CN105428247B - One kind being based on aqueous ultra-thin ZrO2The film crystal tube preparation method of high k dielectric layer - Google Patents
One kind being based on aqueous ultra-thin ZrO2The film crystal tube preparation method of high k dielectric layer Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000013078 crystal Substances 0.000 title claims abstract description 6
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 35
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000010408 film Substances 0.000 claims abstract description 32
- 239000010409 thin film Substances 0.000 claims abstract description 26
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000137 annealing Methods 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 12
- 239000010703 silicon Substances 0.000 claims abstract description 12
- 238000012545 processing Methods 0.000 claims abstract description 7
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000004528 spin coating Methods 0.000 claims description 47
- 239000000243 solution Substances 0.000 claims description 22
- 239000002243 precursor Substances 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 13
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 8
- 238000002207 thermal evaporation Methods 0.000 claims description 7
- 238000005352 clarification Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- 230000002000 scavenging effect Effects 0.000 claims description 3
- 238000002061 vacuum sublimation Methods 0.000 claims description 3
- 150000002169 ethanolamines Chemical class 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000009832 plasma treatment Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000007664 blowing Methods 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 5
- 238000002834 transmittance Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- 238000011160 research Methods 0.000 description 5
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 239000008186 active pharmaceutical agent Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000000306 component Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229940031098 ethanolamine Drugs 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(ii) oxide Chemical compound [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 1
- 229940112669 cuprous oxide Drugs 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005906 dihydroxylation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- ZEWMZYKTKNUFEF-UHFFFAOYSA-N indium;oxozinc Chemical compound [In].[Zn]=O ZEWMZYKTKNUFEF-UHFFFAOYSA-N 0.000 description 1
- 230000007786 learning performance Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
- H01L29/76—Unipolar devices, e.g. field effect transistors
- H01L29/772—Field effect transistors
- H01L29/78—Field effect transistors with field effect produced by an insulated gate
- H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
- H01L29/7869—Thin film transistors, i.e. transistors with a channel being at least partly a thin film having a semiconductor body comprising an oxide semiconductor material, e.g. zinc oxide, copper aluminium oxide, cadmium stannate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/40—Electrodes ; Multistep manufacturing processes therefor
- H01L29/43—Electrodes ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/49—Metal-insulator-semiconductor electrodes, e.g. gates of MOSFET
- H01L29/51—Insulating materials associated therewith
- H01L29/517—Insulating materials associated therewith the insulating material comprising a metallic compound, e.g. metal oxide, metal silicate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—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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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Ceramic Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- Thin Film Transistor (AREA)
Abstract
The invention belongs to semiconductor thin-film transistor preparing technical fields, are related to a kind of based on aqueous ultra-thin ZrO2The film crystal tube preparation method of high k dielectric layer, complete aqueous thin film transistor (TFT) is prepared in conjunction with N-shaped indium oxide and p-type nickel oxide semiconductor channel layer, it selects low-resistance silicon as substrate and gate electrode, the mode that aqueous sol method, UV light processings and thermal annealing are combined is respectively adopted and prepares ultra-thin ZrO2Gate dielectric layer and the good In of high transmittance, chemical stability2O3With NiO semiconductor channel layers, to further prepare high-performance, low energy consumption TFT devices；Its preparation process is simple, and low cost, easy to operate, principle is reliable, good product performance, prepares environmental-friendly, has a extensive future, preparing high performance thin film transistor (TFT) for large area provides feasible scheme.
Description
Technical field:
The invention belongs to semiconductor thin-film transistor preparing technical fields, are related to a kind of based on the thin of the environmentally protective hydrosol
The preparation method of film transistor, especially one kind is with aqueous ultra-thin zirconium oxide (ZrO2) it is high k dielectric layer, with N-shaped indium oxide
(In2O3) and p-type nickel oxide (NiO) be semiconductor channel layer thin film transistor (TFT) preparation method.
Background technology：
In recent years, thin film transistor (TFT) (Thin Film Transistor, TFT) is in driven with active matrix liquid crystal display device
Important function is played in (Active Matrix Liquid Crystal Display, AMLCD), from low temperature amorphous silicon TFT
To high temperature polysilicon TFT, technology is more and more ripe, and application is also from can only drive LCD (Liquid Crystal
Display can not only LCD be driven but also can drive OLED (Organic Light Emitting Display), very by) developing to
To Electronic Paper.TFT has become the core component of FPD industry in past more than ten years, and every display is all integrated with
Millions of or even more than one hundred million a TFT devices.With the development of large scale integrated circuit, as si-substrate integrated circuit core devices
The characteristic size of TFT constantly reduces always, reduces rule and follows Moore's Law.The result of this reduction can not only increase device
Part density reduces unit cost, it is often more important that its each switch operates consumed power and also reduces (IBM therewith
Journal of Research and Development, 43 245,1999).When the feature ruler of super large-scale integration
It is very little when being less than 0.1 μm, silica (SiO2) thickness of dielectric layer is necessarily less than 1.5nm, therefore is difficult control SiO2Film
Pinhold density, so as to cause larger leakage current.Research shows that SiO2When thickness reduces to 1.5nm by 3.5nm grid leakage current by
10-12A/cm2Increase to 10A/cm2(IEEE Electron Device Letters,18209,1997).Larger leakage current meeting
Cause high power consumption and corresponding heat dissipation problem, this all adversely affects device integration, reliability and service life.Mesh
Before, in integrated circuit technology widely used high-k (high k) grid dielectric come increase capacitance density and reduce electric leakage of the grid
Stream, high-g value because of its big dielectric constant, with SiO2In the case of with same equivalent gate oxide thickness (EOT), in fact
Border thickness ratio SiO2Big is more, to solve SiO2The quantum tunneling effect generated due to close to physics thickness limit
(Journal of Applied Physics,89 5243,2001).Therefore it prepares novel, high-performance high-g value and substitutes SiO2
As the top priority of realization large scale integrated circuit.
Since TFT devices are membrane type structures, the electricity of dielectric constant, compactness and the thickness of gate dielectric layer to transistor
Learning performance has important influence.At present as research hotspot high k dielectric materials include ATO (Advanced Materials,
24 2945,2012)、Al2O3(Nature, 489 128,2012)、ZrO2(Advanced Materials,23 971,
2011)、HfO217415,2012) and Y (Journal of Materials Chemistry, 222O3(Applied Physics
123503,2011) etc. Letters, 98.In numerous high-k dielectric materials, ZrO2By its larger dielectric constant (~28),
Wider band gap (5.6eV), the compensation of larger conduction band become the features such as higher channel barrier height of electronics (being more than 2eV)
The primary selection (NPG Asia Materials, 7 e190,2015) of dynamic RAM.So far, ZrO2Film
Preparation mostly uses vacuum technology of preparing, such as molecular beam epitaxy, chemical vapor deposition, electron beam evaporation, magnetron sputtering etc. greatly.This
Class high-vacuum technology needs to rely on expensive equipment and is difficult to realize large area film forming, constrains the life of inexpensive electronic device
Production.In view of new direction-printed electronic device of development of electronic devices in future, preparing film using chemical solution technology will be
One better choice, chemical solution technology superfines, film coating, fiber and other material preparation process in by extensive
Using it has the advantages that its uniqueness：Each component is blended in intermolecular progress during it is reacted, thus the grain size of product is small, equal
Even property is high；Reaction process is easily controllable, some products for being difficult to other methods can be obtained, in addition react at low temperature into
Row, avoids the appearance of high temperature dephasign so that the purity of product, and to prepare the item that device is provided with power on plastics later
Part can make flexible material become a kind of possibility.
Organic system solution is mostly used when currently, preparing film using chemical solution technology as presoma, this method is not only
Increase experimental cost, waste liquid destroys natural environment, is unfavorable for sustainable, Green Development objective.Advanced
Functional Materials,25 2564,2015&DOI:10.1002/adfm.201502612 it is proposed that a kind of utilization
" hydrosol " method prepares the new approaches of ultra-thin high k dielectric film, and successfully prepares high performance yttrium oxide and the high k of scandium oxide
Dielectric film.In addition, by consulting related patents, document, also finds no at present and zirconium oxide is prepared based on water-soluble gluing method
(ZrO2) high k dielectric film and its electronic device relevant report.In hydrosol precursor solution, only metal nitrate and
Deionized water substitutes traditional organic solution (ethylene glycol monomethyl ether etc.) as reaction source, using deionized water and is used as solvent, therefore
Hydrosol technology has many advantages, such as nontoxic, environmentally friendly, cheap compared to conventional organosol method；Additionally due to golden in aqueous solution
It is electrostatical binding to belong between cation and hydrone, has weaker combination energy compared to Covalent bonding together mode in organic solution,
Therefore there is lower decomposition temperature using the film of aqueous solution method spin coating, reliability is prepared using aqueous solution technology
The technical field that high, reproducible, low-temperature decomposition semiconductive thin film is just becoming industrial quarters and scientific research circle is being furtherd investigate.
Currently, using N-shaped indium oxide (In2O3), oxide indium zinc oxygen (IZO) and indium gallium zinc oxygen (IGZO) material be as thin
The preparation of film transistor channel layer and application technology are disclosed document, and numerous studies have been done by the states such as U.S., Japan and Korea S..In2O3Rely on
Its high mobility, amorphous state, high transmittance (visible light>80%) become the strong candidate of semiconductor channel layer material.We
By the access of related patents, document, " hydrosol " method of utilization prepares TFT channel layer and is rarely reported, and is based on aqueous ZrO2High k
The complete aqueous low temperature TFT devices of dielectric layer are even more that nobody sets foot in.In addition, utilizing the report of solwution method TFT most in the prior art
N type semiconductor devices is concentrated on, the research for P-type semiconductor device is almost blank.P-type semiconductor material, such as aoxidize
Nickel (NiO), cuprous oxide and stannous oxide are always microelectronics device as a kind of hole mobile material (N-shaped is electron-transport)
The key breakthrough field of part research urgently broken through, while being also that complementary mos integrated circuit is essential
Component part.After tested, the N-shaped In prepared using above-mentioned material technique2O3/ZrO2With p-type NiO/ZrO2TFT devices not only have
There is higher carrier mobility, and will be greatly improved as the pixel switch of AMLCD with extremely low operation voltage
The aperture opening ratio of active matrix improves brightness, while reducing power consumption；In addition its whole soln preparation process does not depend on expensive Vacuum Deposition
Film device so that cost of manufacture further decreases, and it is very wide that these advantages make it have in following low power consumption electronic display field
Potential market.
Invention content：
It is an object of the invention to overcome disadvantage of the existing technology, seek to design and provide a kind of based on aqueous ultra-thin
ZrO2The film crystal tube preparation method of high k dielectric layer, in combination with n type indium oxides (In2O3) and p-type nickel oxide (NiO) half
Conductor channel layer prepares complete aqueous thin film transistor (TFT) (TFT), selects low-resistance silicon as substrate and gate electrode, is respectively adopted " aqueous
The mode that colloidal sol " method, UV light processings and thermal annealing are combined prepares ultra-thin ZrO2(~10nm) gate dielectric layer and high transmission
The good In of rate, chemical stability2O3With NiO semiconductor channel layers, to further prepare high-performance, low energy consumption TFT devices
Part.
To achieve the goals above, the present invention specifically includes following processing step：
(1)、ZrO2The preparation of precursor solution：By zirconium nitrate Zr (NO3)4·5H2O is dissolved in deionized water, at normal temperatures
The ZrO of the 1-24 hours a concentration of 0.01-0.5mol/L for forming clear of magnetic agitation2Precursor solution；
(2), the preparation of NiO precursor solutions：By nickel acetate C4H6NiO4·4H2O is dissolved in 10mL ethyl alcohol and ethanol amine
In the mixed solvent, the NiO forerunner of the magnetic agitation 1-24 hours at normal temperatures a concentration of 0.01-0.5mol/L for forming clear
Liquid solution, wherein a concentration of 0.01-0.5mol/L of NiO precursor solutions, in the mixed solvent ethyl alcohol and ethanol amine volume ratio are 1-
10:1；
(3)、ZrO2The preparation of film sample：Using plasma cleaning method cleans low-resistance surface of silicon, is cleaning
The ZrO prepared using conventional spin coating technique difference spin-coating step (1) and (2) on two pieces of low-resistance silicon substrates afterwards2Presoma is molten
Liquid and NiO precursor solutions, it is first spin coating 4-8 seconds lower at 400-600 revs/min, then in 3000-6000 revs/min of lower spin coating 15-30
Second, spin coating number is 1-3 times, each spin coating thickness 5-10nm；Film after spin coating is put on roasting glue platform in 100-200 DEG C of item
Cure test sample after progress low temperature baking under part；The cure test sample after baking is existed again after 40~60min of UV light processings
It anneals 1-3 hours at a temperature of 200-600 DEG C, realizes the process of dehydroxylation and metal oxide densification, obtain ZrO2It is thin
Membrane sample；
(4)、In2O3The preparation of channel layer：By indium nitrate In (NO3)3It is dissolved in deionization, it is small that 1-24 is stirred at room temperature
When formed clear a concentration of 0.01-0.5mol/L In2O3Aqueous solution；Then the ZrO obtained in step (3)2Film
Sample surfaces utilize spin coating technique spin coating In2O3Aqueous solution, it is first spin coating 4-8 seconds lower at 400-600 revs/min, then in 2000-
5000 revs/min spin coating 15-30 seconds lower, and spin coating number is 1-3 times, each spin coating thickness 5-10nm；Film after spin coating is put into
120-150 DEG C of roasting glue platform is put into 200-300 DEG C of progress process annealing processing 1-5 hours in Muffle furnace after carrying out curing process, i.e.,
In is prepared2O3Channel layer；
(5), the preparation of NiO raceway grooves：Spin coating technique spin coating NiO forerunner is utilized in the film sample surface that step (3) obtains
Liquid solution, first spin coating 4-8 seconds lower at 400-600 revs/min then spin coating 15-30 seconds lower at 2000-5000 revs/min, spin coating number is
1-3 times, each spin coating thickness 5-10nm；Film after spin coating is put into 120-150 DEG C of roasting glue platform and carries out curing process 30 minutes
After be put into Muffle furnace and carry out 200-300 DEG C of process annealing and handle 1-5 hours, that is, NiO channel layers are prepared；
(6), the preparation in source, drain electrode：Using conventional Vacuum sublimation using stainless steel mask plate respectively in In2O3
With NiO channel layers source metal prepared above, drain electrode to get to based on aqueous ultra-thin ZrO2The N-shaped In of high k dielectric layer2O3And p
Type NiO thin film transistor (TFT)s.
The step (1) of the present invention and the deionized water resistivity involved in (2) are more than 18 M Ω cm.
Plasma clean method involved in the step (3) of the present invention is using oxygen or argon gas as purge gas, work(
Rate is 20-60Watt, and the intake of scavenging period 20-200s, working gas are 20-50SCCM.
N-shaped In prepared by step (5) of the present invention2O3Electrode raceway groove length-width ratio with p-type NiO thin film transistor (TFT)s is 1:4-20,
Thermal evaporation electric current is 30-50A；Source obtained, electric leakage extremely metal Al, Ti or Ni electrodes, thickness of electrode 50-200nm.
Compared with prior art, the present invention haing the following advantages：First, ZrO obtained2The physics of high k gate dielectric layers is thick
Degree is less than 20nm, simultaneously the low-leakage current that has, bulky capacitor density meet microelectronics it is integrated for device size the needs of；
ZrO2The high transmittance that film itself has, it is seen that optical band>90%, meet requirement of the transparent electronics to material itself；
ZrO obtained2Film is amorphous state, it can be achieved that film large area, uniform preparation；Second is that ZrO2Film uses " aqueous sol " work
Skill is prepared, and using nitric acid zirconates and deionized water as reaction source, process is cheap, environmentally protective, and it is sustainable to meet China
Development strategy；Third, the N-shaped In in thin film transistor (TFT)2O3With p-type NiO semiconductor channel layers and ZrO2Dielectric layer utilizes low temperature
Prepared by sol gel process, preparation process does not need high vacuum environment, can carry out in air, reduces production cost, meets " printing
The requirement of electronic device "；Fourth, ZrO2What film was prepared at low temperature, process costs are reduced, to the integrated tool of flexible device
It is of great importance.Fifth, the successful preparation of solwution method p-type NiO TFT, device basis is established for the preparation of next step CMOS；It is made
Standby simple for process, low cost, easy to operate, principle is reliable, good product performance, prepares environmental-friendly, has a extensive future, is big
Area prepares high performance thin film transistor (TFT) and provides feasible scheme.
Description of the drawings：
Fig. 1 be the present invention prepare based on ZrO2The complete aqueous In of high k dielectric layer2O3The structural principle of thin film transistor (TFT) shows
It is intended to.
Fig. 2 be the present invention prepare based on ZrO2The structural principle of the complete aqueous NiO thin film transistor (TFT)s of high k dielectric layer is illustrated
Figure.
Fig. 3 is aqueous ZrO prepared by the present invention2The leakage current test curve figure of high k dielectric layer.
Fig. 4 is aqueous ZrO prepared by the present invention2The capacity measurement curve graph of high k dielectric layer.
Fig. 5 is complete aqueous In prepared by the present invention2O3/ZrO2The output characteristic curve figure of thin film transistor (TFT), wherein grid are inclined
Press VGS=0-2V.
Fig. 6 is complete aqueous In prepared by the present invention2O3/ZrO2The transfer characteristic curve figure of thin film transistor (TFT), wherein source and drain electricity
Press VDS=1V.
Fig. 7 is p-type NiO/ZrO prepared by the present invention2The transfer characteristic curve figure of thin film transistor (TFT), wherein source-drain voltage VDS
=1V.
Specific implementation mode：
It is further illustrated the present invention below by specific embodiment and in conjunction with attached drawing.
Embodiment：
Zirconium nitrate in the present embodiment, nickel nitrate and indium nitrate powder are purchased from Aldrich, and purity is more than 98%；
Its bottom grating structure is with ultra-thin zirconium oxide (ZrO2) for high k dielectric layer and respectively with indium oxide (In2O3) and nickel oxide (NiO) film
Preparation process for the thin film transistor (TFT) of channel layer is：
(1) ultra-thin ZrO is prepared using " aqueous sol " method spin coating2High k dielectric film：
Step 1：Select commercially available single-sided polishing low-resistance silicon as substrate (~0.0015 Ω cm) and gate electrode, low-resistance silicon
Substrate uses hydrofluoric acid, acetone and each 10 minutes of alcohol ultrasonic cleaning substrate successively, high-purity after being rinsed repeatedly with deionized water
Nitrogen dries up；
Step 2：Deionized water 10mL is weighed, zirconium nitrate is dissolved according to 0.1M in aqueous solution, in magnetic agitation after mixing
Under the action of be stirred at room temperature 4 hours formed clarification, water white transparency ZrO2Precursor liquid；
Step 3：Clean low-resistance silicon substrate is put into plasma clean intracavitary, is passed through after chamber is extracted to 0.5Pa
High-purity (99.99%) oxygen, it is 30Watt, scavenging period 120s to control its power, and the intake of oxygen is when work
30SCCM；
Step 4：Prepare ZrO2Sample:The precursor solution prepared in step 2 is spin-coated on to the low-resistance silicon substrate cleaned
On, spin coating number is 2 times, and the parameter of sol evenning machine is set as when spin coating precursor solution：First in 500 revs/min of spin coatings 5 seconds, then
In 5000 revs/min of spin coatings 20 seconds；After spin coating, sample is put into 150 DEG C of baking 10min on roasting glue platform, after curing process
ZrO2Sample UV light processing 40min, after be put into Muffle furnace process annealing and handle, annealing temperature is 250 DEG C, annealing time 1
Hour, obtain ZrO2Sample；
(2) it prepares, spin coating In2O3With NiO precursor solutions, channel layer：
Step 1：After indium nitrate 0.30g and deionized water 10mL are mixed 5.5 are stirred at room temperature under the action of magnetic agitation
Hour formed clarification, water white transparency In2O3Aqueous solution, metal cation total concentration are 0.1M；Again by the nickel acetate of 0.1mol
It is dissolved in 9mL ethyl alcohol and 1 mL ethanol amines, 3h is stirred at room temperature under the action of magnetic agitation after mixing, and to form clarification, light green color saturating
Bright NiO solution；
Step 2：1. preparing In2O3Channel layer:The In that will be prepared in step 12O3Aqueous solution is spin-coated on corona treatment
The ZrO crossed2On sample, the parameter of sol evenning machine is set as when spin coating：5000 revs/min of spin coatings 20 seconds, after spin coating, by sample
150 DEG C of baking 10min on roasting glue platform are put into, the sample after curing process, which is put into process annealing in Muffle furnace, to be handled, annealing temperature
Degree is 250 DEG C, annealing time 1 hour；
2. preparing NiO channel layers：The NiO precursor solutions configured in step 1 are spin-coated on the ZrO that plasma treatment is crossed2
On sample, the parameter of sol evenning machine is set as when spin coating：5000 revs/min of spin coatings 20 seconds, after spin coating, 150 DEG C are put by sample
10min is baked in roasting glue platform, then the low-temperature treatment in Muffle furnace, annealing temperature is 250 DEG C, annealing time 1 hour；
(3) Vacuum sublimation is used to prepare source, leakage metal electrode：
By way of thermal evaporation, in In2O3The stainless steel mask plate system for being 1000/250 μm with breadth length ratio on channel layer
The metal Al of standby 100nm thickness is 40A as source, drain electrode, thermal evaporation electric current, and Al/In is prepared2O3/ZrO2/ Si structures
Thin film transistor (TFT)；It is that 1000/250 μm of stainless steel mask plate prepares 100nm thickness that breadth length ratio is equally used on NiO channel layers
W metal is 60A as source, drain electrode, thermal evaporation electric current, and Ni/NiO/ZrO is prepared2The thin film transistor (TFT) of/Si structures；
(4) to manufactured Al/In2O3/ZrO2/ Si structures (Fig. 1) and Ni/NiO/ZrO2The film of/Si structures (Fig. 2) is brilliant
Body pipe is tested；Aqueous ZrO obtained2Electric leakage current test and capacity measurement the curve difference of dielectric layer are as shown in Figure 3, Figure 4；
Al/In obtained2O3/ZrO2/ Si configuration thin film transistor output characteristic curves are as shown in Figure 5；The Al/In of preparation2O3/ZrO2/
The corresponding transfer characteristic curve of Si configuration thin film transistors is as shown in Figure 6；The Ni/NiO/ZrO of preparation2/ Si structural membrane crystal
Pipe transfer characteristic curve is as shown in fig. 7, wherein Fig. 3, Fig. 5, Fig. 6, Fig. 7 curve are tested by Keithley 2634B semiconductor source tables
It arrives；Fig. 4 curves are tested to obtain by Agilent 4294A.
Claims (1)
1. one kind being based on aqueous ultra-thin ZrO2The film crystal tube preparation method of high k dielectric layer, it is characterised in that with ultra-thin zirconium oxide
It is as the preparation process of the thin film transistor (TFT) of channel layer using indium oxide and nickel oxide film for high k dielectric layer and respectively：
(1) ultra-thin ZrO is prepared using " aqueous sol " method spin coating2High k dielectric film：
Step 1：Select the low-resistance silicon of commercially available single-sided polishing, 0.0015 Ω cm as substrate and gate electrode, low-resistance silicon substrate
Hydrofluoric acid, acetone and each 10 minutes of alcohol ultrasonic cleaning substrate, after being rinsed repeatedly with deionized water, High Purity Nitrogen air-blowing are used successively
It is dry；
Step 2：Deionized water 10mL is weighed, zirconium nitrate is dissolved according to 0.1M in aqueous solution, in the work of magnetic agitation after mixing
Be stirred at room temperature under 4 hours formed clarification, water white transparency ZrO2Precursor liquid；
Step 3：Clean low-resistance silicon substrate is put into plasma clean intracavitary, waits for that plasma clean chamber is extracted to 0.5Pa
It is passed through the oxygen that purity is 99.99% afterwards, it is 30Watt, scavenging period 120s to control its power, and oxygen is passed through when work
Amount is 30SCCM；
Step 4：Prepare ZrO2Sample:The precursor solution prepared in step 2 is spin-coated on the low-resistance silicon substrate cleaned, is revolved
It is 2 times to apply number, and the parameter of sol evenning machine is set as when spin coating precursor solution：First in 500 revs/min of spin coatings 5 seconds, then 5000
Rev/min spin coating 20 seconds；After spin coating, sample is put into 150 DEG C of baking 10min on roasting glue platform, by the ZrO after curing process2
Sample UV light processing 40min, after be put into Muffle furnace process annealing and handle, annealing temperature is 250 DEG C, and annealing time 1 hour obtains
To ZrO2Sample；
(2) it prepares, spin coating In2O3With NiO precursor solutions, channel layer：
Step 1：It is stirred at room temperature under the action of magnetic agitation 5.5 hours after indium nitrate 0.30g and deionized water 10mL are mixed
Formed clarification, water white transparency In2O3Aqueous solution, metal cation total concentration are 0.1M；The nickel acetate of 0.1mol is dissolved in again
3h is stirred at room temperature under the action of magnetic agitation in 9mL ethyl alcohol and 1mL ethanol amines, after mixing and forms clarification, greenish transparent
NiO solution；
Step 2：1. preparing In2O3Channel layer:The In that will be prepared in step 12O3Aqueous solution is spin-coated on plasma treated
ZrO2On sample, the parameter of sol evenning machine is set as when spin coating：5000 revs/min of spin coatings 20 seconds, after spin coating, sample are put into roasting
Sample after curing process is put into process annealing in Muffle furnace and handled by the upper 150 DEG C of bakings 10min of Jiao Tai, annealing temperature 250
DEG C, annealing time 1 hour；
2. preparing NiO channel layers：The NiO precursor solutions configured in step 1 are spin-coated on the ZrO that plasma treatment is crossed2Sample
On, the parameter of sol evenning machine is set as when spin coating：5000 revs/min of spin coatings 20 seconds, after spin coating, 150 DEG C of roasting glues are put by sample
10min is baked in platform, then the low-temperature treatment in Muffle furnace, annealing temperature is 250 DEG C, annealing time 1 hour；
(3) Vacuum sublimation is used to prepare source, leakage metal electrode：
By way of thermal evaporation, in In2O3It is prepared by the stainless steel mask plate for being 1000/250 μm with breadth length ratio on channel layer
The metal Al of 100nm thickness is 40A as source, drain electrode, thermal evaporation electric current, and Al/In is prepared2O3/ZrO2/ Si structures it is thin
Film transistor；It is the metal that 1000/250 μm of stainless steel mask plate prepares 100nm thickness that breadth length ratio is equally used on NiO channel layers
Ni is 60A as source, drain electrode, thermal evaporation electric current, and Ni/NiO/ZrO is prepared2The thin film transistor (TFT) of/Si structures.
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| CN110047942A (en) * | 2019-04-09 | 2019-07-23 | 东华大学 | A kind of aqueous solution composite oxide film transistor and its preparation and application |
| CN110517958A (en) * | 2019-08-09 | 2019-11-29 | 中山大学 | A kind of preparation method of oxide thin film transistor |
| CN110534578B (en) * | 2019-08-15 | 2023-06-30 | 青岛大学 | Thin film transistor, preparation method thereof, array substrate and display panel |
| CN111162118A (en) * | 2020-01-02 | 2020-05-15 | 歌尔股份有限公司 | Field effect transistor and preparation method thereof |
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