CN108807511A - A kind of poly- polyethylene terephthalate substrate heterostructure device and preparation method thereof - Google Patents
A kind of poly- polyethylene terephthalate substrate heterostructure device and preparation method thereof Download PDFInfo
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- CN108807511A CN108807511A CN201810801124.8A CN201810801124A CN108807511A CN 108807511 A CN108807511 A CN 108807511A CN 201810801124 A CN201810801124 A CN 201810801124A CN 108807511 A CN108807511 A CN 108807511A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 97
- 239000005020 polyethylene terephthalate Substances 0.000 title claims abstract description 89
- 229920000139 polyethylene terephthalate Polymers 0.000 title claims abstract description 87
- 239000000758 substrate Substances 0.000 title claims abstract description 67
- -1 poly- polyethylene terephthalate Polymers 0.000 title claims abstract description 53
- 239000010410 layer Substances 0.000 claims abstract description 118
- 239000000463 material Substances 0.000 claims abstract description 77
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000011241 protective layer Substances 0.000 claims abstract description 32
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000005260 corrosion Methods 0.000 claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 108
- 239000007789 gas Substances 0.000 claims description 97
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 73
- 239000001301 oxygen Substances 0.000 claims description 73
- 229910052760 oxygen Inorganic materials 0.000 claims description 73
- 229910052786 argon Inorganic materials 0.000 claims description 54
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 44
- 239000010408 film Substances 0.000 claims description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 34
- 238000005546 reactive sputtering Methods 0.000 claims description 29
- 238000000151 deposition Methods 0.000 claims description 27
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 claims description 17
- 239000011787 zinc oxide Substances 0.000 claims description 17
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 claims description 16
- 239000004411 aluminium Substances 0.000 claims description 15
- 229910052782 aluminium Inorganic materials 0.000 claims description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 15
- 150000005690 diesters Chemical class 0.000 claims description 11
- 229920006389 polyphenyl polymer Polymers 0.000 claims description 10
- 230000004224 protection Effects 0.000 claims description 10
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000004544 sputter deposition Methods 0.000 claims description 9
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 8
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 239000010409 thin film Substances 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 239000008246 gaseous mixture Substances 0.000 claims 2
- 239000002243 precursor Substances 0.000 claims 2
- 239000000376 reactant Substances 0.000 claims 2
- 230000003628 erosive effect Effects 0.000 claims 1
- 238000009738 saturating Methods 0.000 claims 1
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 241000208340 Araliaceae Species 0.000 description 7
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 7
- 235000003140 Panax quinquefolius Nutrition 0.000 description 7
- 235000008434 ginseng Nutrition 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 230000000149 penetrating effect Effects 0.000 description 6
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 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
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000019589 hardness Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. 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
- H01L29/24—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only semiconductor materials not provided for in groups H01L29/16, H01L29/18, H01L29/20, H01L29/22
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. 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
-
- 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
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/34—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies not provided for in groups H01L21/0405, H01L21/0445, H01L21/06, H01L21/16 and H01L21/18 with or without impurities, e.g. doping materials
- H01L21/44—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/38 - H01L21/428
- H01L21/441—Deposition of conductive or insulating materials for electrodes
- H01L21/443—Deposition of conductive or insulating materials for electrodes from a gas or vapour, e.g. condensation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/40—Electrodes ; Multistep manufacturing processes therefor
- H01L29/43—Electrodes ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
Abstract
A kind of polyethylene terephthalate substrate heterojunction structure and preparation method thereof, belongs to technical field of film preparation.The heterojunction structure is that the first AZO transparent conductive film, SnO are sequentially prepared on polyethylene terephthalate substrate layer2Material layer, VO2Material layer, the second AZO transparent conductive film and anticorrosive protective layer.The present invention is with polyethylene terephthalate material substrate substrate, using SnO2As buffer layer, VO2/SnO2Heterojunction structure combines, and using AZO as transparent conductive electrode, corrosion resistant TiN materials are finally deposited, can prepare the cheap device of high quality；Meanwhile the preparation process is simple, it can be achieved that large-scale production.
Description
Technical field
The invention belongs to the manufacturing technology field of reversible semiconductor to metal (SMT) first order transition coating, more particularly to
A kind of poly- polyethylene terephthalate substrate heterostructure device and preparation method thereof.
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 lining
The electrical and optical properties of film of the selection at bottom to being grown have important influence.However, due to the presence of its price problem
And the Discussion On Development of flexible device, it is difficult to prepare the cheap VO of high-quality on flexible PET substrates2Thin-film material matter knot
Structure.So preparing the cheap VO of high quality on flexible PET2Material is assistant officer's problem to be solved.
Invention content
For the above technical problems, the present invention provides a kind of poly- polyethylene terephthalate substrate heterostructure device
And preparation method thereof.
The purpose of the present invention is achieved through the following technical solutions：
A kind of poly- polyethylene terephthalate substrate heterostructure device of the present invention includes polyphenyl dioctyl phthalate successively from top to bottom
Second diester substrate layer, the first conductive layer, SnO2Material layer, VO2Material layer, the second conductive layer, anticorrosive protective layer.
Preferably, first conductive layer and the second conductive layer are AZO transparent conductive film.
Preferably, the anticorrosive protective layer is the anticorrosive protective layers of TiN.
Preferably, the thickness of the poly- polyethylene terephthalate substrate layer is 0.4~1.2mm.
The preparation method of poly- polyethylene terephthalate substrate heterostructure device of the present invention, in poly- ethylene two
The first AZO transparent conductive film, SnO are sequentially prepared on ester substrate layer2Material layer, VO2Material layer, the second AZO transparent conductive film
And anticorrosive protective layer.
Preferably, the first AZO transparency conducting layers are prepared on the poly- polyethylene terephthalate substrate layer：By polyphenyl diformazan
After ten minutes using ionized water ultrasonic cleaning, magnetron sputtering reative cell is sent into drying to sour second diester substrate, in 1.0 × 10-3Pa
Under conditions of vacuum, AZO transparent conductive film electrode is prepared in its poly- polyethylene terephthalate deposition on substrate；Its technological parameter
Condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reactive sputtering is Zinc oxide doped
The purity of aluminium target is 99.9%, and preparation temperature is 200 DEG C~400 DEG C, and preparation time is 60 minutes.
Preferably, SnO is prepared using magnetron sputtering deposition2Material layer, under conditions of 1.0 × 10-3Pa vacuum, work
Skill Parameter Conditions are：For oxygen as gas reaction source, oxygen flow is 80~120sccm, reactive sputtering stannic oxide target
Purity be 99.9%, preparation temperature be 200 DEG C~400 DEG C, preparation time 30 minutes to 180 minutes.
Preferably, VO is prepared using magnetron sputtering deposition2Material layer prepares VO under conditions of 1.0 × 10-3Pa vacuum2
Thin-film material, technological parameter condition are：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1,
The purity of reactive sputtering vanadium dioxide target is 99.9%, and preparation temperature is 100 DEG C~300 DEG C, and preparation time is 180~220
Minute.
Preferably, the second AZO transparent conductive film is prepared using magnetron sputtering：Vacuum is extracted into 1.0 × 10-3Pa vacuum
Under conditions of, technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 5:1,
The purity of the Zinc oxide doped aluminium target of reactive sputtering be 99.9%, preparation temperature be 100 DEG C~300 DEG C, preparation time be 20~
30 minutes.
Preferably, anticorrosive protective layer is prepared using magnetron sputtering, which is that the anticorrosive protections of TiN apply
Layer, technological parameter condition are：For nitrogen as gas reaction source, nitrogen flow is 30~80sccm, reactive sputtering titanium nitride
The purity of target is 99.99%, and underlayer temperature is 100 DEG C~400 DEG C, and preparation time is 15-25 minutes.
Beneficial effects of the present invention are：
1. the present invention using poly- polyethylene terephthalate (PET) material as substrate base, relative to other substrate materials,
The price of poly- polyethylene terephthalate (PET) be it is most cheap, and of large quantities, it is flexible, flexible device can be prepared.Using
SnO2As buffer layer, VO2/SnO2Heterojunction structure combines poly- polyethylene terephthalate (PET) material as substrate, can prepare
Go out the device of high quality inexpensive flexible structure.Using SnO2As buffer layer, flexible PET and VO on the one hand can be alleviated2Material is brilliant
The big problem of lattice mismatch, can prepare the VO of high quality2Material, one side SnO2It is cheap as buffer layer price, to environment friend
It is good.Conductive electrodes of the AZO as device is then used, can be used as transparent conductive electrode between can also reducing film
Lattice mismatch.Then its TiN material is finally deposited, TiN material hardnesses are big, corrosion-resistant, efficiently solve the etching problem of device,
Further improve the service life of device.The preparation process is simple, it can be achieved that large-scale production.
2. the present invention is used as substrate layer using poly- polyethylene terephthalate (PET), since it is flexible substrate, can prepare
AZO conductive films are prepared on its surface in the flexible device for going out high quality, and AZO conductive films are used as electrode, play device electricity
On the one hand the effect of pole connection, SnO2 material layers form PN junction as P-type material with N-shaped VO2 material layers, form device, secondly
SnO2 materials can be used as buffer layer, reduce VO2 materials and be adapted to the poly- polyethylene terephthalate of substrate (PET) lattice, can be made
For the VO2 materials of high quality are gone out, continues to prepare AZO conductive films later, used as device electrode, finally prepare anticorrosive guarantor
Sheath protects device not to be corroded, and enhances its service life.
Description of the drawings
Fig. 1 is the schematic diagram of heterostructure device of the present invention.
Fig. 2 is 1~3 sample VO of the embodiment of the present invention2/SnO2The surface SEM patterns of heterojunction structure.
Fig. 3 is that the combination of 1~3 sample of the embodiment of the present invention can be in the XPS measuring spectrum within the scope of 0-1100eV.
In figure：1. poly- polyethylene terephthalate substrate layer, 2. first conductive layers, 3.SnO2Material layer, 4.VO2Material layer, 5.
Second conductive layer, 6. anticorrosive protective layers.
Specific implementation mode
It elaborates below to the embodiment of the present invention, but protection scope of the present invention is not limited to following embodiments.
XPS uses Thermo Scientific ESCALAB 250XiX X-ray photoelectron spectroscopy X instrument in the present invention,
The equipment uses Aka 1486.8eV radiographic sources, can reach the vacuum chamber of 3x10-8Pa.
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.
As shown in Figure 1, a kind of poly- polyethylene terephthalate (PET) substrate heterojunction structure of the present invention, is wrapped successively from top to bottom
Include poly- polyethylene terephthalate (PET) substrate layer 1, the first conductive layer 2, SnO2Material layer 3, VO2Material layer 4, the second conductive layer 5,
Anticorrosive protective layer 6.
First conductive layer, 2 and second conductive layer 5 is AZO transparent conductive film, and thickness is 100nm to 800nm.Institute
It is the anticorrosive protective layers of TiN to state anticorrosive protective layer 6, and thickness is 500nm to 900nm.The poly- polyethylene terephthalate (PET)
The thickness of substrate layer 1 is 0.4~1.2mm.The SnO2Layer thickness is 500nm to 900nm.The VO2Layer thickness is
400nm to 900nm.
The present invention be sequentially prepared on poly- polyethylene terephthalate (PET) substrate layer 1 the first AZO transparency conducting layers,
SnO2Material layer 3, VO2Material layer 4, the 2nd AZO transparency conducting layers and anticorrosive protective layer 6.
Embodiment 1：The first conductive layer 2 and the second conductive layer 5 are AZO transparent conductive film described in this example, and thickness is equal
For 100nm.The anticorrosive protective layer 6 is the anticorrosive protective layers of TiN, thickness 500nm.The polyethylene terephthalate
(PET) thickness of substrate layer 1 is 0.4；SnO23 thickness of material layer is 500nm；VO24 thickness of material layer is 400nm.
The preparation method of this example carries out as follows：
1. preparing the first AZO transparent conductive film on poly- polyethylene terephthalate (PET) substrate layer 1：By polyphenyl
After ten minutes using ionized water ultrasonic cleaning, magnetron sputtering reative cell is sent into drying to dioctyl phthalate second diester (PET) substrate,
Under conditions of 1.0 × 10-3Pa vacuum, it is thin to prepare AZO electrically conducting transparents in its poly- polyethylene terephthalate (PET) deposition on substrate
Membrane electrode；Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, 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.
2. preparing SnO using magnetron sputtering deposition2Material layer 3, under conditions of 1.0 × 10-3Pa vacuum, technique ginseng
Said conditions are：Oxygen is as gas reaction source, the purity of oxygen flow 80sccm, reactive sputtering stannic oxide target
99.9%, preparation temperature is 200 DEG C, preparation time 30 minutes.
3. preparing VO using magnetron sputtering deposition2Material layer 4 prepares VO under conditions of 1.0 × 10-3Pa vacuum2Film
Material, technological parameter condition are：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reaction
The purity for sputtering vanadium dioxide target is 99.9%, and preparation temperature is
100 DEG C, preparation time is 200 minutes.
4. preparing the second AZO transparent conductive film using magnetron sputtering：Vacuum is extracted into the condition of 1.0 × 10-3Pa vacuum
Under, technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 5:1, reaction is splashed
The purity for penetrating Zinc oxide doped aluminium target is 99.9%, and preparation temperature is 100 DEG C, and preparation time is 30 minutes.
5. preparing anticorrosive protective layer 6 using magnetron sputtering, which is TiN anti-corrosion protection coatings,
Technological parameter condition is：Nitrogen is as gas reaction source, nitrogen flow 30sccm, the purity of reactive sputtering titanium nitride target
It is 99.99%, underlayer temperature is 100 DEG C, and preparation time is 20 minutes.
Embodiment 2：This example is as different from Example 1：2 thickness of the first conductive layer that this example uses is 800nm, and
Two conductive layers, 5 thickness is 600nm.6 thickness of anticorrosive protective layer is 600nm.The polyethylene terephthalate substrate
The thickness of layer 1 is 0.5mm；SnO23 thickness of material layer is 700nm；VO24 thickness of material layer is 500nm.This example preparation method is：
1. preparing the first AZO transparent conductive film on poly- polyethylene terephthalate (PET) substrate layer 1：By benzene two
After ten minutes using ionized water ultrasonic cleaning, magnetron sputtering reative cell is sent into drying to formic acid second diester (PET) substrate, 1.0
Under conditions of × 10-3Pa vacuum, AZO transparent conductive electrodes are prepared in its polyethylene terephthalate (PET) deposition on substrate.Its
Technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reactive sputtering oxygen
The purity for changing zinc doping aluminium target is 99.9%, and preparation temperature is 250 DEG C, and preparation time is 60 minutes.
2. preparing SnO using magnetron sputtering deposition2Material layer 3, under conditions of 1.0 × 10-3Pa vacuum, technique ginseng
Said conditions are：Oxygen is as gas reaction source, the purity of oxygen flow 90sccm, reactive sputtering stannic oxide target
99.9%, preparation temperature is 250 DEG C, preparation time 60 minutes.
3. preparing VO using magnetron sputtering deposition2It is thin to prepare VO2 under conditions of 1.0 × 10-3Pa vacuum for material layer 4
Membrane material.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, instead
The purity that vanadium dioxide target should be sputtered is 99.9%, and preparation temperature is 250 DEG C, and preparation time is 200 minutes.
4. preparing the second AZO transparent conductive film using magnetron sputtering：Vacuum is extracted into the condition of 1.0 × 10-3Pa vacuum
Under, continue to prepare AZO transparent conductive electrodes.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon
Gas and oxygen flow ratio 5:1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, and preparation temperature is 200 DEG C, is prepared
Time is 30 minutes.
5. preparing anticorrosive protective layer 6 using magnetron sputtering, which is TiN anti-corrosion protection coatings,
Technological parameter condition is：Nitrogen is as gas reaction source, nitrogen flow 50sccm, the purity of reactive sputtering titanium nitride target
It is 99.99%, underlayer temperature is 300 DEG C, and preparation time is 20 minutes.
Embodiment 3：This example is as different from Example 1：This example is as different from Example 1：This example use described the
One conductive layer, 2 thickness is 300nm, and 5 thickness of the second conductive layer is 200nm.6 thickness of anticorrosive protective layer is 900nm.It is described
The thickness of polyethylene terephthalate substrate layer 1 is 1.2mm；SnO23 thickness of material layer is 900nm；VO24 thickness of material layer is
800nm.This example preparation method is：
1. preparing the first AZO transparent conductive film on poly- polyethylene terephthalate (PET) substrate layer 1：By polyphenyl
After ten minutes using ionized water ultrasonic cleaning, magnetron sputtering reative cell is sent into drying to dioctyl phthalate second diester (PET) substrate,
Under conditions of 1.0 × 10-3Pa vacuum, AZO electrically conducting transparent electricity is prepared in its poly- polyethylene terephthalate (PET) deposition on substrate
Pole.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reaction is splashed
The purity for penetrating Zinc oxide doped aluminium target is 99.9%, and preparation temperature is 300 DEG C, and preparation time is 60 minutes.
2. preparing SnO using magnetron sputtering deposition2Material layer 3, under conditions of 1.0 × 10-3Pa vacuum, technique ginseng
Said conditions are：Oxygen is as gas reaction source, the purity of oxygen flow 100sccm, reactive sputtering stannic oxide target
99.9%, preparation temperature is 300 DEG C, preparation time 90 minutes.
3. preparing VO using magnetron sputtering deposition2Material layer 4 prepares VO under conditions of 1.0 × 10-3Pa vacuum2Film
Material.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reaction
The purity for sputtering vanadium dioxide target is 99.9%, and preparation temperature is 300 DEG C, and preparation time is 200 minutes.
4. preparing the second AZO transparent conductive film using magnetron sputtering：Vacuum is extracted into the condition of 1.0 × 10-3Pa vacuum
Under, continue to prepare AZO transparent conductive electrodes.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon
Gas and oxygen flow ratio 5:1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, and preparation temperature is 240 DEG C, is prepared
Time is 30 minutes.
5. preparing anticorrosive protective layer 6 using magnetron sputtering, which is TiN anti-corrosion protection coatings,
Technological parameter condition is：Nitrogen is as gas reaction source, nitrogen flow 70sccm, the purity of reactive sputtering titanium nitride target
It is 99.99%, underlayer temperature is 250 DEG C, and preparation time is 20 minutes.
Embodiment 4：This example is as different from Example 1：2 thickness of the first conductive layer that this example uses is 400nm, and
Two conductive layers, 5 thickness is 600nm.6 thickness of anticorrosive protective layer is 800nm.The polyethylene terephthalate substrate
The thickness of layer 1 is 1.0mm；SnO23 thickness of material layer is 600nm；VO24 thickness of material layer is 600nm.This example preparation method is：
1. preparing the first AZO transparent conductive film on poly- polyethylene terephthalate (PET) substrate layer 1：By polyphenyl
After ten minutes using ionized water ultrasonic cleaning, magnetron sputtering reative cell is sent into drying to dioctyl phthalate second diester (PET) substrate,
Under conditions of 1.0 × 10-3Pa vacuum, AZO electrically conducting transparent electricity is prepared in its poly- polyethylene terephthalate (PET) deposition on substrate
Pole.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reaction is splashed
The purity for penetrating Zinc oxide doped aluminium target is 99.9%, and preparation temperature is 350 DEG C, and preparation time is 60 minutes.
2. preparing SnO using magnetron sputtering deposition2Material layer 3, under conditions of 1.0 × 10-3Pa vacuum, technique ginseng
Said conditions are：For oxygen as gas reaction source, oxygen flow is 80~120sccm, reactive sputtering stannic oxide target it is pure
Degree is 99.9%, and preparation temperature is 350 DEG C, preparation time 150 minutes.
3. preparing VO using magnetron sputtering deposition2Material layer 4,1.0 × 10-3Under conditions of Pa vacuum, VO is prepared2Film
Material.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reaction
The purity for sputtering vanadium dioxide target is 99.9%, and preparation temperature is 300 DEG C, and preparation time is 200 minutes.
4. preparing the second AZO transparent conductive film using magnetron sputtering：Vacuum is extracted into the condition of 1.0 × 10-3Pa vacuum
Under, continue to prepare AZO transparent conductive electrodes.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon
Gas and oxygen flow ratio 5:1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, and preparation temperature is 250 DEG C, is prepared
Time is 30 minutes.
5. preparing anticorrosive protective layer 6 using magnetron sputtering, which is TiN anti-corrosion protection coatings,
Technological parameter condition is：Nitrogen is as gas reaction source, nitrogen flow 65sccm, the purity of reactive sputtering titanium nitride target
It is 99.99%, underlayer temperature is 350 DEG C, and preparation time is 20 minutes.
Embodiment 5：This example is as different from Example 1：2 thickness of the first conductive layer that this example uses is 600nm, and
Two conductive layers, 5 thickness is 700nm.6 thickness of anticorrosive protective layer is 550nm.The polyethylene terephthalate substrate
The thickness of layer 1 is 0.6mm；SnO23 thickness of material layer is 650nm；VO24 thickness of material layer is 700nm.This example preparation method is：
1. preparing the first AZO transparent conductive film on poly- polyethylene terephthalate (PET) substrate layer 1：By polyphenyl
After ten minutes using ionized water ultrasonic cleaning, magnetron sputtering reative cell is sent into drying to dioctyl phthalate second diester (PET) substrate,
Under conditions of 1.0 × 10-3Pa vacuum, AZO electrically conducting transparent electricity is prepared in its poly- polyethylene terephthalate (PET) deposition on substrate
Pole.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reaction is splashed
The purity for penetrating Zinc oxide doped aluminium target is 99.9%, and preparation temperature is 400 DEG C, and preparation time is 60 minutes.
2. preparing SnO using magnetron sputtering deposition2Material layer 3, under conditions of 1.0 × 10-3Pa vacuum, technique ginseng
Said conditions are：For oxygen as gas reaction source, oxygen flow is 80~120sccm, reactive sputtering stannic oxide target it is pure
Degree is 99.9%, and preparation temperature is 400 DEG C, preparation time 180 minutes.
3. preparing VO using magnetron sputtering deposition2Material layer 4 prepares VO under conditions of 1.0 × 10-3Pa vacuum2Film
Material.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reaction
The purity for sputtering vanadium dioxide target is 99.9%, and preparation temperature is 300 DEG C, and preparation time is 200 minutes.
4. preparing the second AZO transparent conductive film using magnetron sputtering：Vacuum is extracted into the condition of 1.0 × 10-3Pa vacuum
Under, continue to prepare AZO transparent conductive electrodes.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon
Gas and oxygen flow ratio 5:1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, and preparation temperature is 300 DEG C, is prepared
Time is 30 minutes.
5. preparing anticorrosive protective layer 6 using magnetron sputtering, which is TiN anti-corrosion protection coatings,
Technological parameter condition is：Nitrogen is as gas reaction source, nitrogen flow 80sccm, the purity of reactive sputtering titanium nitride target
It is 99.99%, underlayer temperature is 400 DEG C, and preparation time is 20 minutes.
Embodiment 6：This example is as different from Example 1：2 thickness of the first conductive layer that this example uses is 500nm, and
Two conductive layers, 5 thickness is 400nm.6 thickness of anticorrosive protective layer is 750nm.The polyethylene terephthalate substrate
The thickness of layer 1 is 0.8mm；SnO23 thickness of material layer is 800nm；VO24 thickness of material layer is 550nm.This example preparation method is：
1. preparing the first AZO transparent conductive film on poly- polyethylene terephthalate (PET) substrate layer 1：By polyphenyl
After ten minutes using ionized water ultrasonic cleaning, magnetron sputtering reative cell is sent into drying to dioctyl phthalate second diester (PET) substrate,
Under conditions of 1.0 × 10-3Pa vacuum, it is thin to prepare AZO electrically conducting transparents in its poly- polyethylene terephthalate (PET) deposition on substrate
Membrane electrode；Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, 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 40 minutes.
2. preparing SnO using magnetron sputtering deposition2Material layer 2, under conditions of 1.0 × 10-3Pa vacuum, technique ginseng
Said conditions are：For oxygen as gas reaction source, oxygen flow is 80~120sccm, reactive sputtering stannic oxide target it is pure
Degree is 99.9%, and preparation temperature is 400 DEG C, preparation time 180 minutes.
3. preparing VO using magnetron sputtering deposition2Material layer 3 prepares VO under conditions of 1.0 × 10-3Pa vacuum2Film
Material, technological parameter condition are：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reaction
The purity for sputtering vanadium dioxide target is 99.9%, and preparation temperature is 120 DEG C, and preparation time is 220 minutes.
4. preparing the second AZO transparent conductive film using magnetron sputtering：Vacuum is extracted into the condition of 1.0 × 10-3Pa vacuum
Under, technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 5:1, reaction is splashed
The purity for penetrating Zinc oxide doped aluminium target is 99.9%, and preparation temperature is 100 DEG C, and preparation time is 20 minutes.
5. preparing anticorrosive protective layer 6 using magnetron sputtering, which is TiN anti-corrosion protection coatings,
Technological parameter condition is：Nitrogen is as gas reaction source, and nitrogen flow is 30~80sccm, reactive sputtering titanium nitride target
Purity is 99.99%, and underlayer temperature is 400 DEG C, and preparation time is 15 minutes.
Embodiment 7：This example is as different from Example 1：2 thickness of the first conductive layer that this example uses is 650nm, and
Two conductive layers, 5 thickness is 550nm.6 thickness of anticorrosive protective layer is 550nm.The polyethylene terephthalate substrate
The thickness of layer 1 is 1.2mm；SnO23 thickness of material layer is 700nm；VO24 thickness of material layer is 600nm.This example preparation method is：
1. preparing the first AZO transparent conductive film on poly- polyethylene terephthalate (PET) substrate layer 1：By polyphenyl
After ten minutes using ionized water ultrasonic cleaning, magnetron sputtering reative cell is sent into drying to dioctyl phthalate second diester (PET) substrate,
Under conditions of 1.0 × 10-3Pa vacuum, it is thin to prepare AZO electrically conducting transparents in its poly- polyethylene terephthalate (PET) deposition on substrate
Membrane electrode；Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, 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 50 minutes.
2. preparing SnO using magnetron sputtering deposition2Material layer 2, under conditions of 1.0 × 10-3Pa vacuum, technique ginseng
Said conditions are：For oxygen as gas reaction source, oxygen flow is 80~120sccm, reactive sputtering stannic oxide target it is pure
Degree is 99.9%, and preparation temperature is 280 DEG C, preparation time 100 minutes.
3. preparing VO using magnetron sputtering deposition2It is thin to prepare VO2 under conditions of 1.0 × 10-3Pa vacuum for material layer 3
Membrane material, technological parameter condition are：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, instead
The purity that vanadium dioxide target should be sputtered is 99.9%, and preparation temperature is 150 DEG C, and preparation time is 180 minutes.
4. preparing the second AZO transparent conductive film using magnetron sputtering：Vacuum is extracted into the condition of 1.0 × 10-3Pa vacuum
Under, technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 5:1, reaction is splashed
The purity for penetrating Zinc oxide doped aluminium target is 99.9%, and preparation temperature is 100 DEG C~300 DEG C, and preparation time is 25 minutes.
5. preparing anticorrosive protective layer 6 using magnetron sputtering, which is TiN anti-corrosion protection coatings,
Technological parameter condition is：Nitrogen is as gas reaction source, and nitrogen flow is 30~80sccm, reactive sputtering titanium nitride target
Purity is 99.99%, and underlayer temperature is 100 DEG C~400 DEG C, and preparation time is 25 minutes.
Using scanning electron microscope microscope (SEM) analytical equipment to VO after experiment2/SnO2Ethylene two
The surface topography of ester (PET) heterojunction structure is tested analysis.The results are shown in Figure 2 for it, the film material that can be prepared by Fig. 2
Expect that pattern is very smooth, crystal grain distribution is very uniform, meets the requirement of device.Use XPS to VO later2/SnO2Polyethylene terephthalate
(PET) heterojunction structure is tested analysis, as shown in figure 3, institute that can well in recognition combination object in XPS measuring spectrum
There is element.We detect that there are VO in all samples2Signal.
Claims (10)
1. a kind of poly- polyethylene terephthalate substrate heterostructure device, it is characterised in that：Include polyphenyl two successively from top to bottom
Formic acid second diester substrate layer, the first conductive layer, SnO2Material layer, VO2Material layer, the second conductive layer, anticorrosive protective layer.
2. poly- polyethylene terephthalate substrate heterostructure device according to claim 1, it is characterised in that：Described first leads
Electric layer and the second conductive layer are AZO transparent conductive film.
3. poly- polyethylene terephthalate substrate heterostructure device according to claim 1, it is characterised in that：The anti-corruption
Erosion protective layer is the anticorrosive protective layers of TiN.
4. poly- polyethylene terephthalate substrate heterostructure device according to claim 1, it is characterised in that：The polyphenyl
The thickness of dioctyl phthalate second diester substrate layer is 0.4~1.2mm.
5. a kind of preparation method of poly- polyethylene terephthalate substrate heterostructure device as described in claim 1, feature exist
In：It is sequentially prepared the first AZO transparent conductive film, SnO on poly- polyethylene terephthalate substrate layer2Material layer, VO2Material layer,
Second AZO transparent conductive film and anticorrosive protective layer.
6. preparation method according to claim 5, it is characterised in that：It is prepared on the polyethylene terephthalate substrate layer
First AZO transparency conducting layers：After ten minutes using ionized water ultrasonic cleaning by polyethylene terephthalate substrate, magnetic is sent into drying
It is saturating to prepare AZO under conditions of 1.0 × 10-3Pa vacuum in its polyethylene terephthalate deposition on substrate for control sputtering reative cell
Bright conductive film electrode；Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow
Than 8:1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, and preparation temperature is 200 DEG C~400 DEG C, preparation time
It is 60 minutes.
7. preparation method according to claim 5, which is characterized in that prepare SnO using magnetron sputtering deposition2Material layer,
Under conditions of 1.0 × 10-3Pa vacuum, technological parameter condition is：Oxygen as gas reaction source, oxygen flow is 80~
The purity of 120sccm, reactive sputtering stannic oxide target are 99.9%, and preparation temperature is 200 DEG C~400 DEG C, preparation time 30
Minute was to 180 minutes.
8. preparation method according to claim 5, which is characterized in that prepare VO using magnetron sputtering deposition2Material layer,
Under conditions of 1.0 × 10-3Pa vacuum, VO is prepared2Thin-film material, technological parameter condition are：Argon gas and oxygen are as gaseous mixture
Precursor reactant source, argon gas and oxygen flow ratio 8:1, the purity of reactive sputtering vanadium dioxide target is 99.9%, and preparation temperature is
100 DEG C~300 DEG C, preparation time is 180~220 minutes.
9. preparation method according to claim 5, which is characterized in that prepare the 2nd AZO electrically conducting transparents using magnetron sputtering
Film：Under conditions of vacuum is extracted into 1.0 × 10-3Pa vacuum, technological parameter condition is：Argon gas and oxygen are as gaseous mixture
Precursor reactant source, argon gas and oxygen flow ratio 5:1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, prepares temperature
Degree is 100 DEG C~300 DEG C, and preparation time is 20~30 minutes.
10. preparation method according to claim 5, which is characterized in that anticorrosive protective layer is prepared using magnetron sputtering, it should
Anticorrosive protective layer is TiN anti-corrosion protection coatings, and technological parameter condition is：Nitrogen is as gas reaction source, nitrogen stream
Amount is 30~80sccm, and the purity of reactive sputtering titanium nitride target is 99.99%, and underlayer temperature is 100 DEG C~400 DEG C, is prepared
Time is 15-25 minutes.
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| JP2000058903A (en) * | 1998-08-07 | 2000-02-25 | Canon Inc | Position detection element and its manufacturing method |
| JP2004172167A (en) * | 2002-11-15 | 2004-06-17 | Zenji Hiroi | Solar cell composed of transition metal oxide |
| WO2008052067A2 (en) * | 2006-10-24 | 2008-05-02 | Applied Quantum Technology Llc | Semiconductor grain and oxide layer for photovoltaic cells |
| WO2011118700A1 (en) * | 2010-03-24 | 2011-09-29 | 独立行政法人産業技術総合研究所 | Process for production of optical vanadium dioxide thin film |
| CN104569061A (en) * | 2015-01-26 | 2015-04-29 | 苏州纳格光电科技有限公司 | Metal oxide semiconductor gas sensor and preparation method thereof |
| CN208478342U (en) * | 2018-02-09 | 2019-02-05 | 沈阳工程学院 | A kind of polyethylene terephthalate substrate heterojunction structure |
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| JP2000058903A (en) * | 1998-08-07 | 2000-02-25 | Canon Inc | Position detection element and its manufacturing method |
| JP2004172167A (en) * | 2002-11-15 | 2004-06-17 | Zenji Hiroi | Solar cell composed of transition metal oxide |
| WO2008052067A2 (en) * | 2006-10-24 | 2008-05-02 | Applied Quantum Technology Llc | Semiconductor grain and oxide layer for photovoltaic cells |
| WO2011118700A1 (en) * | 2010-03-24 | 2011-09-29 | 独立行政法人産業技術総合研究所 | Process for production of optical vanadium dioxide thin film |
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| 徐婷婷: "基于AZO/VO2/AZO结构的电压诱导相变红外光调制器", 物理学报, vol. 65, no. 24, pages 248102 - 1 * |
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