CN107240544A - A kind of preparation method of graphical film, thin film transistor (TFT) and memristor - Google Patents
A kind of preparation method of graphical film, thin film transistor (TFT) and memristor Download PDFInfo
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- CN107240544A CN107240544A CN201710309424.XA CN201710309424A CN107240544A CN 107240544 A CN107240544 A CN 107240544A CN 201710309424 A CN201710309424 A CN 201710309424A CN 107240544 A CN107240544 A CN 107240544A
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- film
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- graphical
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- 239000010408 film Substances 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 239000010409 thin film Substances 0.000 title claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 59
- 239000007788 liquid Substances 0.000 claims abstract description 56
- 238000000034 method Methods 0.000 claims abstract description 48
- 239000002243 precursor Substances 0.000 claims abstract description 38
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 239000004065 semiconductor Substances 0.000 claims abstract description 8
- 238000009413 insulation Methods 0.000 claims abstract description 6
- 230000008859 change Effects 0.000 claims abstract description 3
- 229910052738 indium Inorganic materials 0.000 claims description 24
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 24
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 21
- 229910052733 gallium Inorganic materials 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 18
- 229910052710 silicon Inorganic materials 0.000 claims description 18
- 239000010703 silicon Substances 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 15
- 229910052793 cadmium Inorganic materials 0.000 claims description 13
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 13
- 238000000137 annealing Methods 0.000 claims description 10
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 9
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 9
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 9
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 9
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 9
- 238000007711 solidification Methods 0.000 claims description 8
- 230000008023 solidification Effects 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 229910052735 hafnium Inorganic materials 0.000 claims description 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 229910003978 SiClx Inorganic materials 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 229910002804 graphite Inorganic materials 0.000 claims 1
- 239000010439 graphite Substances 0.000 claims 1
- 238000000935 solvent evaporation Methods 0.000 claims 1
- 238000000059 patterning Methods 0.000 abstract description 21
- 230000006978 adaptation Effects 0.000 abstract 1
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 15
- 229910002651 NO3 Inorganic materials 0.000 description 12
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 12
- 238000000576 coating method Methods 0.000 description 11
- 238000001704 evaporation Methods 0.000 description 9
- 230000008020 evaporation Effects 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 238000012545 processing Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000000523 sample Substances 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 description 4
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 4
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
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- 239000003795 chemical substances by application Substances 0.000 description 3
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- 229910021389 graphene Inorganic materials 0.000 description 3
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- MSNOMDLPLDYDME-UHFFFAOYSA-N gold nickel Chemical compound [Ni].[Au] MSNOMDLPLDYDME-UHFFFAOYSA-N 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 230000005499 meniscus Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000427 thin-film deposition Methods 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 206010068150 Acoustic shock Diseases 0.000 description 1
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- 238000003848 UV Light-Curing Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003466 anti-cipated effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 230000008543 heat sensitivity Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
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- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 238000005325 percolation Methods 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02373—Group 14 semiconducting materials
- H01L21/02381—Silicon, silicon germanium, germanium
-
- 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
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
- H01L21/02175—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal
- H01L21/02194—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal the material containing more than one metal element
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02282—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process liquid deposition, e.g. spin-coating, sol-gel techniques, spray coating
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- 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
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02623—Liquid deposition
- H01L21/02628—Liquid deposition using solutions
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02636—Selective deposition, e.g. simultaneous growth of mono- and non-monocrystalline semiconductor materials
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- H01L21/02697—Forming conducting materials on a substrate
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/34—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a 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
- H01L21/445—Deposition of conductive or insulating materials for electrodes from a liquid, e.g. electrolytic deposition
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- 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
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/66007—Multistep manufacturing processes
- H01L29/66969—Multistep manufacturing processes of devices having semiconductor bodies not comprising group 14 or group 13/15 materials
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- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
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- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
- H10N70/021—Formation of switching materials, e.g. deposition of layers
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- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
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- H10N70/801—Constructional details of multistable switching devices
- H10N70/881—Switching materials
- H10N70/883—Oxides or nitrides
- H10N70/8836—Complex metal oxides, e.g. perovskites, spinels
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- Chemical & Material Sciences (AREA)
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- Ceramic Engineering (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
The invention discloses a kind of patterning preparation method of film, this method constructs microchannel by template and substrate, and the driving force produced using film precursor liquid drop to the immersional wetting of substrate is made drop be moved in microchannel and realizes the graphical of film.This method is simple and feasible, wide adaptation range, is customized available for the pattern for realizing all kinds of film forerunner liquors or suspension.The invention discloses a kind of preparation method of thin film transistor (TFT), any layer in semiconductor channel layer, insulation gate dielectric layer, source-drain electrode layer and the gate electrode layer of described thin film transistor (TFT) is prepared using the patterning preparation method of above-mentioned film.The invention also discloses a kind of preparation method of memristor, the bottom electrode layer of described memristor, any layer in change resistance layer and top electrode layer is prepared using the patterning preparation method of above-mentioned film.
Description
Technical field
The present invention relates to technical field of film preparation, more particularly to a kind of graphical film, thin film transistor (TFT) and memristor
The preparation method of device.
Background technology
Due to not needing vacuum condition, instrument and equipment is simple, can be in various matrix surface plated films, and wet method coating technique is in reality
There is unique advantage, in film in terms of the low temperature low-cost large-area preparation of existing electronic component film and other species thin films
Preparation field is used widely.
Wet method coating technique mainly has czochralski method, spin-coating method etc., and precursor liquid of such method based on specific components passes through plating
The operation such as film and follow-up heat treatment obtains required film.For wet method coating process, it can only typically prepare in large area
Entire film and film difficult to realize it is graphical.For such coating process, if the film to be realized is graphical, need
The preparation of film is first carried out, film is patterned in conjunction with methods such as traditional wet etching or photoetching.Such work
It is long to there is process route in skill, and processing procedure is complicated and the problem of high cost, is restricted unavoidably in actual applications.
The graphical of film can also be realized by micro nano transfer printing technology, the realization of transfer be based on material to be transferred for
Template is different with the adhesion energy of substrate, so needing to be surface-treated base material in actual applications.In addition, transfer effect
The speed that fruit is also opened with template etc. is relevant, because influence factor is more, it is difficult to ensure that the success rate of transfer in practical operation.Closely
Nian Lai, the graphical of film can be realized by UV-curing technology while plated film, but before the technological requirement film
Driving liquid has strong absorption to the ultraviolet light of specific wavelength, therefore the technique has larger limitation when driving liquid type before the selection,
Film patterning aspect is being realized, the preparation method lacks versatility.
Sum it up, in current Film patterning preparation technology route, still lack it is a kind of both can be in thin film deposition
During realize the graphical of film and to precursor liquid without harsh requirement and easy-to-use preparation method.
The content of the invention
To achieve the above object, the invention provides a kind of preparation method of graphical film, using template and substrate it
Between the microchannel that is formed, by the capillarity between precursor liquid and substrate, make precursor liquid capillary percolation in the same of thin film deposition
Shi Shixian is graphical.
A kind of preparation method of graphical film, comprises the following steps:
Step 1, prepare film precursor liquid, and select substrate;
Step 2, the substrate is cleaned, and hydrophilic treated is carried out to the aufwuchsplate for cleaning back substrate;
Step 3, a pre-prepd figuratum template of band is selected, and the template is posted and fixed in hydrophilic treated
On substrate afterwards;
Step 4, the film precursor liquid is added dropwise at the microchannel two ends of template and substrate formation, and makes the film forerunner
Liquid fully infiltrates template two ends;
Step 5, wait for quietly, it is to be seen no longer to be moved in microchannel to the film precursor liquid, carry out film precursor liquid molten
The evaporation process of agent, completes the primary solidification of graphical film;
Step 6, confirm film primary solidification after remove removing template, then to substrate and on film make annealing treatment,
Complete the graphical preparation of film.
The key of the preparation method of graphical film proposed by the present invention is film precursor liquid (solution or suspension) energy
It is enough preferably to infiltrate selected substrate, using the mechanism of capillarity, realize infiltration migration of the drop in microchannel, most end form
Into graphical film.
Capillarity, i.e., small into the capillary suitable with the radius of curvature of liquid concave meniscus in some pipe diameters, pipe
Interior liquid infiltrates tube wall and bends liquid surface, and the top layer hydrone on concave meniscus is produced due to the effect of surface tension
The power of one sensing gas phase side, by the pulling of this active force, in the vertical direction raises the liquid level made in pipe, makes liquid
Body rises along tube wall;If acted in the horizontal direction, such power will drive drop to be sprawled to pipeline internal penetration.
Preferably, described substrate is silicon chip, thermal oxide silicon chip, slide etc. have flat surface hard substrate or
Person is the flexible substrate that PET, PI, PDMS etc. have flat surface.
Preferably, described template is the soft template based on flexible macromolecule, such as PDMS, or other can be with substrate
Form the hard template of microchannel;Hard template is easier to realize that pattern is customized;PDMS costs are low, using simple, with substrate it
Between there is good adhesiveness, and the features such as with good chemical inertness, the convenient various patterns of customization.
Preferably, the film precursor liquid is outstanding for the solution based on water or organic solvent or based on water or organic solvent
Supernatant liquid, preferably, the film precursor liquid can select indium, gallium, zinc, cadmium, tin aluminium, yttrium, hafnium, zirconium etc. inorganic salt solution or
Mixed solution and graphene, the solution or suspension of class grapheme two-dimension material, institute of the inorganic salts of wherein several metal
The class grapheme two-dimension material stated is graphene oxide or two-dimensional layer transition metal carbide (MXene);Further preferably, institute
It is the nitrate solution of indium gallium cadmium or MXene suspension to state film precursor liquid.
In step 2, it is described to substrate carry out hydrophilic treated can by Physical such as oxygen plasma bombardment realization or
Handled and realized by the mixed liquor of chemical method such as sulfuric acid and hydrogen peroxide.
Preferably, the pattern in described template is strip striped, width of fringe is with fringe spacing in 0~100 μ
Between m, so that the microchannel size formed between the substrate and the template is also between 0~100 μm, and selection should
Width, the microchannel of preparation has suitable the ratio of width to height, if the width of fringe used is excessive, template is fitted in institute's shape on substrate
Into microchannel be easily recessed, be unfavorable for the holding of anticipated shape and structure.
In step 3, described template fixation procedure is preferably:One quality is acted on for 50~300g counterweight described
In template, and the template posts and fixes the time kept over the substrate between 30-300s.
In step 5, the evaporation process of described film precursor liquid solvent can be preferably:Pass through heating, drying or solvent
Natural evaporation realize the primary solidification of graphical film.
In step 6, conversion of the precursor liquid to semiconductive thin film is realized by heating, the temperature of described annealing is excellent
Elect 100~400 DEG C as, in the annealing region, the heat energy provided allows most film precursor liquid to be converted into enough
Final semiconductive thin film, and can complete the preparation of semiconductive thin film in 400 DEG C so relatively low temperature.
On the other hand, the invention provides a kind of preparation method of thin film transistor (TFT), described thin film transistor (TFT) is partly led
Any layer in body channel layer, insulation gate dielectric layer, source-drain electrode layer and gate electrode layer is using the above-mentioned method system of the present invention
It is standby.
It is different according to the property of prepared film, it will select different when thin film transistor (TFT) difference in functionality layer is prepared
Film precursor liquid.For semiconductor channel layer, more options indium, zinc, the inorganic salt solution of tin, based on indium, zinc, tin it is a variety of inorganic
Mixed salt solution, the solution or suspension of class grapheme two-dimension material (such as graphene oxide, MXene);For insulation gate medium
Layer, more options can be used in preparing high-k, the nitrate of the film precursor liquid, such as aluminium, yttrium of height electric leakage rejection ability,
Hafnium, villaumite of zirconium etc.;For source-drain electrode and gate electrode, the inorganic salts of the higher material of more options intrinsic carrier concentration, such as
Indium for preparing ITO electrode, the inorganic salt solution or mixed solution of tin can also select to prepare the nothing of AZO zinc
Machine salting liquid or Diversity solution.
The third aspect, the invention provides a kind of preparation method of memristor, the bottom electrode layer of described memristor, resistive
Any layer in layer and top electrode layer is prepared using the above-mentioned method of the present invention.
The top electrode and hearth electrode of the memristor can be from the above-mentioned precursor liquids for preparing source-drain electrode, and change resistance layer can be with
Select the precursor liquid for preparing above-mentioned semiconductor channel layer and insulation gate dielectric layer.
Compared to realizing Film patterning technique by two-step method in traditional wet method coating process, equally can be real
On the premise of now thin-film patterning, method proposed by the present invention does not influence the quality of plated film, without complex device, coating cost
It is low.This method is widely applicable, solution or suspension of the film precursor liquid either based on water or organic solvent, can pass through
This method realize the deposition of film with it is graphical.In addition, this method can realize the heavy of film simultaneously in membrane-film preparation process
Product is with graphically, and in addition to possessing solwution method and preparing the low-cost advantage of film, also simple with process, workable is bright
Aobvious feature.
Brief description of the drawings
Fig. 1 is substrate and the schematic diagram of template composition microchannel in the graphically preparation process of film of the invention;
Fig. 2 is that the present invention realizes Film patterning operational flowchart;
Fig. 3 is the preparation method flow chart of graphical film of the invention;
Fig. 4 is the graphical MXene prepared in embodiment 1 optical microscope photograph;
Fig. 5 is that the light microscope of the graphical indium gallium cadmium sull electrical performance testing prepared in embodiment 2 shines
Piece;
Fig. 6 is the I-V response curves of the graphical indium gallium cadmium sull prepared in embodiment 2;
Fig. 7 is the transfer characteristic curve of the graphical indium gallium cadmium sull prepared in embodiment 3;
Fig. 8 is the output characteristic curve of the graphical indium gallium cadmium sull prepared in embodiment 3;
Fig. 9 is the structural representation of the memristor prepared in embodiment 4.
Embodiment
In order to more specifically describe the present invention, below in conjunction with the accompanying drawings and embodiment is to technical scheme
It is described in detail.
The key of the inventive method is that microchannel can be constructed by template, referring to Fig. 1, is embodied as this method
Template and the structural representation after substrate attaching in example, it includes substrate, the template above substrate, and by substrate and mould
The microchannel that plate is constructed jointly.It is pointed out that for the aqueous solution, substrate is carried out the necessity of hydrophily processing with it is important
Property be, the substrate after hydrophilic treated provides good infiltration interface, so solution can preferably infiltrate substrate,
The power for pulling solution to be permeated into microchannel is produced in impregnation process due to the surface tension effects of liquid level, solution is driven
Constantly enter in microchannel.
In the method, substrate provides the interface of infiltration, and the microchannel to be formed that is brought into close contact of template and substrate is provided
The good template of pattern customization, by capillarity of the liquid in template realizes the patterning of film precursor liquid, will be molten
The patterning for being achieved that film is dried in agent, and main process is as shown in Figure 2.
Film patterning operating process is realized in the present invention as shown in figure 3, primary operational includes preparing precursor liquid, prepared
Template, structure microchannel, dropwise addition precursor liquid simultaneously dry, go removing template and annealing etc., the film that can be finally patterned.
Embodiment 1
With made membrane precursor liquid:MXene is scattered in ethanol and obtains MXene suspension;Using preceding needing to be surpassed
Acoustic shock, which is swung, prevents MXene particles from settling for 5 minutes or so.
The selection and processing of template:The upper optical graving that passes through is for the template of bar shaped is gone out on a silicon substrate, by macromolecule prepolymer
DOW CORNING SYLRARD184 and its curing agent are well mixed and template precursor liquid are obtained after low pressure deaeration by a certain percentage;Will
Have figuratum substrate to be placed in plastic culture dish, slowly topple over template precursor liquid, template precursor liquid is totally submerged substrate,
Solidify it PDMS insulation a period of times in electrothermal blast furnace, finally the PDMS templates after solidification are carefully opened, obtained
The PDMS templates of patterning.
Choose and handle substrate:Because the surface smoothness degree of silicon chip is high, the p-type silicon chip that the present embodiment chooses heavy doping is made
For substrate, and substrate is cleaned using acetone, second alcohol and water successively, scavenging period is respectively 10 points, 10 minutes, 5 minutes.
Because oxygen plasma processing method has, processing is simple, and processing time is short, the advantages of efficiency high, and the present embodiment uses model
The oxygen plasma machine of the types of Plasma Preen II -862 carries out hydrophilic treated, the oxygen of oxygen plasma machine to the substrate after cleaning
Throughput is arranged between 4~5SCFH, and power setting is 250W, and the hydrophilic treated time is 2 minutes.
Build microchannel:A pre-prepd PDMS templates with bar paten are selected, are fitted in through over cleaning and parent
On the substrate of water process, and applying pressure makes template close with substrate attaching.It should be noted that two when template is prepared
End must reserve microchannel.
Precursor liquid is added dropwise and dries:MXene hanging drops are left into the two ends of microchannel in PDMS templates, and cover it
Template two ends with microchannel;A 50g or so counterweight is placed above template, it is ensured that enter microchannel in the suspension
During remain and closely contact between template and substrate.After 5-10 minutes, it was observed that liquid level is no longer moved in microchannel
It is dynamic, counterweight is removed, after the residual liquid on substrate is blotted, is dried ethanol in electric drying oven with forced convection, due to MXene's
Heat sensitivity, so temperature is 40 DEG C or so by the present invention, drying time is 30 minutes or so.If film precursor liquid is to temperature
More sensitive, the drying of precursor liquid is preferably able to carry out under vacuo.The advantage so handled is, on the one hand, under vacuo,
The boiling point of ethanol equal solvent will be reduced, and temperature can be completed at a lower temperature for the removing of solvent, and solute can be avoided to be heated
And the series reaction occurred;On the other hand, under vacuo, solvent will be become by thermal evaporation be more prone to, thus microchannel
The removing of internal solvent will be more rapid also more thorough.
Remove removing template:Carefully template is torn since one jiao of template, finally given as shown in Figure 4 graphical thin
Film.
Embodiment 2
By In (NO3)3, Ga (NO3)3With Cd (NO3)3By 2:2:1 mol ratio dissolves in ethanol successively, is made into
The nitrate solution of 0.5Mol/L indium gallium cadmium, at room temperature stirring is well mixed 6 hours solution.Afterwards using 0.22 μm
PTFE filters are filtered to the solution, obtain the film precursor liquid of transparent clarification.
The set-up procedure of template is identical with embodiment 1, in this example, the template microchannel width of use and micro-
Spacing between passage is 80 μm.
The p that this example is 100nm from the thermal oxide layer thickness of No.46 Research Institute, China Electronic Science Group Co., Ltd
Type heavy doping thermal oxide silicon chip.Before use, only needing to that the particulate matter of thermal oxide silicon chip surface is removable without into volume using nitrogen
Outer cleaning process.Hydrophilic treated is carried out to the thermal oxide silicon chip afterwards, processing parameter is in the same manner as in Example 1.
Template after solidification is fitted tightly on thermal oxide silicon chip, microchannel is reserved at the two ends of template, will be configured
The nitrate solution of good indium gallium cadmium drops in the microchannel exit of template both sides respectively, and applies above template 50g weight
Code is to ensure being brought into close contact between template and thermal oxide silicon chip during this.
After 5-10 minutes, it was observed that liquid level is no longer moved in microchannel, counterweight is removed, the residual liquid on substrate is blotted
Afterwards, ethanol is dried in electric drying oven with forced convection.The temperature setting of electric drying oven with forced convection is 50 DEG C, and the time is 30 minutes.
After solvent volatilization is dry, template is carefully opened from one jiao of template, the film containing indium gallium cadmium nitrate patterned.
The film containing indium gallium cadmium nitrate of patterning is handled using air anneal stove, specific process is:
300 DEG C are increased to from room temperature, the heating-up time is 45 minutes, is incubated 60 minutes in the case where this is 300 DEG C afterwards, then, and stove to be annealed delays
Sample is taken out after slow cool down to room temperature.
Plated with nickel gold electrode is steamed by electron beam evaporation on the indium gallium cadmium sull on thermal oxidation silicon piece.Its
In, electrode is realized by metal mask plate and patterned, and the electrode of evaporation is the indium gallium cadmium oxide of strip electrode, electrode and bar shaped
Vertically.Evaporation plating parameter is:The plated film speed of metallic nickel isCoating film thickness is 50nm, and golden plated film speed isCoating film thickness is 20nm.
Electric conductivity to the indium gallium cadmium oxide of patterning is characterized.Using semiconductor parameter instrument (Keithley
4200) electrical performance testing is carried out to the indium gallium cadmium sull, the way of contact of probe and film is as shown in figure 5, thin
Current-voltage (I-V) response curve of film is as shown in Figure 6.
Embodiment 3
By In (NO3)3, Ga (NO3)3With Cd (NO3)3By 2:2:1 mol ratio dissolves in ethanol successively, is made into
0.08Mol/L solution, at room temperature stirring is well mixed 6 hours solution.
The preparation of template is identical with embodiment 1 with patterning process, in the present embodiment, and the template of use is micro- logical
Spacing between road width and microchannel is 80 μm.From the heat of No.46 Research Institute, China Electronic Science Group Co., Ltd
Oxidated layer thickness is 100nm p-type heavy doping thermal oxide silicon chip.Thermal oxide silicon chip surface is carried out at cleaning using ordinary nitrogen
Template after solidification, is then fitted tightly on thermal oxide silicon chip, microchannel is reserved at the two ends of template by reason.It will configure
The nitrate solution of indium gallium cadmium drop in the microchannel exits of template both sides respectively.
After standing 5-10 minutes, after the residual liquid on substrate is blotted, dried in 60 DEG C of electric drying oven with forced convection
Ethanol was dried in 60 minutes, then open template, obtain patterning the film containing indium gallium cadmium nitrate.
Carried out using film of patterning of the tubular annealing stove to substrate and on substrate containing indium gallium cadmium nitrate
Annealing.Processing procedure is:Will be from the temperature rise of tubular annealing furnace chamber to 300 DEG C, the heating-up time is 45 minutes, then 300
60 minutes are incubated at DEG C, stove to be annealed takes out sample after being slowly cooled to room temperature.
Plated with nickel gold electrode is steamed by electron beam evaporation on the indium gallium cadmium sull on thermal oxidation silicon piece.Its
Middle electrode realizes and patterned that the electrode of evaporation is the indium gallium cadmium oxide of strip electrode, electrode and bar shaped by metal mask plate
Vertically.Evaporation plating parameter is:The plated film speed of metallic nickel is Coating film thickness is 50nm, and golden plated film speed is
Coating film thickness is 20nm.
Sample is made annealing treatment in atmosphere to improve the Ohmic contact between source-drain electrode and oxide semiconductor,
300 DEG C are annealed into, the time is 60 minutes.
Electric conductivity to the indium gallium cadmium oxide of patterning is characterized.Using semiconductor parameter instrument (Keithley
4200) electrical performance testing is carried out to the metal-oxide film.Before testing, in one jiao of scraping of the thermal oxide piece, work is made
Exposed for the silicon substrate of hearth electrode.The transfer characteristic curve and output characteristic curve for finally measuring the thin film transistor (TFT) are distinguished
As shown in Figure 7 and Figure 8, it is 1.98cm to calculate gained field-effect transistor saturation mobility2/(V s)。
Embodiment 4
By Al (NO3)3Dissolving in deionized water, is made into 0.3Mol/L solution, and stirring at room temperature mixes 6 hours solution
Close uniform.
The preparation of template and patterning process are same as Example 2, in addition, the template used and substrate and substrate
Pretreatment process is also same as Example 2.Afterwards, template is fitted tightly on the thermal oxide silicon chip by hydrophilic treated,
The two ends of template reserve microchannel.The aluminum nitrate solution configured is dropped in the microchannel exit of template both sides respectively.
After standing 5-10 minutes, after the residual liquid on substrate is blotted, dried in 60 DEG C of electric drying oven with forced convection
Solvent was dried in 60 minutes.Then template is opened, patterned film is obtained.
Afterwards, patterned film is made annealing treatment using air anneal stove, specific process is:It is increased to from room temperature
350 DEG C, the heating-up time is 54 minutes, 120 minutes is incubated at 350 DEG C afterwards, then, after stove to be annealed is slowly cooled to room temperature
Sample is taken out.
Horizontal silver electrode is deposited on the aluminum oxide strip film of preparation by electron beam evaporation.Wherein, electrode leads to
Cross metal mask plate and realize patterning.The electrode of evaporation is the film normal of strip electrode, electrode and bar shaped, and evaporation plating parameter is:
The plated film speed of argent isCoating film thickness is 50nm.
Finally, the electric property of the aluminum oxide of patterning is carried out using semiconductor parameter instrument (Keithley 4200)
Characterize, the structural representation of prepared memristor is as shown in Figure 9.
Embodiment described above only expresses the several embodiments of the present invention, and it describes more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (8)
1. a kind of preparation method of graphical film, including:
Step 1, prepare film precursor liquid, and select substrate;
Step 2, the substrate is cleaned, and hydrophilic treated is carried out to the aufwuchsplate for cleaning back substrate;
Step 3, a pre-prepd figuratum template of band is selected, and the template is posted and fixed after hydrophilic treated
On substrate;
Step 4, the film precursor liquid is added dropwise at the microchannel two ends of template and substrate formation, and fills the film precursor liquid
Sub-dip profit template two ends;
Step 5, wait for quietly, it is to be seen no longer to be moved in microchannel to the film precursor liquid, carry out film precursor liquid solvent
Evaporation process, completes the primary solidification of graphical film;
Step 6, confirm film primary solidification after remove removing template, then to substrate and on film make annealing treatment, completion
The graphical preparation of film.
2. the preparation method of graphical film as claimed in claim 1, it is characterised in that described substrate is silicon chip, hot oxygen
Any of SiClx piece, slide, PET, PI, PDMS.
3. the preparation method of graphical film as claimed in claim 1, it is characterised in that described template is based on flexible high
The soft template of molecule or the hard template with substrate formation microchannel.
4. the preparation method of the graphical film as described in claim 1 or 3, it is characterised in that the pattern in described template
For strip striped, width of fringe and fringe spacing are between 0~100 μm.
5. the preparation method of film as claimed in claim 1 graphical, it is characterised in that described film precursor liquid be indium,
Gallium, zinc, cadmium, tin, aluminium, yttrium, hafnium, the mixed solution and graphite of the inorganic salt solution of zirconium or wherein several metal inorganic salt
The solution or suspension of alkene, class grapheme two-dimension material.
6. the preparation method of film as claimed in claim 1 graphical, it is characterised in that described template fixation procedure is:
One quality is acted in the template for 50~300g counterweight, and the template is posted and fixed over the substrate
The time of holding is between 30-300s.
7. a kind of preparation method of thin film transistor (TFT), it is characterised in that the semiconductor channel layer of described thin film transistor (TFT), insulation
Any layer in gate dielectric layer, source-drain electrode layer and gate electrode layer is prepared using any described method of claim 1~6.
8. a kind of preparation method of memristor, it is characterised in that the bottom electrode layer of described memristor, change resistance layer and top electrode layer
In any layer prepared using any described method of claim 1~6.
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CN110146555A (en) * | 2019-05-30 | 2019-08-20 | 河海大学常州校区 | A kind of humidity sensor based on redox graphene humidity sensitive thin film, method of preparation and use |
CN113097074A (en) * | 2021-04-06 | 2021-07-09 | 南京大学 | Patterned electrode integration and surface passivation method of two-dimensional material |
CN113113535A (en) * | 2021-03-30 | 2021-07-13 | 天津理工大学 | Based on MoS2All-solid-state electrolyte memristor and preparation method thereof |
CN118145593A (en) * | 2024-05-09 | 2024-06-07 | 南京邮电大学 | TMDC material patterning method based on soft nano-imprinting |
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CN101061576A (en) * | 2004-06-21 | 2007-10-24 | 3M创新有限公司 | Patterning and aligning semiconducting nanoparticles |
CN101080670A (en) * | 2004-12-13 | 2007-11-28 | 3M创新有限公司 | Method for patterning surface modification |
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CN101061576A (en) * | 2004-06-21 | 2007-10-24 | 3M创新有限公司 | Patterning and aligning semiconducting nanoparticles |
CN101080670A (en) * | 2004-12-13 | 2007-11-28 | 3M创新有限公司 | Method for patterning surface modification |
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CN110146555A (en) * | 2019-05-30 | 2019-08-20 | 河海大学常州校区 | A kind of humidity sensor based on redox graphene humidity sensitive thin film, method of preparation and use |
CN113113535A (en) * | 2021-03-30 | 2021-07-13 | 天津理工大学 | Based on MoS2All-solid-state electrolyte memristor and preparation method thereof |
CN113097074A (en) * | 2021-04-06 | 2021-07-09 | 南京大学 | Patterned electrode integration and surface passivation method of two-dimensional material |
CN113097074B (en) * | 2021-04-06 | 2024-02-09 | 南京大学 | Two-dimensional material patterned electrode integration and surface passivation method |
CN118145593A (en) * | 2024-05-09 | 2024-06-07 | 南京邮电大学 | TMDC material patterning method based on soft nano-imprinting |
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