CN101841003B - Double-layer structure deep-ultraviolet transparent conductive film and preparation method thereof - Google Patents
Double-layer structure deep-ultraviolet transparent conductive film and preparation method thereof Download PDFInfo
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- CN101841003B CN101841003B CN2010101382221A CN201010138222A CN101841003B CN 101841003 B CN101841003 B CN 101841003B CN 2010101382221 A CN2010101382221 A CN 2010101382221A CN 201010138222 A CN201010138222 A CN 201010138222A CN 101841003 B CN101841003 B CN 101841003B
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Abstract
The invention relates to a tin-doped indium oxide (ITO)/gallium oxide (Ga2O3) double-layer structure deep-ultraviolet transparent conductive film and a preparation method thereof, and belongs to the technical field of electronic materials. The preparation method comprises the following steps: ultraviolet optical quartz glass is used as the substrate, and radio-frequency magnetron sputtering is carried out on the Ga2O3 ceramic target to prepare a Ga2O3 layer the thickness of which is 30-60 nm; and direct-current magnetron sputtering is carried out on an ITO target to prepare an ITO layer the thickness of which is 15-29 nm. The pressure intensity of argon gas for sputtering is 0.2-2 Pa, the power for radio-frequency sputtering is 50-100 W, the substrate temperature is 200-300 DEG C, the current for direct-current sputtering is 80-150 mA, and the voltage for direct-current sputtering is 200-400 V. The prepared film has the advantages of low resistivity, high transmittivity within the range of visible light, ultraviolet light and deep-ultraviolet light, and other favorable photoelectric properties. The film otained by the method of the invention has wide application prospects in the fields of ultraviolet photoelectric devices and the like.
Description
(1) technical field:
The present invention relates to a kind of double-layer structure deep-ultraviolet transparent conductive film and preparation method thereof, belong to technical field of electronic materials.
(2) background technology:
Deep-UV light-emitting diode is widely used in high-density optic recording, fields such as excitation source, secure communication, space technology, medical treatment and high speed resolution process public hazards material biological and chemical sensor.Up to now, deep uv light source is that the Ultra-Violet Laser and the Gas lamp of media is main flow with gases such as PRK and various double-frequency lasers and solid, has the shortcoming that volume is big, the life-span is short, price is high, is difficult to practical application.Organic electroluminescence device (OLEDs) has obtained people and has paid close attention to widely owing to have characteristics such as high efficiency, high brightness, wide visual angle, low-power consumption, self-luminous, response speed be fast.Organic semiconducting materials is cut out adjustable photoelectric properties through molecule, realizes the deep ultraviolet electroluminescence.Organic deep-UV light-emitting diode has that volume is little, in light weight, voltage is low, electric current is little, brightness is high and advantage such as luminescence response speed is fast; Easily and transistor and the supporting use of integrated circuit; Solar cell for supplying power easy to use can be applied in a lot of fields.
The nesa coating that is used as organic deep-UV light-emitting diode anode electrode plays a part key to organic deep-UV light-emitting diode performance, and nesa coating is born the DUV dual-use function of electrode and the radiation of transmit layer.Present tin oxide (the SnO that studies the more indium oxide of mixing tin (being called for short ITO) film, mixes antimony
2: Sb) film, mix the tin oxide (SnO of fluorine
2: F) film, the optical band gap of mixing the nesa coatings such as zinc oxide (ZnO:Al) film of aluminium are generally less than 3.7eV, and optically transparent wave-length coverage is limited in the 400-700nm visible light wave range, in the ultraviolet light zone, is opaque.Deep-ultraviolet transparent conductive film becomes the bottleneck of restriction deep ultraviolet organic electroluminescence device research.Continuous development along with transparent optical electronics and opto-electronic device requires the transparent region of nesa coating to expand to deep ultraviolet.Deep-ultraviolet transparent conductive film has important application in various fields such as the analytical instrument of ultraviolet photolithographic, ultra-violet light-emitting device, ultraviolet detector, DNA and high protein, ultra-violet curings, and therefore preparing deep-ultraviolet transparent conductive film has very big using value.
Ga
2O
3It is a kind of deep-ultraviolet transparent conductor oxidate of broad stopband; Energy gap 4.8-5.1eV; Corresponding ABSORPTION EDGE is positioned at 240nm-280nm, is the semi-conducting material of direct band gap, reaches more than 80% in the transmitance of ultraviolet region; Remedied traditional nesa coating at the regional opaque shortcoming of deep ultraviolet, Ga
2O
3It is a kind of very potential deep-ultraviolet transparent electric conducting material.In recent years, to Ga
2O
3The research of base nesa coating mainly concentrates on to mix through the cation displacement and improves its photoelectric properties, and studying more is Sn
4+Displacement Ga
3+The Sn doping β-Ga that forms
2O
3Film.Preparation Sn doping β-Ga
2O
3The method of film has pulsed laser deposition (Pulsed laser deposition) method, referring to people's such as Masahiro Orita " the high conduction of low temperature preparation, deep-ultraviolet transparent β-Ga
2O
3Film ", " solid film " 411 (2002) 134-139 (Masahiro Orita, Hidenori Hiramatsu, Hiromichi Ohta, et al.Preparation of highly conductive, deepultraviolet transparent β-Ga
2O
3Thin film at low deposition temperatures, Thin SolidFilms 411 (2002) 134-139).The Sn doping β-Ga of pulsed laser deposition preparation
2O
3Film conductivity 8.2S.cm
-1(resistivity 0.12 Ω .cm), 380-435 ℃ of thin film deposition underlayer temperature.The pulsed laser deposition apparatus expensive is difficult to the large tracts of land film forming; Sn doping β-Ga with the pulsed laser deposition preparation
2O
3Film resistor is too high, and the commercial application that distance is actual also has very big distance.Therefore, be necessary to study a kind of novel deep-ultraviolet transparent conductive film.
(3) summary of the invention:
The object of the present invention is to provide a kind of have commercial production property, a kind of tin-doped indium oxide (ITO)/gallium oxide (Ga that technology stability is good
2O
3) double-layer structure deep-ultraviolet transparent conductive film and preparation method thereof, make its technology simple, with low cost, be convenient to the large tracts of land film forming, the transparency is good to the DUV zone visible for made nesa coating, electric property is superior to Sn doping β-Ga
2O
3Film, photoelectric properties are stable.
The present invention proposes a kind of double-layer structure deep-ultraviolet transparent conductive film, and this nesa coating is by tin-doped indium oxide (ITO)/gallium oxide (Ga
2O
3) two-layer composition, wherein ITO layer thickness 15-29nm, preferably 22nm; Ga
2O
3Layer thickness 30-60nm, preferred 50nm.The ultraviolet optics quartz glass is selected JGS1 far ultraviolet optics quartz glass or JGS2 ultraviolet optics quartz glass for use.
Preparation double-decker tin-doped indium oxide (ITO)/gallium oxide (Ga that the present invention proposes
2O
3) preparation method of deep-ultraviolet transparent conductive film utilizes the rf magnetron sputtering of prior art and method that magnetically controlled DC sputtering combines to prepare double-decker tin-doped indium oxide (ITO)/gallium oxide (Ga
2O
3) deep-ultraviolet transparent conductive film.Preparation of the present invention is to be target with gallium oxide ceramic target and tin-doped indium oxide target, Ga
2O
3Ceramic target purity 99.99wt%, SnO in the ITO target
2/ (In
2O
3+ SnO
2) ratio be 10wt%.With JGS1 far ultraviolet optics quartz glass or JGS2 ultraviolet optics quartz glass is substrate, and substrate dries up with nitrogen gun with acetone, alcohol and deionized water ultrasonic waves for cleaning.With mechanical pump and molecular pump sputtering chamber is vacuumized, sputtering chamber vacuum degree is less than 6.0 * 10
-4Pa.Adjustment mass flowmenter flow velocity and slide valve switch charge into high-purity argon gas in sputtering chamber, make the ar pressure 0.2-2Pa of sputtering chamber.Heated substrates makes substrate temperature 200-320 ℃.Open Ga
2O
3The radio-frequency power supply of ceramic target, sputter Ga in advance
2O
3Ceramic target, radio frequency sputtering power 50-100W; After treating that radio frequency glow discharge is stable, substrate is gone to Ga
2O
3Target position correspondence position sputtering sedimentation Ga
2O
3Layer, thickness 30-60nm.Open the DC power supply of ITO target, preparatory sputtering ITO target, direct current sputtering electric current 80-150mA, direct current sputtering voltage 200-400V; After treating that direct current glow discharge is stable, substrate is gone to ITO target position correspondence position sputtering sedimentation ITO layer, thickness 15-29nm.Substrate disc rotates to guarantee that substrate is in the relative position of different targets during alternating sputtering.Adopt said method to form double-decker tin-doped indium oxide (ITO)/gallium oxide (Ga at last
2O
3) deep-ultraviolet transparent conductive film.
The present invention's preparation technology parameter preferably is following:
Substrate temperature 250-300 ℃, sputter gas ar pressure 0.5-1Pa.Rf magnetron sputtering Ga
2O
3During the target plated film, radio frequency sputtering power 60-80W; During magnetically controlled DC sputtering ITO target plated film, direct current sputtering electric current 100-140mA, direct current sputtering voltage 280-360V.
Double-decker tin-doped indium oxide (ITO)/gallium oxide (Ga that the inventive method makes
2O
3) deep-ultraviolet transparent conductive film thickness is 45-89nm.Can be as required, through control sputter Ga
2O
3Film and ito thin film time are controlled thickness and total film thickness separately.
Experimental result shows, the ITO/Ga of the present invention's preparation
2O
3Bilayer film has Ga
2O
3The deep-ultraviolet transparent optical property of film and the satisfactory electrical conductivity of ito thin film.Under preferred processing condition, promptly substrate temperature 250-300 ℃, sputter gas ar pressure 0.5-1Pa; Ga
2O
3The commodity Ga of rf magnetron sputtering purity 99.99% is adopted in the preparation of film
2O
3Ceramic target, sputtering power 60-80W, sputter thickness 50nm; Magnetically controlled DC sputtering ITO target, SnO in the ITO target are adopted in the preparation of ito thin film
2/ (In
2O
3+ SnO
2) ratio be 10wt%, direct current sputtering electric current 100-140mA, direct current sputtering voltage 280-360V, sputter thickness 22nm.Double-decker 22nmITO/50nmGa
2O
3Film spectrum regional transmission optical wavelength extends to DUV zone (λ＜300nm); At 280nm optical transmittance (not containing substrate) is 77.6%; At 300nm optical transmittance (not containing substrate) is 90.4%; Be higher than 88% at 300-800nm spectral region mean transmissivity (not containing substrate), pellicular front resistance is 323 Ω, and film resiativity is 2.32 * 10
-3Ω .cm.The inventive method has IP prospecting, and the technology cost is low, and the large tracts of land film forming is convenient in stable performance.The deep-ultraviolet transparent conductive film of the present invention preparation has potential using value in the ultraviolet light photo device, have a good application prospect aspect effectively the utilizing of solar cell window electrode pair ultraviolet light wave band and DUV wave band expanding.
(4) description of drawings:
The double-decker 22nmITO/50nmGa of sputter preparation among Fig. 1 embodiment 1
2O
3Film is at the transmittance curve of 200-800nm scope.
The double-decker 22nmITO/40nmGa of sputter preparation among Fig. 2 embodiment 2
2O
3Film is at the transmittance curve of 200-800nm scope.
The double-decker 29nmITO/50nmGa of sputter preparation among Fig. 3 embodiment 3
2O
3Film is at the transmittance curve of 200-800nm scope.
The double-decker 22nmITO/60nmGa of sputter preparation among Fig. 4 embodiment 4
2O
3Film is at the transmittance curve of 200-800nm scope.
The double-decker 15nmITO/50nmGa of sputter preparation among Fig. 5 embodiment 5
2O
3Film is at the transmittance curve of 200-800nm scope.
The double-decker 22nmITO/30nmGa of sputter preparation among Fig. 6 embodiment 6
2O
3Film is at the transmittance curve of 200-800nn scope.
(5) embodiment: following specific embodiments of the invention elaborates:
Embodiment 1:22nmITO/50nmGa
2O
3
Substrate is selected JGS1 far ultraviolet optics quartz glass for use, with acetone, alcohol and deionized water ultrasonic waves for cleaning substrate, dries up with nitrogen gun.Ga with purity 99.99wt%
2O
3Ceramic target is installed in the radio frequency negative electrode target groove in the magnetron sputtering chamber, with SnO
2/ (In
2O
3+ SnO
2) ratio is that the ITO target of 10wt% is installed in the direct current negative electrode target groove in the magnetron sputtering chamber.The JGS1 far ultraviolet optics quartz glass that cleaned is put into substrate holder, insert substrate holder in the substrate disc in the sputtering chamber.With mechanical pump and molecular pump sputtering chamber is vacuumized, make sputtering chamber vacuum degree less than 6.0 * 10
-4Pa.Temperature controller is set, regulates the heating current heated substrates, make substrate temperature be stabilized in 250 ℃.Adjust mass flowmenter flow velocity and slide valve switch, in sputtering chamber, charge into the argon gas of purity 99.99%, make the ar pressure 0.5Pa of sputtering chamber; Open Ga
2O
3The radio-frequency power supply of ceramic target, sputter Ga in advance
2O
3Ceramic target, radio frequency sputtering power 70W, treat that radio frequency glow discharge is stable after, substrate is gone to Ga
2O
3Target position correspondence position sputtering sedimentation Ga
2O
3Layer, thickness 50nm.Open the DC power supply of ITO target, sputtering ITO target in advance, direct current sputtering electric current 120mA, direct current sputtering voltage 320V, treat that direct current glow discharge is stable after, substrate is gone to ITO target position correspondence position sputtering sedimentation ITO layer, thickness 22nm.Substrate disc is rotated to guarantee that substrate is in the relative position of different targets during alternating sputtering.Adopt said method to form double-decker 22nmITO/50nmGa at last
2O
3Deep-ultraviolet transparent conductive film.Prepared double-decker 22nmITO/50nmGa
2O
3Deep-ultraviolet transparent conductive film is as shown in Figure 1 at the transmittance curve of 200-800nm scope.At 280nm optical transmittance (not containing substrate) is 77.6%, is 90.4% at 300nm optical transmittance (not containing substrate), is higher than 88% at 300-800nm spectral region mean transmissivity (not containing substrate), and pellicular front resistance is 323 Ω, and film resiativity is 2.32 * 10
-3Ω .cm.
Embodiment 2:22nmITO/40nmGa
2O
3
Preparation technology is with embodiment 1, and that different is radio frequency sputtering deposition Ga
2O
3Layer thickness 40nm.Adopt above-mentioned technology to form double-decker 22nmITO/40nmGa at last
2O
3Deep-ultraviolet transparent conductive film.Prepared double-decker 22nmITO/40nmGa
2O
3Deep-ultraviolet transparent conductive film is as shown in Figure 2 at the transmittance curve of 200-800nm scope.At 280nm optical transmittance (not containing substrate) is 75.8%, is 82.6% at 300nm optical transmittance (not containing substrate), is higher than 86% at 300-800nm spectral region mean transmissivity (not containing substrate), and pellicular front resistance is 334 Ω, and film resiativity is 2.07 * 10
-3Ω .cm.
Embodiment 3:29nmITO/50nmGa
2O
3
Preparation technology is with embodiment 1, and different is that substrate is selected JGS2 ultraviolet optics quartz glass for use, 300 ℃ of substrate temperatures; Sputter gas ar pressure 1.0Pa, radio frequency sputtering power 60W, direct current sputtering electric current 140mA; Direct current sputtering voltage 360V, sputtering sedimentation ITO layer thickness 29nm.Adopt above-mentioned technology to form double-decker 29nmITO/50nmGa at last
2O
3Deep-ultraviolet transparent conductive film.Prepared 29nmITO/50nm Ga
2O
3Double-layer structure deep-ultraviolet transparent conductive film is as shown in Figure 3 at the transmittance curve of 200-800nm scope.At 280nm optical transmittance (not containing substrate) is 70.9%, is 87.5% at 300nm optical transmittance (not containing substrate), is higher than 88% at 300-800nm spectral region mean transmissivity (not containing substrate), and pellicular front resistance is 262 Ω, and film resiativity is 2.07 * 10
-3Ω .cm.
Embodiment 4:22nmITO/60nmGa
2O
3
Preparation technology is with embodiment 1, and different is 270 ℃ of substrate temperatures, sputter gas ar pressure 0.8Pa, radio frequency sputtering power 80W, radio frequency sputtering deposition Ga
2O
3Layer thickness 60nm, direct current sputtering electric current 100mA, direct current sputtering voltage 280V.Adopt above-mentioned technology to form double-decker 22nmITO/60nmGa at last
2O
3Deep-ultraviolet transparent conductive film.Prepared double-decker 22nmITO/60nmGa
2O
3Deep-ultraviolet transparent conductive film is as shown in Figure 4 at the transmittance curve of 200-800nm scope.At 280nm optical transmittance (not containing substrate) is 72.4%, is 89.7% at 300nm optical transmittance (not containing substrate), is higher than 88% at 300-800nm spectral region mean transmissivity (not containing substrate), and pellicular front resistance is 335 Ω, and film resiativity is 2.74 * 10
-3Ω .cm.
Embodiment 5:15nmITO/50nmGa
2O
3
Preparation technology is with embodiment 1, and different is that substrate is selected JGS2 ultraviolet optics quartz glass for use, 200 ℃ of substrate temperatures; Sputter gas ar pressure 2.0Pa, radio frequency sputtering power 100W, direct current sputtering electric current 150mA; Direct current sputtering voltage 400V, sputtering sedimentation ITO layer thickness 15nm.Adopt above-mentioned technology to form double-decker 15nmITO/50nmGa at last
2O
3Deep-ultraviolet transparent conductive film.Prepared double-decker 15nmITO/50nmGa
2O
3Deep-ultraviolet transparent conductive film is as shown in Figure 5 at the transmittance curve of 200-800nm scope.At 280nm optical transmittance (not containing substrate) is 62.4%, is 73.8% at 300nm optical transmittance (not containing substrate), is higher than 80% at 300-800nm spectral region mean transmissivity (not containing substrate), and pellicular front resistance is 1509 Ω, and film resiativity is 9.7 * 10
-3Ω .cm.
Embodiment 6:22nmITO/30nmGa
2O
3
Preparation technology is with embodiment 1, and different is 320 ℃ of substrate temperatures, sputter gas ar pressure 0.2Pa, radio frequency sputtering power 50W, direct current sputtering electric current 80mA, direct current sputtering voltage 200V, radio frequency sputtering deposition Ga
2O
3Layer thickness 30nm.Adopt above-mentioned technology to form double-decker 22nmITO/30nmGa at last
2O
3Deep-ultraviolet transparent conductive film.Prepared double-decker 22nmITO/30nmGa
2O
3Deep-ultraviolet transparent conductive film is as shown in Figure 6 at the transmittance curve of 200-800nm scope.At 280nm optical transmittance (not containing substrate) is 71.1%, is 77.4% at 300nm optical transmittance (not containing substrate), is higher than 86% at 300-800nm spectral region mean transmissivity (not containing substrate), and pellicular front resistance is 330 Ω, and film resiativity is 1.71 * 10
-3Ω cm.
Claims (10)
1. a double-layer structure deep-ultraviolet transparent conductive film is characterized in that this conducting film is by ITO/Ga
2O
3Two-layer composition, ITO layer thickness 15-29nm wherein, Ga
2O
3Layer thickness 30-60nm.
2. a kind of double-layer structure deep-ultraviolet transparent conductive film according to claim 1 is characterized in that spectral transmission area light wavelength extends to the DUV zone of wavelength less than 300nm, is higher than 80% in 300-800nm spectral region average transmittance.
3. a kind of double-layer structure deep-ultraviolet transparent conductive film according to claim 1 is characterized in that ITO layer thickness 22nm, Ga
2O
3Layer thickness 50nm.
4. the preparation method of a double-layer structure deep-ultraviolet transparent conductive film, it is characterized in that adopting the ultraviolet optics quartz glass is substrate, rf magnetron sputtering Ga in argon atmosphere
2O
3Ceramic target prepares Ga
2O
3Layer, magnetically controlled DC sputtering ITO target prepares the ITO layer.Sputter gas ar pressure 0.2-2Pa, radio frequency sputtering power 50-100W, substrate temperature 200-320 ℃, direct current sputtering electric current 80-150mA, direct current sputtering voltage 200-400V.
5. the preparation method of a kind of double-layer structure deep-ultraviolet transparent conductive film according to claim 4 is characterized in that described ultraviolet optics quartz glass is JGS1 far ultraviolet optics quartz glass or JGS2 ultraviolet optics quartz glass.
6. the preparation method of a kind of double-layer structure deep-ultraviolet transparent conductive film according to claim 4 is characterized in that SnO in the ITO target
2/ (In
2O
3+ SnO
2) ratio be 10wt%.
7. the preparation method of a kind of double-layer structure deep-ultraviolet transparent conductive film according to claim 4 is characterized in that substrate temperature 250-300 ℃.
8. the preparation method of a kind of double-layer structure deep-ultraviolet transparent conductive film according to claim 4 is characterized in that sputter gas ar pressure 0.5-1Pa.
9. the preparation method of a kind of double-layer structure deep-ultraviolet transparent conductive film according to claim 4 is characterized in that rf magnetron sputtering Ga
2O
3During the target plated film, radio frequency sputtering power 60-80W.
10. the preparation method of a kind of double-layer structure deep-ultraviolet transparent conductive film according to claim 4, when it is characterized in that magnetically controlled DC sputtering ITO target plated film, direct current sputtering electric current 100-140mA, direct current sputtering voltage 280-360V.
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| CN102290338B (en) * | 2011-09-15 | 2013-04-10 | 江苏汇景薄膜科技有限公司 | Room-temperature large-area deposition production process for transparent conductive film |
| CN104090433A (en) * | 2014-06-19 | 2014-10-08 | 合肥鑫晟光电科技有限公司 | Array substrate and display device |
| CN109136869B (en) * | 2018-07-17 | 2020-07-31 | 中山市华南理工大学现代产业技术研究院 | Metal gallium oxide-doped transparent conductive film for ultraviolet band and preparation method thereof |
| CN108950482A (en) * | 2018-08-23 | 2018-12-07 | 张治国 | A kind of ultraviolet 300nm is semi-transparent-copper and indium doped transparent conductive film and preparation method thereof |
| CN112420888B (en) * | 2021-01-21 | 2021-04-23 | 华灿光电（浙江）有限公司 | Ultraviolet light-emitting diode epitaxial wafer and preparation method thereof |
| JP7257562B2 (en) * | 2021-04-27 | 2023-04-13 | Ｊｘ金属株式会社 | LAMINATED FUNCTION AS TRANSPARENT CONDUCTIVE FILM, METHOD FOR MANUFACTURING SAME, AND OXIDE SPUTTERING TARGET FOR MANUFACTURING SAME LAMINATED PRODUCT |
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