CN104480442A - Method for preparing transparent conductive film containing aluminum zinc hydroxide - Google Patents
Method for preparing transparent conductive film containing aluminum zinc hydroxide Download PDFInfo
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- CN104480442A CN104480442A CN201410740483.9A CN201410740483A CN104480442A CN 104480442 A CN104480442 A CN 104480442A CN 201410740483 A CN201410740483 A CN 201410740483A CN 104480442 A CN104480442 A CN 104480442A
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- film
- zinc oxide
- vacuum cavity
- sputtering
- oxide aluminum
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a method for preparing a transparent conductive film containing aluminum zinc hydroxide. The method comprises the following steps: firstly, vacuuming the back bottom of a sputtering vacuum cavity to 8.0*10<-4>Pa, adjusting the temperature of a sample platform to the room temperature, then opening a needle valve, introducing steam into the vacuum cavity, adjusting the steam to 3*10<-3>-1.0*10<-2>Pa through the needle valve, further introducing argon into the vacuum cavity, and adjusting the vacuum degree of the cavity to 0.5-2Pa by using a mass flowmeter, and adjusting the sputtering power to 80-120W and carrying out deposition for 40-60 minutes.
Description
Technical field
The present invention relates to a kind of method preparing hydrogeneous zinc-oxide-base transparent conducting film.
Background technology
Transparent conductive film has low resistivity and high visible light transmissivity, and at solar cell, as fields such as silica-based solar cell, cadmium telluride thin-film battery and copper indium gallium selenide film batteries, and the field such as energy-saving window has a wide range of applications.Current investigation and application is ito thin film the most widely, but the crustal abundances such as its starting material In used are very low, resource-constrained, therefore its price is higher, and with the increase of application quantity, price will go up fast, the development of the emerging industries such as serious restriction solar cell.By zinc-oxide-base transparent conducting film prepared by the element dopings such as Al, Sc, Ga, performance and ito thin film close, and its prices of raw and semifnished materials are cheap.Preparation technology at present for zinc-oxide-base transparent conducting film has carried out a large amount of research work, but when preparing zinc oxide in large size base transparent conducting film, homogeneity and reliability of technology become distinct issues, restrict it and replace the application of ito thin film in fields such as solar cells.
The industrialized process for preparing of zinc-oxide-base transparent conducting film mainly contains magnetically controlled DC sputtering, rf magnetron sputtering and pulsed magnetron sputtering, uses the zinc oxide ceramic target that target is mainly alumina doped.Pass into oxygen during deposition, improve the optical property of film, but oxygen partial pressure interval is less, technique controlling difficulty strengthens.In sputter procedure, high oxygen partial pressure easily produces negative oxygen ion reverse sputtering, comparatively serious to film bombardment, introduces stress, causes film over-all properties to decline.Hydrogen enters zinc oxide aluminum film lattice or is compounded to form shallow donor with Lacking oxygen, increases the carrier concentration of film, thus improves Electrical performance.In sputtering atmosphere, introduce hydrogen is the conventional means realizing hydrogen doping, and hydrogen atom combination can be very high in hydrogen, only there is minute quantity by plasma body ionization, produce a small amount of hydrogen atom, therefore when using hydrogen to carry out hydrogen doping, doping efficiency is not high, and there is part hydrogen molecule and enter film, and these hydrogen molecules improve electric property and are no advantage, cause larger lattice distortion on the contrary, make Film Optics penalty.
Summary of the invention
The object of the invention is to overcome prior art hydrogen doping process Middle molecule hydrogen to enter film and cause performance degradation, hydrogen doping efficiency low, and when relatively preparing film under elevated oxygen level, the shortcoming of the problems such as the gravitation introduced by negative oxygen ion reverse sputtering, proposes a kind of method preparing hydrogeneous zinc oxide aluminum transparent electroconductive film.
Preparation method of the present invention is rf magnetron sputtering, and target adopts the zinc oxide aluminum ceramic target of alumina weight per-cent 3%, and substrate is common soda glass.The present invention with the water vapour being contained in sealing water pot in mixture of ice and water and being formed for reactant gases, due to mixture of ice and water at ambient pressure homo(io)thermism be 0 DEG C, therefore the present invention adopts needle-valve and thermostat to control vapor flow.Use high purity oxygen for compared with reactant gases with traditional technology, cheap.
The present invention is under the effect of magnetron sputtering glow plasma, and water vapour decomposes Generation of atoms hydrogen and atomic oxygen.Hydrogen atom can enter zinc oxide aluminum transparent electroconductive film and form shallow donor, improve its electric property, because hydrogen atom is small-sized, the lattice distortion entering film generation is very little, in vacuum cavity, most of hydrogen exists with atomic form, hydrogen molecule quantity is little, and the probability that hydrogen enters film with molecular form is very little, and the transparent conductive film that therefore prepared by the present invention has low resistivity and high transmitance.Hydrogen atom can etch the zinc oxide aluminum film in growth simultaneously, is etched away high-energy regions high for defect concentration, increases roughness of film, reduces the optical reflection of film.Zinc oxide aluminum transparent electroconductive film prepared by the present invention, for solar cell, can improve photon utilization ratio, thus improves battery conversion efficiency.Hydrogen can enter the Lacking oxygen in film, and is passivated, and prevents in use procedure, and the oxygen molecule in air is adsorbed on Lacking oxygen place, affects its performance, to improve it in the total stability of use procedure.
Zinc oxide aluminum ceramic target contains Sauerstoffatom, and during Slag coating zinc oxide aluminum transparent electroconductive film, the oxygen partial pressure passing into vacuum cavity requires lower.When using water vapour as reactant gases, decompose the Sauerstoffatom activity generated high, therefore compared with ordinary method, with water vapour as reactant gases, zinc oxide aluminum film can be prepared under extremely low oxygen partial pressure, thus the negative oxygen ion reverse sputtering that can greatly reduce in sputter procedure, improve thin-film electro performance.
The present invention adopts zinc oxide aluminum ceramic target radio frequency magnetron sputtering method, and step is as follows:
(1) successively with acetone, deionized water, alcohol ultrasonic cleaning soda-lime glass substrate 5min, then dry soda-lime glass substrate, this substrate is loaded the sample table of magnetron sputtering equipment, zinc oxide aluminum ceramic target is installed;
(2) open magnetron sputtering equipment vacuum pump set, the vacuum cavity back end vacuum of magnetron sputtering equipment is evacuated to 8.0 × 10
-4pa, sample table does not heat;
(3) water storing tank is put into the bubble chamber that mixture of ice and water is housed, and thermal equilibrium 20min; By mixture of ice and water and needle-valve co-controlling vapor flow that homo(io)thermism under normal pressure is 0 DEG C;
(4) open the needle-valve connected on water storing tank pipeline, water storing tank is connected with vacuum cavity stainless steel gas circuit, in vacuum cavity, pass into water vapour; Adjust vapor flow by needle-valve, make the pressure range of water vapour be 3 × 10
-3pa ~ 1.0 × 10
-2pa; In vacuum cavity, pass into argon gas again, adjust the vacuum tightness of vacuum cavity to 0.5Pa ~ 2Pa by mass flowmeter.Start sputtering, sputtering power is adjusted to 80W ~ 120W.After aura is stable, remove baffle plate, start deposited oxide zinc-aluminium film, depositing time is 40min ~ 60min, deposits complete taking-up zinc oxide aluminum film sample.
Described zinc oxide aluminum ceramic target purity is 99.99%, wherein Al
2o
3weight percent is 3%, and target-substrate distance is 110mm, and prepared zinc oxide aluminum film thickness is 800nm.
Beneficial effect of the present invention is: the present invention take water vapour as reactant gases, prepares hydrogeneous zinc oxide aluminum transparent electroconductive film by sputtering zinc oxide aluminium ceramic target.The reactant gases that the method uses is cheap, and sputtering technology reliability is high, is introduced by hydrogen in film, and prepared zinc oxide aluminum film can keep high transmitance while having low resistivity, film excellent combination property.
Accompanying drawing explanation
Fig. 1 is film transmission rate and the reflectivity collection of illustrative plates of the embodiment of the present invention 1 preparation;
Fig. 2 is film transmission rate and the reflectivity collection of illustrative plates of the embodiment of the present invention 2 preparation;
Fig. 3 is film transmission rate and the reflectivity collection of illustrative plates of the embodiment of the present invention 3 preparation;
Fig. 4 is film transmission rate and the reflectivity collection of illustrative plates of the embodiment of the present invention 4 preparation;
Fig. 5 is film transmission rate and the reflectivity collection of illustrative plates of the embodiment of the present invention 5 preparation.
Embodiment
Embodiment 1
(1) with acetone, deionized water, alcohol successively ultrasonic cleaning soda-lime glass substrate 5min, load the sample table of magnetron sputtering equipment after drying, and zinc oxide aluminum ceramic target is installed;
(2) open vacuum pump set, sputtering vacuum cavity back end vacuum is evacuated to 8.0 × 10
-4pa, sample table does not heat;
(3) water storing tank is put into mixture of ice and water, and thermal equilibrium 20min;
(4) open the needle-valve on water storing tank pipeline, in vacuum cavity, pass into water vapour.Adjusting water vapour by needle-valve is 3 × 10
-3pa; In vacuum cavity, pass into argon gas again, by mass flowmeter adjustment chamber vacuum to 1.0Pa, open sputtering, sputtering power is increased to 80W, after aura is stable, remove baffle plate, start deposited oxide zinc-aluminium film, depositing time is 60min.
Described zinc oxide aluminum ceramic target purity is 99.99%, Al
2o
3weight percent content is 3%, and target-substrate distance is 110mm, and the film thickness of preparation is 800nm.
Fig. 1 is transmittance curve and the reflectance curve of transparent conductive film ultraviolet-visible-infrared spectrophotometer test prepared by the present embodiment, and its 400nm ~ 800nm scope average transmittances is 89%, and resistivity is 4.2 × 10
-4Ω cm, surfaceness is 10nm.
Embodiment 2
(1) with acetone, deionized water, alcohol successively ultrasonic cleaning soda-lime glass substrate 5min, load the sample table of magnetron sputtering equipment after drying, and zinc oxide aluminum ceramic target is installed;
(2) open vacuum pump set, sputtering vacuum cavity back end vacuum is evacuated to 8.0 × 10
-4pa, sample table does not heat;
(3) water storing tank is put into mixture of ice and water, and thermal equilibrium 20min;
(4) open the needle-valve on water storing tank pipeline, in vacuum cavity, pass into water vapour.Adjusting water vapour by needle-valve is 8 × 10
-3pa; In vacuum cavity, pass into argon gas again, by mass flowmeter adjustment chamber vacuum to 1.0Pa, open sputtering, sputtering power is increased to 120W, after aura is stable, remove baffle plate, start deposited oxide zinc-aluminium film, depositing time is 40min.
Described zinc oxide aluminum ceramic target purity is 99.99%, Al
2o
3weight percent content is 3%, and target-substrate distance is 110mm, and the film thickness of preparation is 800nm.
Fig. 2 is transmittance curve and the reflectance curve of transparent conductive film ultraviolet-visible-infrared spectrophotometer test prepared by the present embodiment, and its 400nm ~ 800nm scope average transmittances is 87%, and resistivity is 3.6 × 10
-4Ω cm, surfaceness is 16nm.
Embodiment 3
(1) with acetone, deionized water, alcohol successively ultrasonic cleaning soda-lime glass substrate 5min, load the sample table of magnetron sputtering equipment after drying, and zinc oxide aluminum ceramic target is installed;
(2) open vacuum pump set, sputtering vacuum cavity back end vacuum is evacuated to 8.0 × 10
-4pa, sample table does not heat;
(3) water storing tank is put into mixture of ice and water, and thermal equilibrium 20min;
(4) open the needle-valve on water storing tank pipeline, in vacuum cavity, pass into water vapour.Adjusting water vapour by needle-valve is 1.0 × 10
-2pa; In vacuum cavity, pass into argon gas again, by mass flowmeter adjustment chamber vacuum to 0.5Pa, open sputtering, sputtering power is increased to 100W, after aura is stable, remove baffle plate, start deposited oxide zinc-aluminium film, depositing time is 50min.
Described zinc oxide aluminum ceramic target purity is 99.99%, Al
2o
3weight percent content is 3%, and target-substrate distance is 110mm, and the film thickness of preparation is 800nm.
Fig. 3 is transmittance curve and the reflectance curve of transparent conductive film ultraviolet-visible-infrared spectrophotometer test prepared by the present embodiment, and its 400nm ~ 800nm scope average transmittances is 88%, and resistivity is 4.0 × 10
-4Ω cm, surfaceness is 14nm.
Embodiment 4
(1) with acetone, deionized water, alcohol successively ultrasonic cleaning soda-lime glass substrate 5min, load the sample table of magnetron sputtering equipment after drying, and zinc oxide aluminum ceramic target is installed;
(2) open vacuum pump set, sputtering vacuum cavity back end vacuum is evacuated to 8.0 × 10
-4pa, sample table does not heat;
(3) water storing tank is put into mixture of ice and water, and thermal equilibrium 20min;
(4) open the needle-valve on water storing tank pipeline, in vacuum cavity, pass into water vapour.Adjusting water vapour by needle-valve is 8.0 × 10
-3pa; In vacuum cavity, pass into argon gas again, by mass flowmeter adjustment chamber vacuum to 2.0Pa, open sputtering, sputtering power is increased to 100W, after aura is stable, remove baffle plate, start deposited oxide zinc-aluminium film, depositing time is 45min.
Described zinc oxide aluminum ceramic target purity is 99.99%, Al
2o
3weight percent content is 3%, and target-substrate distance is 110mm, and the film thickness of preparation is 800nm.
Fig. 4 is transmittance curve and the reflectance curve of transparent conductive film ultraviolet-visible-infrared spectrophotometer test prepared by the present embodiment, and its 400nm ~ 800nm scope average transmittances is 85%, and resistivity is 5.8 × 10
-4Ω cm, surfaceness is 20nm.
Embodiment 5
(1) with acetone, deionized water, alcohol successively ultrasonic cleaning soda-lime glass substrate 5min, load the sample table of magnetron sputtering equipment after drying, and zinc oxide aluminum ceramic target is installed;
(2) open vacuum pump set, sputtering vacuum cavity back end vacuum is evacuated to 8.0 × 10
-4pa, sample table does not heat;
(3) water storing tank is put into mixture of ice and water, and thermal equilibrium 20min;
(4) open the needle-valve on water storing tank pipeline, in vacuum cavity, pass into water vapour.Adjusting water vapour by needle-valve is 1.0 × 10
-2pa; In vacuum cavity, pass into argon gas again, by mass flowmeter adjustment chamber vacuum to 1.5Pa, open sputtering, sputtering power is increased to 120W, after aura is stable, remove baffle plate, start deposited oxide zinc-aluminium film, depositing time is 40min.
Described zinc oxide aluminum ceramic target purity is 99.99%, Al
2o
3weight percent content is 3%, and target-substrate distance is 110mm, and the film thickness of preparation is 800nm.
Fig. 5 is transmittance curve and the reflectance curve of transparent conductive film ultraviolet-visible-infrared spectrophotometer test prepared by the present embodiment, and its 400nm ~ 800nm scope average transmittances is 83%, and resistivity is 5.3 × 10
-4Ω cm, surfaceness is 19nm.
Claims (3)
1. prepare a method for hydrogeneous zinc-oxide-base transparent conducting film, it is characterized in that, described preparation method adopts ceramic target rf magnetron sputtering, and step is as follows:
(1) the back end vacuum of sputtering vacuum cavity is evacuated to 8.0 × 10
-4pa;
(2) water pot is put into the bubble chamber that mixture of ice and water is housed, and thermal equilibrium 20min;
(3) open the needle-valve on the pipeline connecting water storing tank, in vacuum cavity, pass into water vapour, adjustment needle-valve, adjustment passes into the vapor flow of vacuum cavity, and controlling water vapour pressure is 3 × 10
-3pa ~ 1.0 × 10
-2pa; In vacuum cavity, pass into argon gas again, sputter the vacuum tightness of vacuum cavity to 0.5Pa ~ 2Pa by mass flowmeter adjustment; Start sputtering, sputtering power is adjusted to 80W ~ 120W; After aura is stable, remove baffle plate, start deposited oxide zinc-aluminium film, depositing time is 40min ~ 60min, deposits complete taking-up zinc oxide aluminum film sample.
2. the method for the hydrogeneous zinc oxide aluminum transparent electroconductive film of preparation according to claim 1, it is characterized in that, using described water vapour as reactant gases, under the dual function of plasma body and underlayer temperature, water vapour decomposes generation atomic oxygen and atomic hydrogen, atomic oxygen provides Sauerstoffatom for zinc oxide aluminum transparent conducting film is formed, and atomic hydrogen forms shallow donor in zinc oxide aluminum film.
3. the method for the hydrogeneous zinc oxide aluminum transparent electroconductive film of preparation according to claim 1, is characterized in that, described ceramic target purity is 99.99%, Al
2o
3weight percent content be 3%, target-substrate distance is 110mm, and prepared zinc oxide aluminum film thickness is 800nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410740483.9A CN104480442A (en) | 2014-12-05 | 2014-12-05 | Method for preparing transparent conductive film containing aluminum zinc hydroxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410740483.9A CN104480442A (en) | 2014-12-05 | 2014-12-05 | Method for preparing transparent conductive film containing aluminum zinc hydroxide |
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| CN104480442A true CN104480442A (en) | 2015-04-01 |
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| CN201410740483.9A Pending CN104480442A (en) | 2014-12-05 | 2014-12-05 | Method for preparing transparent conductive film containing aluminum zinc hydroxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI686489B (en) * | 2016-06-23 | 2020-03-01 | 日商愛發科股份有限公司 | Stress adjustment method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08134638A (en) * | 1994-11-04 | 1996-05-28 | Asahi Glass Co Ltd | Formation of titanium oxide film |
| JP2002363732A (en) * | 2001-03-15 | 2002-12-18 | Asahi Glass Co Ltd | Transparent conductive film manufacturing method, and transparent substrate having transparent conductive film |
| JP2004059964A (en) * | 2002-07-25 | 2004-02-26 | Matsushita Electric Ind Co Ltd | Transparent conductive film and method for manufacturing the same |
| CN103526169A (en) * | 2013-09-23 | 2014-01-22 | 中国科学院电工研究所 | Preparation method of aluminum-doped zinc oxide (AZO) transparent conducting film |
| CN103757594A (en) * | 2014-01-10 | 2014-04-30 | 深圳大学 | Method for preparing high-performance AZO transparent electro-conductive film on flexible substrate at room temperature |
-
2014
- 2014-12-05 CN CN201410740483.9A patent/CN104480442A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08134638A (en) * | 1994-11-04 | 1996-05-28 | Asahi Glass Co Ltd | Formation of titanium oxide film |
| JP2002363732A (en) * | 2001-03-15 | 2002-12-18 | Asahi Glass Co Ltd | Transparent conductive film manufacturing method, and transparent substrate having transparent conductive film |
| JP2004059964A (en) * | 2002-07-25 | 2004-02-26 | Matsushita Electric Ind Co Ltd | Transparent conductive film and method for manufacturing the same |
| CN103526169A (en) * | 2013-09-23 | 2014-01-22 | 中国科学院电工研究所 | Preparation method of aluminum-doped zinc oxide (AZO) transparent conducting film |
| CN103757594A (en) * | 2014-01-10 | 2014-04-30 | 深圳大学 | Method for preparing high-performance AZO transparent electro-conductive film on flexible substrate at room temperature |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI686489B (en) * | 2016-06-23 | 2020-03-01 | 日商愛發科股份有限公司 | Stress adjustment method |
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Application publication date: 20150401 |