CN102226265A - Amorphous oxide thin film and preparation method thereof - Google Patents
Amorphous oxide thin film and preparation method thereof Download PDFInfo
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- CN102226265A CN102226265A CN 201110163539 CN201110163539A CN102226265A CN 102226265 A CN102226265 A CN 102226265A CN 201110163539 CN201110163539 CN 201110163539 CN 201110163539 A CN201110163539 A CN 201110163539A CN 102226265 A CN102226265 A CN 102226265A
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Abstract
The invention discloses an amorphous oxide thin film; the chemical formula of the amorphous oxide thin film disclosed by the invention is InxAlyZnO(2+1.5x+1.5y), wherein 1<=x<=2 and 0<y<2; and the resistivity of the thin film is 10<-4>-10<6> Omega cm, the average transmission of visible light is more than 85% and the surface roughness is less than 1nm. The amorphous oxide thin film is prepared by the magnetron sputtering or pulsed laser deposition method. The In, Al and Zn elements in the thin film have the functions of increasing the mobility, controlling the carrier concentration and enhancing the amorphous state stability. The amorphous oxide thin film is suitable to be used as the channel layer of the thin film transistor or the transparent electrode.
Description
Technical field
The present invention relates to a kind of amorphous oxides film and preparation method thereof.
Background technology
At present, Jue Daduoshuo flat-panel display device all is an Actire matrix display device.In Actire matrix display device, introduce thin film transistor (TFT) switching element and storage capacitance, can improve the display device performance greatly, realize that the video of large vol, high definition and full color shows that this makes TFT become the dominant technology of flat pannel display now.That use in Actire matrix display device at present, mainly is non-crystalline silicon (TFT of α-Si), but α-low (＜1cm of Si-TFT mobility
2/ Vs), can't drive the large size high-clear display, this also is that the following 3D of development shows biggest obstacle.Non-crystalline silicon tft is opaque in the visible region simultaneously, and pixel aperture ratio can not reach 100%, in order to obtain enough brightness, needs to increase light source intensity, thereby increases watt consumption; Si photosensitivity in visible-range is strong in addition, need add mask layer (black matrix), and the process complexity that these all will increase the TFT indicating meter raises the cost, and reduces reliability.
Low and the opaque problem at the non-crystalline silicon tft mobility, a kind of effective solution are to adopt the broad stopband oxide semiconductor material instead of amorphous silicon of high mobility as channel layer.ZnO can grow in rare several oxide compound to obtain the film that crystalline quality is good, mobility is high under lesser temps even room temperature.ZnO also is a kind of wide bandgap semiconductor (energy gap is 3.37eV under the room temperature) simultaneously, in visible-range, has higher transmittance, thereby there is not a problem of non-crystalline silicon sensitivity of light, so the film crystal based on the ZnO material is in control extensive studies in recent years, but, be difficult to satisfy the requirement of flat pannel display large-area uniformity because the ZnO channel layer is a polycrystal film.For these reasons, it is the transparent amorphous oxides of representative with InGaZnO that people have developed, and with respect to polycrystalline ZnO TFT, InGaZnO is that channel layer is applied to can solve inhomogeneity problem in the thin film transistor; With respect to non-crystalline silicon tft, InGaZnO has high mobility, visible transparent, has advantages such as low temperature process.Amorphous oxides will become the critical material of flat pannel display of future generation, also be the critical material that flexible demonstration and full impregnated obviously show.But also there is deficiency in InGaZnO, all is noble metal such as In and Ga, the device cost height, and InGaZnO channel layer and source-drain electrode are difficult for forming good ohmic contact simultaneously, influence the performance of device.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of channel layer that can be used as thin film transistor or as amorphous oxides film of transparency electrode and preparation method thereof.
Amorphous oxides film of the present invention, its chemical formula are In
xAl
yZnO
2+1.5x+1.5y, 1 ≦
x≦ 2,0＜
y＜2, film resiativity is 10
-4~ 10
6Ω cm, mobility is greater than 10cm
2/ Vs, the visible light average transmittances is greater than 85%, and surfaceness is less than 1nm.
Amorphous oxides film of the present invention can adopt magnetron sputtering or pulse laser sediment method preparation, and step is as follows:
1) with pure In
2O
3, pure Al
2O
3Press atomic ratio In:Al:Zn=x:y:1 with pure ZnO, 1 ≦
x≦ 2,0＜
y＜2 ratio sintering is made ceramic target;
2) adopt magnetically controlled sputter method, as target, deposit one deck amorphous oxides film with ceramic target on substrate, sputtering condition is: the distance between target and the substrate is 5～10 cm, and growth room's vacuum tightness is evacuated to 1 * 10 at least
-3Pa, sputtering power are 50 ~ 300W, and working gas is Ar and O
2Mixed gas, oxygen partial pressure is 0 ~ 5%, total pressure is 0.6 ~ 1.2Pa; Growth temperature is a room temperature to 400 ℃;
Perhaps adopt pulse laser sediment method, as target, deposit one deck amorphous oxides film with ceramic target on substrate, mode of deposition is: the distance between target and the substrate is 4～6 cm, and growth room's vacuum tightness is evacuated to 1 * 10
-3Pa, the growth room feeds the O of 0 ~ 100 SCCM
2, the control total pressure is 0.001 ~ 10 Pa, and underlayer temperature is a room temperature to 400 ℃, and regulating laser energy is 50 ~ 300 mJ.
Above-mentioned substrate can be sapphire, quartz, glass, ethylene diester (PET), poly-carbonic acid dead drunk (PC) or polyimide (PI).
Above-mentioned pure In
2O
3, pure Al
2O
3With the purity of pure ZnO all more than 99.99%.
The thickness of amorphous oxides film of the present invention is by growth or depositing time decision, can be used as the channel layer of thin film transistor or as transparency electrode according to the difference of Al content.
The beneficial effect that the present invention compared with prior art has is:
1) In
xAl
yZnO
2+1.5x+1.5y(1 ≦
x≦ 2,0＜
y＜2) be a kind of transparent amorphous oxide semiconductor material, be easy to large-area preparation, good uniformity, roughness of film is low, and the big area magnetron sputtering equipment compatibility with industry is generally used is fit to scale operation.
2) In
xAl
yZnO
2+1.5x+1.5yThe noncrystal membrane preparation temperature is low, can be in lesser temps even room temperature deposition, so can use glass substrate and polymer flexible substrate; This noncrystal membrane still can fine maintenance noncrystalline state under 500 ℃ simultaneously, thereby device subsequent disposal wider range.
3) amorphous In
xAl
yZnO
2+1.5x+1.5yThe relative non-crystalline silicon tft of TFT that film is made channel layer has more excellent performance.At first, because amorphous In
xAl
yZnO
2+1.5x+1.5yMiddle In has than the symmetric 5S of long radius ball-type
2Electronic orbit, adjacent In atom 5S
2The overlapping passage that just forms electric transmission of electronic orbit, thereby amorphous In
xAl
yZnO
2+1.5x+1.5yThe TFT that film is made channel layer has big field-effect mobility; Secondly, In
xAl
yZnO
2+1.5x+1.5yBe the ionic linkage semi-conductor, relatively the semi-conductive non-crystalline silicon of covalent linkage has lower defect state density, thereby compares with non-crystalline silicon tft and to have littler the subthreshold value amplitude of oscillation and operating voltage.
4) amorphous In
xAl
yZnO
2+1.5x+1.5yFilm is made channel layer TFT good uniformity, compares product good article rate height, good stability with ZnO-TFT.
5) amorphous In
xAl
yZnO
2+1.5x+1.5yIn the film, In, Al and Zn element work to improve mobility, control carrier concentration respectively and strengthen non-crystalline state stability.Compare with the InGaZnO-TFT that has invented at present, Al has the effect identical with Ga, can also reduce the TFT off-state current simultaneously.Al is with respect to more cheapness and environmental protection of Ga among the present invention, and product cost is low, is easy to extensively promote and use.
6) amorphous In
xAl
yZnO
2+1.5x+1.5yFilm is made channel layer TFT and is had field-effect mobility height, the subthreshold value amplitude of oscillation and advantages such as operating voltage is little, good stability, is fit to be applied to big area high definition active matrix liquid crystal and shows that (AMLCD) and active matrix organic light-emitting diode show (AMOLED) field.
7) amorphous In
xAl
yZnO
2+1.5x+1.5yFilm is made electrode, has lower surfaceness, has higher visible light transmissivity and good electric property simultaneously concurrently, more is applicable to the electrode of photoelectric device.
Description of drawings
Fig. 1 is as the amorphous In of electrode
xAl
yZnO
2+1.5x+1.5yUltraviolet-visible infrared transmission spectrum.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further illustrated:
Embodiment 1:
1) is 99.99% In with purity
2O
3, Al
2O
3With ZnO powder be source material, press atomic ratio In:Al:Zn=2:1:1 weighing, load weighted powder is poured into is equipped with in agate ball and the alcoholic acid ball grinder, ball milling is 48 hours on ball mill, makes powder fining and uniform mixing.Then raw material is separated oven dry, add binding agent and grind compression moulding.The idiosome of moulding is put into sintering oven,, obtain In 1300 ℃ of sintering 3 hours
2AlZnO
6.5Ceramic target.
2) glass substrate is fixed on the sample tray after cleaning, puts into the reaction vacuum chamber.With In
2AlZnO
6.5Ceramic target is contained on the magnetron sputtering target head.The distance of regulating substrate and target is 7cm.Growth room's vacuum tightness is evacuated to 1 * 10
-3Pa, the growth room feeds Ar and O
2Mixed gas, oxygen partial pressure is 1%, total pressure is that 1 Pa at room temperature deposits, depositing time is 10min, film thickness 50nm.
In
2AlZnO
6.5Film has very high surface finish, and surfaceness is less than 1nm.Resistivity is 10
5Ω cm, visible light average transmittances 90%.
Adopt In
2AlZnO
6.5Film is as the channel layer of thin film transistor, and the field-effect mobility of thin film transistor is 2 cm
2/ Vs, threshold voltage is 10V, switch current ratio is greater than 10
7
Embodiment 2:
1) is 99.99% In with purity
2O
3, Al
2O
3With ZnO powder be source material, press atomic ratio In:Al:Zn=1:0.1:1 weighing.Load weighted powder poured into be equipped with in agate ball and the alcoholic acid ball grinder, ball milling is 48 hours on ball mill, makes powder fining and uniform mixing.Then raw material is separated oven dry, add binding agent and grind compression moulding.The idiosome of moulding is put into sintering oven,, obtain InAl 1300 ℃ of sintering 3 hours
0.1ZnO
2.55Ceramic target.
2) glass substrate is fixed on the sample tray after cleaning, puts into the reaction vacuum chamber.With InAl
0.1ZnO
2.55Ceramic target is contained on the pulsed laser deposition target head.The distance of regulating substrate and target is 5.5cm.Growth room's vacuum tightness is evacuated to 1 * 10
-3Pa, growth room feed the O of 2.2 SCCM
2, the control total pressure is 0.01Pa, and underlayer temperature rises to 350 ℃, and regulating laser energy is 300 mJ, and depositing time is 30 min, film thickness 150nm.
InAl
0.1ZnO
2.55Film has very high surface finish, and surfaceness is less than 1nm.Also have simultaneously excellent electric property and optical property, resistivity is 8 * 10
-4Ω cm, carrier concentration reaches 3 * 10
20Cm
-3, hall mobility is 19 cm
2/ Vs.Average transmittances is seen Fig. 1 greater than 86% in visible-range.
Claims (3)
1. an amorphous oxides film is characterized in that chemical formula is In
xAl
yZnO
2+1.5x+1.5y, 1 ≦
x≦ 2,0＜
y＜2, film resiativity is 10
-4~ 10
6Ω cm, visible light average transmittances are greater than 85%, and surfaceness is less than 1 nm.
2. the preparation method of the described amorphous oxides film of claim 1 is characterized in that step is as follows:
1) with pure In
2O
3, pure Al
2O
3Press atomic ratio In:Al:Zn=x:y:1 with pure ZnO, 1 ≦
x≦ 2,0＜
y＜2 ratio sintering is made ceramic target;
2) adopt magnetically controlled sputter method, as target, deposit one deck amorphous oxides film with ceramic target on substrate, sputtering condition is: the distance between target and the substrate is 5～10 cm, and growth room's vacuum tightness is evacuated to 1 * 10 at least
-3Pa, sputtering power are 50 ~ 300W, and working gas is Ar and O
2Mixed gas, oxygen partial pressure is 0 ~ 5%, total pressure is 0.6 ~ 1.2Pa; Growth temperature is a room temperature to 400 ℃;
Perhaps adopt pulse laser sediment method, as target, deposit one deck amorphous oxides film with ceramic target on substrate, mode of deposition is: the distance between target and the substrate is 4～6 cm, and growth room's vacuum tightness is evacuated to 1 * 10
-3Pa, the growth room feeds the O of 0 ~ 100 SCCM
2, the control total pressure is 0.001 ~ 10 Pa, and underlayer temperature is a room temperature to 400 ℃, and regulating laser energy is 50 ~ 300 mJ.
3. by the preparation method of the described a kind of amorphous oxides film of claim 2, its feature is sapphire, quartz, glass, ethylene diester, the poly-dead drunk or polyimide of carbonic acid at substrate.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173732A (en) * | 2013-03-08 | 2013-06-26 | 北京航空航天大学 | Preparation method of (doped amorphous) p-type transparent conductive oxide films |
| CN103219393A (en) * | 2013-04-16 | 2013-07-24 | 浙江大学 | Amorphous oxide thin film for thin film transistor channel layer and manufacturing method thereof |
| CN104078513A (en) * | 2014-07-15 | 2014-10-01 | 浙江大学 | Amorphous oxide semiconductor film and preparation method and application thereof |
| CN104810387A (en) * | 2013-12-31 | 2015-07-29 | 财团法人工业技术研究院 | P-type metal oxide semiconductor material and method for fabricating the same |
| CN105040107A (en) * | 2015-06-02 | 2015-11-11 | 济南大学 | Additional electrostatic field assisted semiconductor material doping method |
| CN105039875A (en) * | 2015-08-24 | 2015-11-11 | 浙江大学 | Ni-Nb metal thin film with ultra-low roughness and preparation method of Ni-Nb metal thin film |
| CN106711200A (en) * | 2016-10-20 | 2017-05-24 | 浙江大学 | P-type ZnRhMo amorphous oxide semiconductor film and preparation method thereof |
| CN108987468A (en) * | 2018-06-26 | 2018-12-11 | 浙江大学 | A kind of I-V race codope amorphous oxide semiconductor film and thin film transistor (TFT) |
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| JP2001123268A (en) * | 1999-10-28 | 2001-05-08 | Okura Ind Co Ltd | Method for forming transparent conductive film |
| CN101709453A (en) * | 2009-12-14 | 2010-05-19 | 浙江大学 | Method for preparing ZnO doped Al transparent conductive film at room temperature |
| CN201713564U (en) * | 2010-02-02 | 2011-01-19 | 深圳市海森应用材料有限公司 | Izao transparent conductive film |
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2011
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Patent Citations (3)
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| JP2001123268A (en) * | 1999-10-28 | 2001-05-08 | Okura Ind Co Ltd | Method for forming transparent conductive film |
| CN101709453A (en) * | 2009-12-14 | 2010-05-19 | 浙江大学 | Method for preparing ZnO doped Al transparent conductive film at room temperature |
| CN201713564U (en) * | 2010-02-02 | 2011-01-19 | 深圳市海森应用材料有限公司 | Izao transparent conductive film |
Non-Patent Citations (1)
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| 《半导体学报》 20040630 袁国栋等 直流反应磁控溅射Al，N共掺方法生长p型ZnO薄膜及其特性 第668-673页 1-3 第25卷, 第6期 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173732A (en) * | 2013-03-08 | 2013-06-26 | 北京航空航天大学 | Preparation method of (doped amorphous) p-type transparent conductive oxide films |
| CN103173732B (en) * | 2013-03-08 | 2014-12-03 | 北京航空航天大学 | Preparation method of (doped amorphous) p-type transparent conductive oxide films |
| CN103219393A (en) * | 2013-04-16 | 2013-07-24 | 浙江大学 | Amorphous oxide thin film for thin film transistor channel layer and manufacturing method thereof |
| CN104810387A (en) * | 2013-12-31 | 2015-07-29 | 财团法人工业技术研究院 | P-type metal oxide semiconductor material and method for fabricating the same |
| CN104810387B (en) * | 2013-12-31 | 2017-11-28 | 财团法人工业技术研究院 | P-type metal oxide semiconductor material and its manufacture method |
| CN104078513A (en) * | 2014-07-15 | 2014-10-01 | 浙江大学 | Amorphous oxide semiconductor film and preparation method and application thereof |
| CN105040107A (en) * | 2015-06-02 | 2015-11-11 | 济南大学 | Additional electrostatic field assisted semiconductor material doping method |
| CN105039875A (en) * | 2015-08-24 | 2015-11-11 | 浙江大学 | Ni-Nb metal thin film with ultra-low roughness and preparation method of Ni-Nb metal thin film |
| CN106711200A (en) * | 2016-10-20 | 2017-05-24 | 浙江大学 | P-type ZnRhMo amorphous oxide semiconductor film and preparation method thereof |
| CN106711200B (en) * | 2016-10-20 | 2020-05-19 | 浙江大学 | P-type ZnRhMO amorphous oxide semiconductor film and preparation method thereof |
| CN108987468A (en) * | 2018-06-26 | 2018-12-11 | 浙江大学 | A kind of I-V race codope amorphous oxide semiconductor film and thin film transistor (TFT) |
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Application publication date: 20111026 |