CN103274435B - Titanium aluminum oxide thin film and preparation method and application thereof - Google Patents
Titanium aluminum oxide thin film and preparation method and application thereof Download PDFInfo
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- CN103274435B CN103274435B CN201310191783.1A CN201310191783A CN103274435B CN 103274435 B CN103274435 B CN 103274435B CN 201310191783 A CN201310191783 A CN 201310191783A CN 103274435 B CN103274435 B CN 103274435B
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Abstract
The invention belongs to the technical field of preparation of transistors, and in particular relates to a titanium aluminum oxide thin film and a preparation method and application thereof. The aluminum oxide titanium thin film is prepared by a sol-gel method. The method comprises the following steps of: with ethylene glycol monomethyl ether as a solvent and concentrated hydrochloric acid as an additive, dissolving Al(C4H9O)3 and Ti(C4H9O)4 in the solvent to form a clear and stable precursor solution; and spirally coating the precursor solution on a glass substrate, and obtaining the aluminum oxide titanium thin film after thermal pretreatment and subsequent high-temperature heat treatment. The invention further relates to a preparation method of a thin film transistor by using titanium aluminum oxide as a gate dielectric layer. According to the IZO thin film transistor with the titanium aluminum oxide as the gate dielectric layer, the switching current ratio is greater than 1*10<6>, the saturation migration rate is greater than 1.1cm<2>/Vs, and the subthreshold amplitude is less than 1.5V/dec.
Description
Technical field
The invention belongs to transistor preparing technical field, be specifically related to a kind of Titanium aluminum oxide thin film and its preparation method and application.
Background technology
Thin film transistor (Thin Film Transistor:TFT) is a kind of field-effect transistor (Field Effect Transistor:FET), is made up of semiconductor active layer and channel layer, medium layer and insulation layer, gate electrode, source electrode and drain electrode.Field-effect transistor relies on the advantages such as its volume is little, lightweight, life-span length, power consumptive province to be widely used in various electronic circuit.In recent years, along with the development of flat panel display, the liquid-crystal display (Liquid Crystal Displays:LCD) driven by TFT, active matrix organic light emitting diode display (Active Matrix/Organic Light Emitting Diode:AMOLED), become the pillar in display field.And thin-film transistor technologies has become the symbolic technology of flat pannel display (FPD), be characterized in the tft array preparing several ten million number micron (μm) sizes on the substrate that diagonal lines number meter (m) is long, formed " large-scale microelectronics ".
Along with improving constantly of monitor resolution, while transistor density increases, size is constantly reducing, the electrical leakage problems having occurred power problems thereupon and caused due to gate dielectric layer lower thickness.Adopt the silicon-dioxide (SiO that high-k (high-k) material substitution is traditional
2) be the approach most possibly solved the problem.Adopt high-k material, except can effective suppressor grid medium layer leakage current, effectively can also reduce the driving voltage of thin film transistor, thus reduction device power consumption, make the appearance of the ultrahigh resolution indicating meter of reduce power consumption become possibility.
In numerous high-k materials, aluminum oxide is owing to having the energy gap (8.9 eV) close with silicon-dioxide, very low leakage current density, and excellent interface performance, paid close attention to widely, adopt its thin film transistor as gate dielectric layer material also of common occurrence.But, blemish in an otherwise perfect thing be that compared with the high-k material common with other, specific inductivity of aluminum oxide is lower (<10).And titanium dioxide is another kind of common high-k material, its specific inductivity up to more than 100, and has the feature of nontoxic pollution-free.Titanium dioxide, because of its narrower energy gap (3.0--3.2 eV), though have high specific inductivity, and is not suitable as gate dielectric layer material.2005, Applied Physics Letters publishes one section and is entitled as: the article of Hybride titanium-aluminum oxide layer as alternative high-k gate dielectric for the next generation of complementary metal-oxide-semiconductor devices, adopt the method for magnetron sputtering to prepare Titanium aluminum oxide thin film, and point out that its excellent dielectric properties can as the equivalent material of high-k of new generation.But the Titanium aluminum oxide thin film adopting collosol and gel to prepare but has no report.
Along with the development of technique of display, the size of indicating meter is increasing, and resolving power is more and more higher, and the consequent is exactly the production cost increased by geometric progression.The chains that high vacuum apparatus and operating cost have almost become restriction oxide compound TFT to develop in large size flat display field.Sol-gel method utilizes organic solvent or the corresponding metallic salt of water dissolution, stirs and form stable colloidal sol, and utilize the method such as rotary coating, spray ink Printing, lift, spray pyrolysis, deposition oxide film under certain temperature condition.As compared to traditional physical vapor deposition (Physical Vapor Deposition, PVD) and chemical vapour deposition (Chemical Vapor Deposition, CVD), solution method is without the need to the vacuum apparatus of costliness; By the proportioning of component each in precursor solution, can effectively control the component preparing film; The film of preparation has the advantage such as planeness that can be comparable with PVD/CVD.
The present invention proposes the compound method of titanium aluminum oxide presoma and the preparation method of film, obtains the Titanium aluminum oxide thin film that surfacing, optics and electric property are excellent, and applies it in IZO thin film transistor, obtains good device performance.
Summary of the invention
The object of the invention is to the methods and applications proposing simple, the lower-cost preparation Titanium aluminum oxide thin film of a kind of technique.
The preparation method of Titanium aluminum oxide thin film provided by the invention, adopt sol-gel method, concrete steps are as follows:
(1) aluminium titanium precursors solution is prepared
Take ethylene glycol monomethyl ether as solvent, by aluminium secondary butylate Al (C
4h
9o)
3dissolve wherein, after stirring formation settled solution through 0.2-1.0 hours, then by tetrabutyl titanate Ti (C
4h
9o)
4dissolve wherein, stirred to clarify solution through 0.2-1.0 hours; Then add the concentrated hydrochloric acid that concentration is 38% wherein, and vibrate, leave standstill 48 hours after the precursor solution of clear stable to be formed and form gel; Wherein the volume ratio of ethylene glycol monomethyl ether and concentrated hydrochloric acid is 10:1-10:3, and in solution, the mol ratio of Al ion, Ti ion is 0.9:0.1-0.1:0.9, Al ion volumetric molar concentration is 0.1-1.5 M;
(2) Titanium aluminum oxide thin film is prepared
Aluminium titanium precursors solution rotating step (1) prepared is coated on glass substrate, thermal pretreatment; Apply precursor solution again, through repeated multiple times, then carry out high-temperature heat treatment in an atmosphere, obtain the Titanium aluminum oxide thin film of target thickness.
In the present invention, the rotating speed of described rotary coating aluminium titanium precursors solution is 2000-6000 revs/min, and each coating time is 20-40 seconds.
In the present invention, described thermal pretreatment temperature is 150-250 DEG C, and each thermal pretreatment time is 5-30 minutes.
In the present invention, the step of described high-temperature heat treatment is, by the film after thermal pretreatment, heats up from room temperature with the temperature rise rate of 5-20 DEG C of per minutes, until 300-500 DEG C, constant temperature maintains 30-240 minutes, then naturally cools to room temperature.
The Titanium aluminum oxide thin film prepared by the present invention has excellent performance, can be used as gate dielectric layer for the preparation of thin film transistor.The concrete steps of preparation are as follows:
(1) depositing Al gate electrode on common glass substrates;
(2) adopt above-mentioned sol-gel method, the substrate of depositing Al gate electrode prepares Titanium aluminum oxide thin film, as gate dielectric layer;
(3) on above-mentioned Titanium aluminum oxide thin film gate dielectric layer, IZO semiconductor film is prepared;
(4) on IZO semiconductor film, prepare source, drain electrode, obtain thin film transistor.
The present invention adopts the concentrated hydrochloric acid of 38% to add in precursor solution as additive, and the introducing of hydrochloric acid effectively can suppress hydrolysis and the alcoholysis process of presoma, guarantees that film is unlikely to the too fast film that causes of hydrolysis in preheating treatment procedure coarse even muddy.Repeatedly Tu method is revolved in preheating again, and revolve Tu with single and prepare compared with the Titanium aluminum oxide thin film of same thickness, the film of preparation has less defect, more excellent dielectric properties, more even curface.Above-mentioned titanium aluminum oxide is adopted to be greater than 1 × 10 as the IZO thin film transistor switch current ratio of gate dielectric layer
6, saturated mobility is greater than 1.1 cm
2/ Vs, subthreshold swing is less than 1.5 V/dec.
Accompanying drawing explanation
Fig. 1 is the transmittance graph of the 150 nm Titanium aluminum oxide thin film prepared in embodiment.
Fig. 2 is the capacitance-voltage scanning curve of the 150 nm Titanium aluminum oxide thin film prepared in embodiment.
Fig. 3 is the surface topography of the 150 nm Titanium aluminum oxide thin film prepared in embodiment.
Fig. 4 is the transfer characteristic curve of the thin film transistor prepared in embodiment.
Fig. 5 is the output characteristic curve of the thin film transistor prepared in embodiment.
Embodiment
Specifically the present invention is set forth further below by embodiment.
A preparation for Titanium aluminum oxide thin film, concrete steps are as follows:
(1) aluminium titanium precursors solution is prepared
Take ethylene glycol monomethyl ether as solvent, by aluminium secondary butylate Al (C
4h
9o)
3dissolve wherein, after stirring formation settled solution through 0.5 hour, then by tetrabutyl titanate Ti (C
4h
9o)
4dissolve wherein, stirred to clarify solution through 0.2 hour, then add the concentrated hydrochloric acid that concentration is 38% wherein, and thermal agitation, stir after after 4 hours and leave standstill 48 hours formation gels.Wherein the volume ratio of ethylene glycol monomethyl ether and concentrated hydrochloric acid is 10:1, and in solution, the mol ratio of Al ion, Ti ion is 1.0:0-0.2:0.8, Al ion volumetric molar concentration is 0.6M.
(2) Titanium aluminum oxide thin film is prepared
Aluminium titanium precursors solution rotating step (1) prepared is coated on glass substrate, repetitive coatings precursor solution after thermal pretreatment, through repeatedly several times after high-temperature heat treatment again in air obtain the Titanium aluminum oxide thin film of target thickness.
Described sol-gel method prepares the method for Titanium aluminum oxide thin film, and rotary coating rotating speed is 4500 revs/min, and the time is 30 seconds.
Described sol-gel method prepares the method for Titanium aluminum oxide thin film, and the thermal pretreatment temperature of employing is 220 DEG C, 5 minutes time; Film after thermal pretreatment, heat up with the temperature rise rate of 10 DEG C of per minutes from room temperature, until 500 DEG C, constant temperature maintains 60 minutes, naturally cools to room temperature.
Adopt described Titanium aluminum oxide thin film as the thin film transistor of gate dielectric layer, concrete preparation method is as follows:
(1) the method depositing Al gate electrode on common glass substrates of thermal evaporation is utilized;
(2) on the substrate of depositing Al gate electrode, the method for revolving Tu (4500 revs/min, 30 seconds time) and thermal pretreatment (220 DEG C, 5 minutes time) is utilized to deposit certain thickness Titanium aluminum oxide thin film;
(3) heated up from room temperature with the temperature rise rate of 10 DEG C of per minutes by above-mentioned film, until 500 DEG C, constant temperature maintains 60 minutes, naturally cools to room temperature, obtains 150 nm titanium aluminum oxide gate dielectric layer films;
(4) on above-mentioned titanium aluminum oxide gate dielectric layer, IZO semiconductor film is prepared;
(5) on IZO semiconductor film, prepare source, drain electrode, obtain thin film transistor
Different al: the transmission curve of Ti mol ratio film as shown in Figure 1.Fig. 2 is the change curve of Titanium aluminum oxide thin film capacitance-voltage scanning curve with Al:Ti mol ratio.Fig. 3 is Al:Ti mol ratio 0.6:0.4, and annealing temperature is 500 DEG C, and the surface topography of the Titanium aluminum oxide thin film of 60 minutes, mean roughness is 0.184 nm.Fig. 4, Fig. 5 are respectively and adopt Al:Ti mol ratio 0.6:0.4 Titanium aluminum oxide thin film as the transfer characteristic curve of the IZO thin film transistor of gate dielectric layer and output characteristic curve.The switch current ratio of device is greater than 1 × 10
6, saturated mobility is greater than 1.1 cm
2/ Vs, subthreshold swing is less than 1.5 V/dec.
Claims (3)
1. a preparation method for Titanium aluminum oxide thin film, is characterized in that concrete steps are as follows:
(1) aluminium titanium precursors solution is prepared
Take ethylene glycol monomethyl ether as solvent, by aluminium secondary butylate Al (C
4h
9o)
3dissolve wherein, after stirring formation settled solution through 0.2-1.0 hours, then by tetrabutyl titanate Ti (C
4h
9o)
4dissolve wherein, stirred to clarify solution through 0.2-1.0 hours; Then add the concentrated hydrochloric acid that concentration is 38% wherein, and vibrate, leave standstill 45-60 hour after the aluminium titanium precursors solution of clear stable to be formed and form gel; Wherein the volume ratio of ethylene glycol monomethyl ether and concentrated hydrochloric acid is 10:1-10:3, and in solution, the mol ratio of Al ion, Ti ion is 0.9:0.1-0.1:0.9, Al ion volumetric molar concentration is 0.1-1.5 M;
(2) Titanium aluminum oxide thin film is prepared
Aluminium titanium precursors solution rotating step (1) prepared is coated on glass substrate, thermal pretreatment; Coated with aluminum titanium precursors solution again, through repeated multiple times, then carries out high-temperature heat treatment in an atmosphere, obtains the Titanium aluminum oxide thin film of target thickness;
Wherein, the rotating speed of described rotary coating aluminium titanium precursors solution is 2000-6000 revs/min, and each coating time is 20-40 seconds; The temperature of described thermal pretreatment is 150-250 DEG C, and each thermal pretreatment time is 5-30 minutes;
The step of described high-temperature heat treatment is, by the film after thermal pretreatment, heats up from room temperature with the temperature rise rate of 5-20 DEG C of per minutes, until 300-500 DEG C, constant temperature maintains 30-240 minutes, then naturally cools to room temperature.
2. the Titanium aluminum oxide thin film prepared by preparation method described in claim 1.
3. Titanium aluminum oxide thin film described in claim 2 is preparing the application in thin film transistor as gate dielectric layer, it is characterized in that concrete steps are as follows:
(1) depositing Al gate electrode on common glass substrates;
(2) adopt preparation method described in claim 1, the substrate of depositing Al gate electrode prepares Titanium aluminum oxide thin film, as gate dielectric layer;
(3) on above-mentioned Titanium aluminum oxide thin film gate dielectric layer, IZO semiconductor film is prepared;
(4) on IZO semiconductor film, prepare source, drain electrode, obtain thin film transistor.
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| CN103746099B (en) * | 2014-01-17 | 2015-10-28 | 江苏华盛精化工股份有限公司 | The preparation method of the carbon fibre material of a kind of tin ash parcel, product and application |
| CN107686121B (en) * | 2017-08-28 | 2019-07-23 | 西安理工大学 | A kind of preparation method of nano oxidized aluminium film |
| CN108486551A (en) * | 2018-04-12 | 2018-09-04 | 西安理工大学 | A kind of preparation method of nano oxidized aluminized coating |
| CN109775739B (en) * | 2019-04-04 | 2020-06-23 | 江南大学 | Anti-poison graded porous nano aluminum oxide material and preparation method thereof |
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| CN101721918A (en) * | 2009-12-31 | 2010-06-09 | 太原理工大学 | Method for preparing TiO2/Al2O3 composite film |
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