CN108766890A - A kind of method of low temperature preparation metal oxide thin-film transistor - Google Patents
A kind of method of low temperature preparation metal oxide thin-film transistor Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- 239000010409 thin film Substances 0.000 title claims abstract description 24
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 11
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 11
- 239000010408 film Substances 0.000 claims abstract description 38
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000009832 plasma treatment Methods 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims description 51
- 239000007788 liquid Substances 0.000 claims description 49
- 239000000758 substrate Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 238000004140 cleaning Methods 0.000 claims description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 19
- 229910052710 silicon Inorganic materials 0.000 claims description 19
- 239000010703 silicon Substances 0.000 claims description 19
- 238000000137 annealing Methods 0.000 claims description 17
- 238000003851 corona treatment Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 230000005611 electricity Effects 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000004528 spin coating Methods 0.000 claims description 5
- 238000002207 thermal evaporation Methods 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- 239000007772 electrode material Substances 0.000 claims description 4
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000009841 combustion method Methods 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 238000001548 drop coating Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 238000007641 inkjet printing Methods 0.000 claims description 3
- 229910001510 metal chloride Inorganic materials 0.000 claims description 3
- 229910001512 metal fluoride Inorganic materials 0.000 claims description 3
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 230000033116 oxidation-reduction process Effects 0.000 claims description 2
- 239000012498 ultrapure water Substances 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000003247 decreasing effect Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000012546 transfer Methods 0.000 description 5
- 239000008186 active pharmaceutical agent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 3
- 150000001342 alkaline earth metals Chemical class 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- 229910052735 hafnium Inorganic materials 0.000 description 3
- 238000002161 passivation Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- LKRFCKCBYVZXTC-UHFFFAOYSA-N dinitrooxyindiganyl nitrate Chemical compound [In+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O LKRFCKCBYVZXTC-UHFFFAOYSA-N 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 206010034960 Photophobia Diseases 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 235000003642 hunger Nutrition 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
- 150000002500 ions Chemical class 0.000 description 1
- 208000013469 light sensitivity Diseases 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—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
-
- 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
- H01L21/0242—Crystalline insulating materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02565—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02656—Special treatments
- H01L21/02664—Aftertreatments
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/34—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies not provided for in groups H01L21/0405, H01L21/0445, H01L21/06, H01L21/16 and H01L21/18 with or without impurities, e.g. doping materials
- H01L21/46—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/428
- H01L21/477—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
Abstract
The present invention provides a kind of methods of low temperature preparation metal oxide thin-film transistor, and this method is in low temperature preparation In2O3During film, pass through NH3In after plasma treatment preannealing2O3Film realizes further decreasing for preparation temperature, realizes and In of good performance is prepared under conditions of 130 DEG C of air are annealed 4 hours2O3Film.Scheme of the present invention has at low cost, simple for process, good product performance, environment environmental protection is prepared, the advantages that having a extensive future.Substantially increase the compatibility of TFT and flexible base board.
Description
Technical field
The invention belongs to technical field of semiconductors, and in particular to a kind of side of low temperature preparation metal oxide thin-film transistor
Method.
Background technology
The research of flexible display device gradually causes the attention of domestic and international scientific research personnel.Flexible display device has very high
Potential advantage, such as its is frivolous, is hardly damaged, it is flexible the features such as.Mobile phone, computer, TV have become modern humans' life
In indispensable major part, with the continuous upgrading of consumer experience, at present portable mobile apparatus, wearable display production
The rapid growth of product etc. demand so that Flexible Displays are persistently by the extensive concern of industry.2017SID display weeks are looked back,
As the important component of exhibition, Flexible Displays and printing technology have declared publicly the direction that the following display develops：Flexibility can roll over
Folded, extensible, fusion touches.World-famous display device manufacturer (Samsung, JDI, LG, BOE, heavenly steed etc.) shows one after another
Oneself unique Flexible Displays product.
In order to realize that better user experience, novel flexible display device develop towards transparent electronics.Transparent electricity
Sub- requirement on devices circuit is transparent, and it is to prepare transparent thin film transistor (TFT) (TFT) to realize the key of transparent circuitry.Thin film transistor (TFT)
(TFT) in the integrated component of the switch control element or peripheral driving circuit that are mainly used in various displays.Past
In more than ten years, non-crystalline silicon tft and multi-crystal TFT become the Primary Component in electronic plane display industry.However, non-crystalline silicon tft
There are some inborn physical obstacles：Such as light sensitivity height, field-effect mobility is relatively low and the opacity etc. of material, makes it
It is above limited by very large in integrated etc. the application of OLED pixel driving and LCD and OLED peripheral driving circuits；And
The technological temperature of polycrystalline SiTFT is higher, and cost of manufacture is high, and the uniformity of transistor performance is poor, unsuitable
Large scale FPD and the application of Flexible Displays.Therefore for the development of transparent flexible display technology, there is an urgent need to develop more
For advanced transparent film transistor technology.From 2004, Japanese Tokyo Xi Yexiuxiong seminars of polytechnical university reported tool
Have high visible light transmissivity, high field-effect mobility, good preparation uniformity and consistency, can low temperature preparation IGZO-TFT with
Come, attracts wide attention rapidly.
By the development of nearly more than ten years, it is heavy that oxide TFT has possessed direct current/magnetron sputtering, molecular beam epitaxy, laser pulse
A variety of preparation methods such as product, solwution method.With the development of thin film transistor (TFT), each seminar is dedicated to improving the same of device performance
When, in conjunction with the demand of industrialization, exploitation low price, low temperature, it is simple, nontoxic, be easy to preparation method prepared by large area gradually by
The attention of each seminar.Show that water causes solwution method to remove the device dependence for having solwution method through various preparation method comparative studies
It is low, it is easy to operate, it is easy to control the building-up process of film by chemical property, it can be achieved that prepared by large area, and may be implemented
Other than the features such as nano level uniform preparation.Since water is as solvent, rather than the organic solvents such as common alcohol ether so that water causes
The preparation process of method is healthy, safe, environmental-friendly.Since water quality method does not contain organic substance so that it is relatively low
At a temperature of the preparation of film can be realized, even as low as 200 DEG C are prepared In2O3-TFT.In view of common plastic substrate
The tolerable temperature of (such as PI) is usually less than 200 DEG C, even for newly developed heat safe plastic substrate, due to plastic substrate
The difference of coefficient of thermal expansion between semiconductive thin film, it is still desirable to which the preparation temperature of device is better closer to room temperature, so into one
The preparation temperature that step reduces sull is imperative.
Invention content
To solve the above-mentioned problems, the present invention provides a kind of method of low temperature preparation metal oxide thin-film transistor,
It is characterized in that, the method is in low temperature preparation In2O3During film, pass through NH3In after plasma treatment preannealing2O3It is thin
Film realizes further decreasing for preparation temperature, is then prepared under conditions of 130 DEG C of air are annealed 4 hours functional
In2O3Thin film transistor (TFT)；
Further, it the described method comprises the following steps：
1)：Prepare In2O3The precursor liquid of base or zno-based oxide；
2)：Cleaning and surface active are carried out to substrate；
3)：Prepare sull；
4)：Using NH3The sull of corona treatment precuring；
5)：By NH in step 4)3Film after corona treatment is placed in air annealing device to be moved back with 100-250 DEG C
Fiery annealing temperature 0.5-8 hours；
6)：By NH in step 5)3Film after corona treatment is prepared by the way of thermal evaporation or magnetron sputtering
Source-drain electrode, to realize the preparation of metal oxide thin-film transistor；
Further, precursor liquid includes that water causes method low temperature precursor liquid, combustion method low temperature precursor liquid, oxidation in the step 1)
Reduction method precursor liquid and organic solvent precursor liquid, the predecessor for preparing the precursor liquid include metal nitrate, metal chloride,
Metal fluoride and organic metal salt；
Further, precursor liquid includes doping In in the step 1)2O3Or binary oxide precursor liquid, the doping of ZnO
In2O3Or ternary oxide precursor liquid, the doping In of ZnO2O3Or the quaternary oxide precursor liquid and doping In of ZnO2O3Or ZnO
Multivariant oxide precursor liquid, and then corresponding sull is prepared；
Further, the step 1) is specially that predecessor is dissolved in deionized water or ammonium hydroxide, the magnetic force at 0-100 DEG C
Stirring 0.5-24 hours, forms the precursor liquid of clear, the wherein a concentration of 0.01-0.5mol/L of precursor liquid；
Further, it is deionized water, high purity water, ammonium hydroxide or hydrogen peroxide that the water, which causes the used solvent of method,；
Further, the step 2) includes：
2-1)：Use deionized water, acetone, isopropanol, deionized water in supersonic wave cleaning machine successively the substrate after cutting
In be respectively cleaned by ultrasonic 5-30min, dried up with nitrogen；
2-2)：Substrate after cleaning is put into plasma cleaning intracavitary, in O at 20-100 DEG C21- is handled in plasma
30min so that substrate surface activates, and surface wettability improves；
Further, substrate includes glass, silicon chip, thermal oxide silicon chip and plastic substrate in the step 2)；
Further, the step 3) be specially using spin coating, rod coating, lifting, drop coating or inkjet printing technology system
Wet film is prepared on the substrate surface-treated by step 2) in standby technology, the precursor liquid obtained using step 1)；Big
In gas, it is placed on 50-150 DEG C of preannealing 1-30min in heating dish, obtains the sull of precuring；
Further, plasma treatment process is using NH in the step 4)3As air source, power 1-100W,
Temperature is 25-250 DEG C, processing time 1-40min, and the intake of working gas is 10-200sccm；
Further, the air source NH in the step 4) during plasma treatment3H may be used in gas2With N2Combination
Air source is replaced, i.e., by H2With N2Plasma treatment or H are carried out successively2With N2It is carried out at the same time plasma cleaning；
Further, the step 6) is specially to prepare the electrode material of 20-200nm thickness as source, drain electrode, wherein ditch
Road area breadth length ratio is 1-20, under the conditions of 100-250 DEG C, the good thin film transistor (TFT) of processability；
Further, the electrode material includes Al, Au, Ag, Cu, Ni, Mo, ITO and AZO, the thin film transistor (TFT) packet
Include bottom gate top contact, the contact of bottom gate bottom, top-gated top contact and the contact of top-gated bottom；
Beneficial effects of the present invention are as follows：
1)：Using NH3Sull after corona treatment preannealing can significantly reduce the heat treatment of film
Temperature is, it can be achieved that low temperature preparation metal-oxide film；
2)：With In2O3For film, it is based on solwution method, 180 DEG C of low temperature preparations below is realized, generally requires by means of fast
The special annealings device such as fast annealing stove or vacuum annealing furnace carries out annealing in 1 hour or more, in contrast, the present invention is realizing
During 180 DEG C of low temperature preparations below, manufacturing cost is reduced to a certain extent；
3)：Due to NH2 -, NH2-, N3-The presence of plasma and active group plays film surface certain self-passivation
Effect is conducive to the stability for improving device；
4)：Under the premise of ensureing transistor electricity performance, the low temperature preparation of TFT is further realized, and then reduce and prepare
Influence of the process to flexible substrate；
5) at low cost, simple for process, good product performance prepares environment environmental protection, the advantages that having a extensive future, greatly improves
The compatibility of TFT and flexible base board.
Description of the drawings
Fig. 1 is O2P after plasma treatment cleaning adulterates thermal oxidation silicon piece substrate；
Fig. 2 is the active layer schematic diagram carried out using heating dish after preannealing；
Fig. 3 is NH3The active layer schematic diagram of plasma treatment precuring；
Fig. 4 is the oxide active layer schematic diagram after annealing；
Fig. 5 is to generate source-drain electrode schematic diagram；
Fig. 6 is to have NH under 150 DEG C of preparation temperatures3The TFT of corona treatment active layer is in different VDSUnder transfer it is special
Property schematic diagram；
Fig. 7 is under 150 DEG C of preparation temperatures, and whether there is or not NH3The TFT transfer characteristic schematic diagrams of corona treatment active layer；
Fig. 8 is under 130 DEG C of preparation temperatures, and whether there is or not NH3The TFT transfer characteristic schematic diagrams of corona treatment active layer；
In legend, 1 is p++-Si；2 be 100nm thickness SiO2；3a is the In after preannealing2O3Film；3b is after after annealing
In2O3Film；4a and 4b is Al source-drain electrodes；5 be O2Plasma treatment；6 be NH3Plasma treatment.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.On the contrary, the present invention cover it is any be defined by the claims the present invention spirit and scope on do
Replacement, modification, equivalent method and scheme.Further, in order to make the public have a better understanding the present invention, below to this
It is detailed to describe some specific detail sections in the datail description of invention.It is thin without these for a person skilled in the art
The description of section part can also understand the present invention completely.
The invention will be further described in the following with reference to the drawings and specific embodiments, but not as a limitation of the invention.
Below most preferred embodiment is enumerated for the present invention：
As shown in Fig. 1-Fig. 7, the present invention provides a kind of method of low temperature preparation metal oxide thin-film transistor, the present invention
It is the low temperature preparation method of the metal oxide thin-film transistor based on solwution method, in the premise for ensureing transistor electricity performance
Under, the low temperature preparation of TFT is further realized, and then reduce influence of the preparation process to flexible substrate.The method includes following
Step：
(1)、In2O3The preparation of base or zno-based oxide precursor liquid：This sentences In2O3For the preparation of precursor liquid, by nitre
Sour indium is dissolved in the aqueous solvents such as deionized water or ammonium hydroxide, and magnetic agitation 0.5-24 hours at 0-100 DEG C, it is saturating to obtain clarification
Bright In2O3Precursor liquid, wherein In2O3A concentration of 0.01-0.5mol/L of precursor liquid；
(2), base-plate cleaning and surface active：The use of substrate includes glass, silicon chip, thermal oxide silicon chip, plastic substrate etc.
Common a variety of substrate forms.For this sentences thermal oxidation silicon substrate, thermal oxide silicon chip after cutting use successively deionized water,
Acetone, isopropanol, deionized water are respectively cleaned by ultrasonic 5-30min in supersonic wave cleaning machine, are then dried up with nitrogen；After cleaning
Thermal oxide silicon chip be put into plasma cleaning intracavitary, in O at 20-100 DEG C21-30min is handled in plasma so that substrate surface
Activation, surface wettability improve；
(3), the preparation of sull：Using conventional spin coating, rod coating, lifting, drop coating or inkjet printing technology etc.
Solwution method technology of preparing uses the precursor solution that (1) obtains to be prepared by (2) surface-treated thermal oxidation silicon on piece
Wet film；In an atmosphere, it is placed on 50-150 DEG C of preannealing 1-30min in heating dish.Obtain the sull of precuring；
(4), using NH3The sull of corona treatment precuring.
(5), the plasma treatment process involved in above-mentioned (4) uses NH3As air source, power 1-100W, temperature
It it is 25-250 DEG C, the intake of processing time 1-40min, working gas are 10-200sccm.
(6), by NH in above-mentioned (4)3It is common that film after corona treatment is placed in heating dish, Muffle furnace, batch-type furnace etc.
Air annealing device in annealed 0.5-8 hours with 100-250 DEG C of annealing temperature.
(7), it using thermal evaporation or magnetron sputtering and other electrode preparation methods, prepares and uses on sull
The electrode of 20-200nm thickness as source, is leaked such as Al, Au, Ag, Cu, Ni, Mo, ITO, AZO and other transparent electrode materials
Electrode.Wherein channel region breadth length ratio is 1-20.Prepare the thin film transistor (TFT) of bottom gate top contact type.
(8), the NH involved by above-mentioned (4) and (5)3Corona treatment film surface reduces the method for preparation temperature not only
Suitable for the thin film transistor (TFT) of bottom gate top contact, it is equally applicable to the film of the contact of bottom gate bottom, top-gated top contact, the contact of top-gated bottom
In transistor.
The precursor liquid can be water cause method low temperature precursor liquid, combustion method low temperature precursor liquid, oxidation-reduction method precursor liquid,
Can be common organic solvent precursor liquid, which includes In2O3With binary oxides precursor liquid, each element (example such as ZnO
Such as：Alkali metal, alkaline-earth metal, Al, Hf, Ga, Zn etc.) doping In2O3Or the ternary oxides such as ZnO precursor liquid, various elements (example
Such as：Alkali metal, alkaline-earth metal, Al, Hf, Ga etc.) adulterate quaternarys oxide precursor liquid and other various elements such as InZnO or ZTO
(such as：Alkali metal, alkaline-earth metal, Al, Hf, Ga etc.) codope In2O3Or the multivariant oxides precursor liquid such as ZnO.Its predecessor can
To be metal nitrate, metal chloride, metal fluoride, organic metal salt etc..
The principle of the present invention is as follows：
NH3Free radical is resolved under plasmoid：
NH3→NH2 -+H·
NH2 -→NH2-+H·
NH2-→N3-+ H,
Since the ionic radius of H is minimum, during plasma treatment, H is easier to penetrate into sull
Lacking oxygen is filled up in inside, fills up defect, increases carrier concentration；Since the ionic radius of N is larger, deeper cannot penetrate into
Enter inside sull, but NH2 -, NH2-, N3-Deng the insatiable hunger in metastable active ion and sull surface
It is reacted with key, to realize the self-passivation of film surface, improves the stability of device to a certain extent.Ensureing transistor electricity
Under the premise of performance, to further decrease the preparation temperature of sull.In view of principles above, the present invention relates to H2Deng from
Daughter and N2Plasma handles the method for realizing the preparation temperature for further decreasing sull successively.Using NH3Plasma
Sull after body processing preannealing can significantly reduce the heat treatment temperature of film, it can be achieved that low temperature preparation metal oxygen
Compound.With In2O3For film, it is based on solwution method, 180 DEG C of low temperature preparations below is realized, generally requires by means of short annealing
The special annealings device such as stove or vacuum annealing furnace carries out annealing in 1 hour or more, in contrast, the present invention realize 180 DEG C with
Under low temperature preparation during, reduce manufacturing cost to a certain extent.Furthermore due to NH2 -, NH2-, N3-Plasma and activity
The presence of group plays the role of film surface certain self-passivation, is conducive to the stability for improving device.
Embodiment 1：
Substrate in the present embodiment selects the thermal oxidation silicon wafer that the p of commercially available single-sided polishing is adulterated, thermal oxidation silicon
Thickness is 100nm.Indium nitrate powder is bought in Alfa companies.Specific preparation process is as follows：
Step 1：Prepare In2O3Indium nitrate is dissolved in deionized water, in magnetic agitation platform by precursor liquid according to 0.2mol/L
On be stirred at room temperature 6 hours, obtain the In of water white transparency2O3Precursor liquid is stood with spare；Using the preceding water system using 0.22 μ L
Filtering head filters precursor liquid, to remove insoluble matter impurity；
Step 2：Substrate cleans：Thermal oxide silicon chip after cutting uses deionized water, acetone, isopropanol, deionization successively
Water is respectively cleaned by ultrasonic 10min in supersonic wave cleaning machine, is dried up with nitrogen；
Step 3：As shown in Figure 1, substrate surface activates：Thermal oxide silicon chip after cleaning is put into plasma cleaning intracavitary,
In O under room temperature210min is handled in plasma so that substrate surface activates, and surface wettability improves；
Step 4：The In obtained using step 12O3Precursor solution is spun on the surface-treated thermal oxidation silicon on piece of step 3；
The wet film that will be obtained after spin coating is placed on 120 DEG C of preannealing 10min in heating dish in an atmosphere.It obtains as shown in Figure 2
The sull of precuring；
Step 5：As shown in figure 3, at 150 DEG C, the sull that step 4 is obtained carries out NH3Corona treatment
10min, it is 50W to control its plasma treatment power, NH when work3Air flux be 100sccm；
Step 6：In an atmosphere, the sample that step 5 obtains is placed in heating dish and is annealed 4 hours for 150 DEG C, obtained such as Fig. 4
Shown in In2O3Film；
Step 7：By the way of thermal evaporation, in In2O3The metal Al conducts of 100nm thickness are prepared on film using mask plate
Source, drain electrode.Wherein channel region breadth length ratio is 1000/100 μm.To obtain p as shown in Figure 5++-Si/SiO2(100nm)/
In2O3The thin film transistor (TFT) of the bottom gate top contact type of/Al structures.
Step 8：To the In being prepared2O3- TFT is respectively in VDS=10V and VDSI-V tests are carried out under conditions of=20V,
Its transfer characteristic curve is as shown in Figure 6.
Embodiment 2：
Opposite embodiment 1 casts out the NH of step 5 after carrying out step 1-43Plasma treatment procedure is directly walked
Rapid 6-8.Comparison of the effect of embodiment 2 i.e. as embodiment 1, compares the In after preannealing2O3Film is whether there is or not NH3Plasma
To the influence of the electric property of its TFT under conditions of body processing procedure, as shown in Figure 7.
Embodiment 3：
Step 1：Prepare In2O3Indium nitrate is dissolved in deionized water, in magnetic agitation platform by precursor liquid according to 0.2mol/L
On be stirred at room temperature 6 hours, obtain the In of water white transparency2O3Precursor liquid is stood with spare；Using the preceding water system using 0.22 μ L
Filtering head filters precursor liquid, to remove insoluble matter impurity；
Step 2：Substrate cleans：Thermal oxide silicon chip after cutting uses deionized water, acetone, isopropanol, deionization successively
Water is respectively cleaned by ultrasonic 10min in supersonic wave cleaning machine, is dried up with nitrogen；
Step 3：As shown in Figure 1, substrate surface activates：Thermal oxide silicon chip after cleaning is put into plasma cleaning intracavitary,
In O under room temperature210min is handled in plasma so that substrate surface activates, and surface wettability improves；
Step 4：The In obtained using step 12O3Precursor solution is spun on the surface-treated thermal oxidation silicon on piece of step 3；
The wet film that will be obtained after spin coating is placed on 80 DEG C of preannealing 10min in heating dish in an atmosphere.It obtains as shown in Figure 2 pre-
Cured sull；
Step 5：As shown in figure 3, at 130 DEG C, the sull that step 4 is obtained carries out NH3Corona treatment
10min, it is 50W to control its plasma treatment power, NH when work3Air flux be 100sccm；
Step 6：In an atmosphere, the sample that step 5 obtains is placed in heating dish and is annealed 4 hours for 130 DEG C, obtained such as Fig. 4
Shown in In2O3Film；
Step 7：By the way of thermal evaporation, in In2O3The metal Al conducts of 100nm thickness are prepared on film using mask plate
Source, drain electrode.Wherein channel region breadth length ratio is 1000/100 μm.To obtain p as shown in Figure 5++-Si/SiO2(100nm)/
In2O3The thin film transistor (TFT) of the bottom gate top contact type of/Al structures.
Step 8：To the In being prepared2O3- TFT is respectively in VDSI-V tests are carried out under conditions of=10V, transfer is special
Linearity curve is as shown in Figure 8.
Embodiment 4：
Opposite embodiment 3 casts out the NH of step 5 after carrying out step 1-43Plasma treatment procedure is directly walked
Rapid 6-8.Comparison of the effect of embodiment 4 i.e. as embodiment 3, compares the In after preannealing2O3Film is whether there is or not NH3Plasma
To the influence of the electric property of its TFT under conditions of body processing procedure, as shown in Figure 8.
Embodiment described above, only one kind of the present invention more preferably specific implementation mode, those skilled in the art
The usual variations and alternatives that member carries out within the scope of technical solution of the present invention should be all included within the scope of the present invention.
Claims (9)
1. a kind of method of low temperature preparation metal oxide thin-film transistor, which is characterized in that the method is in low temperature preparation
In2O3During film, pass through NH3In after plasma treatment preannealing2O3Film realizes the further drop of preparation temperature
It is low, In of good performance then is prepared under conditions of 130 DEG C of air are annealed 4 hours2O3Thin film transistor (TFT).
2. according to the method described in claim 1, it is characterized in that, the described method comprises the following steps：
1)：Prepare In2O3The precursor liquid of base or zno-based oxide；
2)：Cleaning and surface active are carried out to substrate；
3)：Prepare sull；
4)：Using NH3The sull of corona treatment precuring；
5)：By NH in step 4)3Film after corona treatment is placed in air annealing device with 100-250 DEG C of annealing temperature
Degree annealing 0.5-8 hours；
6)：By NH in step 5)3Film after corona treatment prepares source and drain electricity by the way of thermal evaporation or magnetron sputtering
Pole, to realize the preparation of metal oxide thin-film transistor.
3. according to the method described in claim 2, it is characterized in that, precursor liquid includes that water causes method low temperature forerunner in the step 1)
Liquid, combustion method low temperature precursor liquid, oxidation-reduction method precursor liquid and organic solvent precursor liquid, prepare the predecessor packet of the precursor liquid
Include metal nitrate, metal chloride, metal fluoride and organic metal salt.
4. according to the method described in claim 2, it is characterized in that, precursor liquid includes doping In in the step 1)2O3Or ZnO
Binary oxide precursor liquid, doping In2O3Or ternary oxide precursor liquid, the doping In of ZnO2O3Or the quaternary oxide of ZnO
Precursor liquid and doping In2O3Or the multivariant oxide precursor liquid of ZnO, and then corresponding sull is prepared.
5. according to the method described in claim 2, it is characterized in that, the step 1) is specially that predecessor is dissolved in deionized water
Or ammonium hydroxide forms the precursor liquid of clear, the wherein concentration of precursor liquid magnetic agitation 0.5-24 hours at 0-100 DEG C
For 0.01-0.5mol/L, it is deionized water, high purity water, ammonium hydroxide or hydrogen peroxide that the water, which causes the used solvent of method,.
6. according to the method described in claim 2, it is characterized in that, the step 2) includes：
2-1)：Use deionized water, acetone, isopropanol, deionized water each in supersonic wave cleaning machine successively the substrate after cutting
It is cleaned by ultrasonic 5-30min, is dried up with nitrogen；
2-2)：Substrate after cleaning is put into plasma cleaning intracavitary, in O at 20-100 DEG C21-30min is handled in plasma, is made
Substrate surface activation is obtained, surface wettability improves.
7. according to the method described in claim 2, it is characterized in that, the step 3) be specially using spin coating, rod coating, lifting,
The technology of preparing of drop coating or inkjet printing technology, the precursor liquid obtained using step 1), surface-treated by step 2)
Substrate on wet film is prepared；In an atmosphere, it is placed on 50-150 DEG C of preannealing 1-30min in heating dish, obtains precuring
Sull.
8. according to the method described in claim 2, it is characterized in that, plasma treatment process is using NH in the step 4)3Make
For air source, power 1-100W, temperature is 25-250 DEG C, processing time 1-40min, and the intake of working gas is 10-
200sccm, the wherein air source in plasma treatment process are NH3Gas uses H2With N2Combination air source, using combination air source when
By H2With N2Plasma treatment or H are carried out successively2With N2It is carried out at the same time plasma cleaning.
9. according to the method described in claim 2, it is characterized in that, the step 6) is specially to prepare the electrode of 20-200nm thickness
Material is 1-20 as source, drain electrode, wherein channel region breadth length ratio, under the conditions of 100-250 DEG C, the good film of processability
Transistor, the electrode material include Al, Au, Ag, Cu, Ni, Mo, ITO and AZO, and the thin film transistor (TFT) includes bottom gate apical grafting
Tactile, bottom gate bottom contact, top-gated top contact and top-gated bottom contact, and substrate includes glass, silicon chip, thermal oxide silicon chip in the step 2)
And plastic substrate.
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