless steel substrate/the 2nd AZO electrically conducting transparents it is thin
P-NiO films are prepared on film, 1.0 × 10-3Under conditions of Pa vacuum, technological parameter condition is：It is anti-using oxygen as gas
Ying Yuan, oxygen flow 120sccm use nickel oxide for target, and the purity of reactive sputtering nickel oxide target is 99.9%, system
Standby temperature is 400 DEG C, and it is thin to obtain flexible stainless steel substrate/second AZO transparent conductive film/p-NiO for preparation time 180 minutes
Film.
3), using magnetron sputtering reative cell it is above-mentioned 2) in obtained flexible stainless steel substrate/the 2nd AZO electrically conducting transparents it is thin
VO is prepared on film/p-NiO films2Film, 1.0 × 10-3Under conditions of Pa vacuum, technological parameter condition is：With argon gas and
Oxygen is as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, using vanadium dioxide as target, reactive sputtering vanadium dioxide
The purity of target is 99.9%, and preparation temperature is 300 DEG C, and preparation time is 200 minutes, obtains flexible stainless steel substrate/the second
AZO transparent conductive film/p-NiO films/VO2Film.
4), continue using magnetron sputtering reative cell it is above-mentioned 3) in obtain flexible stainless steel substrate/the 2nd AZO is transparent leads
Conductive film/p-NiO films/VO2The first AZO transparent conductive film is prepared on film, 1.0 × 10-3Under conditions of Pa vacuum, after
It is continuous to prepare AZO transparent conductive film.Its technological parameter condition is：Using argon gas and oxygen as mixed gas reaction source, argon gas and
Oxygen flow is than 5:1, using Zinc oxide doped aluminium as target, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, system
Standby temperature is 300 DEG C, and preparation time is 30 minutes, and it is thin to obtain flexible stainless steel substrate/second AZO transparent conductive film/p-NiO
Film/VO2The AZO transparent conductive film of film/first.
5), continue using magnetron sputtering reative cell it is above-mentioned 4) in obtain flexible stainless steel substrate/the 2nd AZO is transparent leads
Conductive film/p-NiO films/VO2TiAlN thin film is prepared in the AZO transparent conductive film of film/first, technological parameter condition is：With
Nitrogen is as gas reaction source, and nitrogen flow 80sccm, using titanium nitride as target, the purity of reactive sputtering titanium nitride target is
99.99%, underlayer temperature is 400 DEG C, and preparation time is 20 minutes, and it is thin to obtain flexible stainless steel substrate/the 2nd AZO electrically conducting transparents
Film/p-NiO films/VO2Film/the first AZO transparent conductive film/TiAlN thin film, obtains n-VO2/ P-NiO heterojunction structures test sample
Product 5.
Using atomic force microscope microscope (AFM) analytical equipment to the n-VO of laboratory sample 1~4 after experiment2/P-
The surface VO of NiO heterojunction structures2Pattern is tested analysis.Its result can be seen that system referring to shown in Fig. 2-5 by Fig. 2-5
Standby n-VO2/ P-NiO heterojunction structure film morphologies are very smooth, and crystal grain distribution is very uniform, meet the requirement of device.
Using scanning electron microscope microscope (SEM) analytical equipment to laboratory sample 1~3 under the conditions of 500nm
VO2The cross section of/P-NiO heterojunction structures is tested analysis.Its result is detected referring to FE-SEM shown in Fig. 6-8, is illustrated
Lower VO2The plane of crystal pattern of/p-NiO hetero-junctions with thickness situation of change.All samples crystal face is all very smooth, crystal face crystal grain
It is uniformly distributed.In addition, we are therefrom observed that VO2Interface between film layer and p-NiO film layers is very clear.
The above description is merely a specific embodiment, when cannot be limited the scope of implementation of the present invention with this, it is all according to
Equivalent variations made by the present invention and modification, should all belong to the scope of protection of the present invention.
Claims (8)
1. one kind being based on n-VO2The heterojunction structure of/p-NiO, which is characterized in that from upper layer to lower layer include TiAlN thin film, the successively
One AZO transparent conductive film, VO2Film, p-NiO films, the second AZO transparent conductive film and flexible stainless steel substrate.
2. heterojunction structure according to claim 1, which is characterized in that the p-NiO films are buffer layer, and TiAlN thin film is to protect
Sheath, the first AZO transparent conductive film and the second AZO transparent conductive film are used as conductive electrode and slow down layer.
3. one kind being based on n-VO2The preparation method of the heterojunction structure of/p-NiO, which is characterized in that
The second AZO transparent conductive film, p-NiO films, VO are sequentially prepared on flexible stainless steel substrate2Film, the first AZO are saturating
Bright conductive film and TiAlN thin film.
4. preparation method according to claim 3, which is characterized in that prepare the second AZO transparent conductive film, not by flexibility
Become rusty steel substrate successively use ethyl alcohol, deionized water carry out ultrasonic cleaning, use EtOH Sonicate scavenging period for 5 minutes, go from
5 minutes sub- water ultrasonic cleaning time was dried up using nitrogen and is sent into magnetron sputtering reative cell, 1.0 × 10-3The condition of Pa vacuum
Under, using argon gas and oxygen as mixed gas reaction source, argon gas and oxygen flow ratio 8:1-10：1, be with Zinc oxide doped aluminium
The purity of target, the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, and preparation temperature is 200 DEG C~400 DEG C, and preparation time is
60 minutes~80 minutes, obtain the AZO transparent conductive film of flexible stainless steel substrate/second.
5. preparation method according to claim 3, which is characterized in that using magnetron sputtering reative cell in flexible stainless base steel
P-NiO films are prepared in the AZO transparent conductive film of piece/second, 1.0 × 10-3Under conditions of Pa vacuum, using oxygen as gas
Reaction source, oxygen flow are 80sccm~120sccm, and using nickel oxide as target, the purity of reactive sputtering nickel oxide target is
99.9%, preparation temperature is 200 DEG C~400 DEG C, and preparation time 30 minutes~180 minutes obtains flexible stainless steel substrate/the second
AZO transparent conductive film/p-NiO films.
6. preparation method according to claim 3, which is characterized in that using magnetron sputtering reative cell in flexible stainless base steel
VO is prepared on piece/the second AZO transparent conductive film/p-NiO thin-film materials2Thin-film material, 1.0 × 10-3The condition of Pa vacuum
Under, prepare VO2Thin-film material, using argon gas and oxygen as mixed gas reaction source, argon gas and oxygen flow ratio 8:1-10：1, with
Vanadium dioxide is target, and the purity of reactive sputtering vanadium dioxide target is 99.9%, and preparation temperature is 100 DEG C~300 DEG C, is prepared
Time is -250 minutes 200 minutes, obtains flexible stainless steel substrate/second AZO transparent conductive film/p-NiO films/VO2It is thin
Film.
7. preparation method according to claim 3, which is characterized in that using magnetron sputtering reative cell in flexible stainless base steel
Piece/the second AZO transparent conductive film/p-NiO films/VO2The first AZO transparent conductive film is prepared on film, with argon gas and oxygen
Gas is as mixed gas reaction source, argon gas and oxygen flow ratio 5:1~8:1, using Zinc oxide doped aluminium as target, reactive sputtering oxygen
The purity for changing zinc doping aluminium target is 99.9%, and preparation temperature is 100 DEG C~300 DEG C, and preparation time is 30 minutes~50 minutes,
Obtain flexible stainless steel substrate/second AZO transparent conductive film/p-NiO films/VO2The AZO transparent conductive film of film/first.
8. preparation method according to claim 3, which is characterized in that using magnetron sputtering reative cell in flexible stainless base steel
Piece/the second AZO transparent conductive film/p-NiO films/VO2The anticorrosive guarantors of TiN are prepared in the AZO transparent conductive film of film/first
Coating is protected, with nitrogen as gas reaction source, nitrogen flow is 30~80sccm, using titanium nitride as target, reactive sputtering nitridation
The purity of titanium target material is 99.99%, and preparation temperature is 100 DEG C~400 DEG C, and preparation time is 20 minutes~30 minutes, is obtained soft
Property stainless steel substrate/second AZO transparent conductive film/p-NiO films/VO2Film/the first AZO transparent conductive film/TiN is thin
Film.
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