CN102134704A - Preparation method of multilayer transparent conductive film, film prepared thereby, and application thereof - Google Patents
Preparation method of multilayer transparent conductive film, film prepared thereby, and application thereof Download PDFInfo
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- CN102134704A CN102134704A CN201110044945XA CN201110044945A CN102134704A CN 102134704 A CN102134704 A CN 102134704A CN 201110044945X A CN201110044945X A CN 201110044945XA CN 201110044945 A CN201110044945 A CN 201110044945A CN 102134704 A CN102134704 A CN 102134704A
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Abstract
The invention relates to the preparation field of semiconductor material, and provides a preparation method of a multilayer transparent conductive film, the film prepared thereby, and the application thereof. The preparation method comprises the steps of: mixing Ga2O3 powder and ZnO powder, sintering the mixture and taking the product as GZO target material, wherein the mass ratio between the Ga2O3 powder and ZnO powder is 1/99-1/19; providing Cu target material; putting the GZO target material and the Cu target material into a magnetron sputtering cavity; vacuumizing and alternately sputtering a GZO layer and a Cu layer on a substrate; and finally obtaining the GZO-Cu-GZO transparent conductive film with a sandwich structure. The invention also provides the multilayer transparent conductive film prepared by the method, and the application of the film in a semiconductor photoelectric device.
Description
Technical field
The invention belongs to the photoelectric semiconductor material preparation field, be specifically related to a kind of preparation method of multi-layer transparent electroconductive film and the film and the application of preparation thereof.
Background technology
Transparent conductive film is the photoelectric material that optical clear performance and conductivity is compounded in one, because it has excellent photoelectric characteristic, becomes hot research in recent years and advanced subject, can be widely used in solar cell, LED, TFT, screen display fields such as LCD and touch-screen.A kind of transparent conductive film material that though ito thin film is present comprehensive photoelectric properties excellence, be most widely used, but indium is poisonous, cost an arm and a leg, poor stability, problem such as be reduced in hydrogen plasma atmosphere easily, people try hard to seek a kind of ITO replacement material of cheap and excellent performance.Wherein, gallium-doped zinc oxide (Ga-doped ZnO, be called for short GZO film) has the material cheapness, and is nontoxic, can become the most competitive transparent conductive film material with characteristics such as comparable electricity of ITO and optical properties.
Adopt magnetically controlled sputter method to prepare the GZO film, have the sedimentation rate height, the film tack is good, easy to control and can realizes advantage such as big area deposition, thus become in the current suitability for industrialized production research at most, a ripe and the most most widely used method of technology.But low temperature is preparation down, and heat treated not is difficult to obtain the GZO film of low-resistivity.
Ultra-thin conductive metal layer also can be used as nesa coating, but at present applicablely has only gold and silver and platinum constant resistance rate is low and chemical stability is good precious metal, and the cost costliness has limited its application.
Summary of the invention
Based on above problem, the embodiment of the invention provides a kind of preparation method of multi-layer transparent electroconductive film and the film and the application of preparation thereof.
The embodiment of the invention is achieved in that first aspect provides a kind of preparation method of multi-layer transparent electroconductive film, and it comprises the steps:
With Ga
2O
3Powder and ZnO powder mix, and sintering is as the GZO target, described Ga
2O
3The mass ratio of powder and described ZnO powder is 1/99～1/19;
Cu is provided target;
Described GZO target and described Cu target are packed in the magnetron sputtering cavity, and alternately sputter GZO layer and Cu layer on substrate obtain the GZO-Cu-GZO transparent conductive film of sandwich structure.
The transparent conductive film that another purpose of the embodiment of the invention is to provide the preparation method of above-mentioned multi-layer transparent electroconductive film to obtain, described multi-layer transparent electroconductive film comprises a GZO layer, Cu layer and the 2nd GZO layer, the thickness of a described GZO layer is 20nm～120nm, the thickness of Cu layer is 3nm～20nm, and the thickness of the 2nd GZO layer is 30nm～150nm.。
Another purpose of the embodiment of the invention is to provide the application of transparent conductive film in semiconductor photoelectric device of preparation method's acquisition of adopting above-mentioned multi-layer transparent electroconductive film.
The embodiment of the invention is a target with GZO and Cu, adopts magnetron sputtering method, and alternating sputtering obtains multi-layer transparent electroconductive film, and it has the sedimentation rate height, underlayer temperature is relatively low, the film tack is good, easy to control and can realize advantage such as big area deposition.In addition, the GZO-Cu-GZO of sandwich structure, intermediary copper layer plays electric action, and the oxide skin at two ends not only has certain conductive capability, and can play effect anti-reflection and the super thin copper layer of protection.Further, be intermediate conductive layer with copper, can reach the low resistance of integral multi-layered transparent conductive film, reduce cost simultaneously.
Description of drawings
Fig. 1 is preparation method's the schema of the multi-layer transparent electroconductive film of the embodiment of the invention;
Fig. 2 is a Cu layer thickness and the transmittance under ultraviolet-visible light and the change curve of square resistance in the multi-layer transparent electroconductive film of the embodiment of the invention 1～4;
Fig. 3 is the transmitted light spectrogram of the embodiment of the invention 1 multi-layer transparent electroconductive film under ultraviolet-visible light.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer,, the present invention is described in further detail below in conjunction with drawings and Examples.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
See also Fig. 1, the preparation method of a kind of multi-layer transparent electroconductive film of the embodiment of the invention is shown, it comprises the steps:
S01: with Ga
2O
3Powder and ZnO powder mix, and sintering is as the GZO target, described Ga
2O
3The mass ratio of powder and described ZnO powder is 1/99～1/19;
S02: Cu is provided target;
S03: described GZO target and described Cu target are packed in the magnetron sputtering cavity, vacuumize, alternately sputter GZO layer and Cu layer on substrate obtain the GZO-Cu-GZO transparent conductive film of sandwich structure.
Among the step S01, with Ga
2O
3Powder and ZnO powder mix, and for example at 900 ℃～1350 ℃ sintering temperatures, obtain the GZO ceramic target.Preferably, Ga
2O
3The mass ratio of powder and ZnO powder is 1/80～1/40, more preferably, and Ga
2O
3The mass ratio of powder and ZnO powder is 1/70～1/60.In a preferred embodiment of the invention, the GZO target is selected Ga for use
2O
3The mass ratio of powder and ZnO powder is 1/66.
Among the step S02, the Cu target can be any commercially available or self-control target, and in a preferred embodiment of the invention, the purity of Cu is 99.999% in the Cu target.
Among the step S03, the GZO-Cu-GZO transparent conductive film of sandwich structure is made up of two-layer GZO layer sandwich Cu layer.Substrate can be substrates commonly used such as quartz substrate, Sapphire Substrate.Use acetone, dehydrated alcohol and deionized water supersound washing before using, and dry up with high pure nitrogen.The distance of target and substrate is preferably 60mm～90mm.Target vacuumizes after packing in the sputter cavity, with mechanical pump or molecular pump the vacuum tightness of cavity is evacuated to 1.0 * 10
-3Pa～1.0 * 10
-5More than the Pa, be preferably 6.0 * 10
-4Pa.For the GZO-Cu-GZO transparent conductive film of sandwich structure, intermediary copper layer plays electric action, and the oxide skin at two ends plays a part anti-reflection and the super thin copper layer of protection, obtain the multi-layer transparent electroconductive film of excellent performance, and processing condition are provided with extremely important.Processing parameter is: inert gas flow is 15sccm～35sccm, is preferably 20sccm, and operating pressure is 0.2Pa～2.0Pa, is preferably 1.0Pa, and the sputtering power of GZO layer is 60W～160W, and the sputtering power of Cu layer is 30W～100W.More preferably, the sputtering power of described GZO layer is 90W～110W, and the sputtering power of described Cu layer is 50W～70W.The thickness of the GZO-Cu-GZO transparent conductive film of sandwich structure is extremely important.The GZO layer thickness is too big, can cause too high in resistance, but the blocked up transmittance that then can cause of Cu descends.Therefore, the transparent conductive film that obtains excellent performance need limit the thickness of each layer.Preferably, wherein a GZO layer is 20nm～120nm, more preferably, is 40nm～60nm, the thickness of Cu layer is 3nm～20nm, more preferably, the Cu layer thickness is 9nm～11nm, and the Cu layer is thin excessively, it is very poor that electroconductibility can become, the thickness of the 2nd GZO layer is 30nm～150nm, and more preferably, the thickness of GZO layer is 70nm～90nm.
The embodiment of the invention also provides a kind of film that adopts preparation method's preparation of described multi-layer transparent electroconductive film, multi-layer transparent electroconductive film comprises a GZO layer, Cu layer and the 2nd GZO layer, wherein the thickness of a GZO layer is 20nm～120nm, the thickness of Cu layer is 3nm～20nm, and the thickness of the 2nd GZO layer is 30nm～150nm.。
And adopt described method in the application of preparation in the semiconductor photoelectric device, mainly be application in the transparency electrode of transparent heating unit, antistatic, electromagnetic wave proof film, sun power.
The preparation method of the multilayer conductive film that the embodiment of the invention provides adopts magnetron sputtering method, alternating sputtering, the restriction bed thickness, the GZO-Cu-GZO transparent conductive film of preparation sandwich structure has been realized the at utmost reduction of sheet resistance, remains on the high permeability of visible region simultaneously.Cu has stable performance with respect to other metallic conduction materials, and cheap advantage selects suitable magnetron sputtering technique can obtain the transparent conductive film of the sandwich structure of excellent performance.
Below in conjunction with specific embodiment specific implementation of the present invention is described in detail:
Embodiment 1:
Select Ga for use
2O
3: ZnO=1: 66 (mass ratio) powder, through behind the uniform mixing, 1250 ℃ of high temperature sinterings become the ceramic target of Φ 60 * 2mm, and (Φ 50 * 3mm) packs in the vacuum cavity with Cu target customized.Then, successively use acetone, dehydrated alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up, put into vacuum cavity with high pure nitrogen.Is the distance setting of target and substrate 50mm.With mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 6.0 * 10
-4Pa, the argon gas of feeding 20sccm, pressure is adjusted to 1.0Pa.The sputtering power 100W of GZO target, the sputtering power 60W of Cu target.The GZO-Cu-GZO film threeply degree that obtains is respectively 50nm, 10nm, and 80nm, square resistance are 15 Ω/, the visible light average transmittances is 85%.
Embodiment 2:
Select Ga for use
2O
3: ZnO=1: 66 (mass ratio) powder, through behind the uniform mixing, 1250 ℃ of high temperature sinterings become the ceramic target of Φ 60 * 2mm, and (Φ 50 * 3mm) packs in the vacuum cavity with Cu target customized.Then, successively use acetone, dehydrated alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up, put into vacuum cavity with high pure nitrogen.Is the distance setting of target and substrate 50mm.With mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 6.0 * 10
-4Pa, the argon gas of feeding 20sccm, pressure is adjusted to 1.0Pa.The sputtering power 100W of GZO target, the sputtering power 60W of Cu target.The GZO-Cu-GZO film threeply degree that obtains is respectively 70nm, 5nm, and 80nm, square resistance are 300 Ω/, the visible light average transmittances is 92%.
Embodiment 3:
Select Ga for use
2O
3: ZnO=1: 66 (mass ratio) powder, through behind the uniform mixing, 1250 ℃ of high temperature sinterings become the ceramic target of Φ 60 * 2mm, and (Φ 50 * 3mm) packs in the vacuum cavity with Cu target customized.Then, successively use acetone, dehydrated alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up, put into vacuum cavity with high pure nitrogen.Is the distance setting of target and substrate 50mm.With mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 6.0 * 10
-4Pa, the argon gas of feeding 20sccm, pressure is adjusted to 1.0Pa.The sputtering power 100W of GZO target, the sputtering power 60W of Cu target.The GZO-Cu-GZO film threeply degree that obtains is respectively 70nm, 15nm, and 100nm, square resistance are 10 Ω/, the visible light average transmittances is 72%.
Embodiment 4:
Select Ga for use
2O
3: ZnO=1: 66 (mass ratio) powder, through behind the uniform mixing, 1250 ℃ of high temperature sinterings become the ceramic target of Φ 60 * 2mm, and (Φ 50 * 3mm) packs in the vacuum cavity with Cu target customized.Then, successively use acetone, dehydrated alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up, put into vacuum cavity with high pure nitrogen.Is the distance setting of target and substrate 50mm.With mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 6.0 * 10
-4Pa, the argon gas of feeding 20sccm, pressure is adjusted to 1.0Pa.The sputtering power 100W of GZO target, the sputtering power 60W of Cu target.The GZO-Cu-GZO film threeply degree that obtains is respectively 80nm, 20nm, and 50nm, square resistance are 5 Ω/, the visible light average transmittances is 60%.
Embodiment 5:
Select Ga for use
2O
3: ZnO=1: 99 (mass ratio) powder, through behind the uniform mixing, 1200 ℃ of high temperature sinterings become the ceramic target of Φ 60 * 2mm, and (Φ 50 * 3mm) packs in the vacuum cavity with Cu target customized.Then, successively use acetone, dehydrated alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up, put into vacuum cavity with high pure nitrogen.Is the distance setting of target and substrate 60mm.With mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 6.0 * 10
-4Pa, the argon gas of feeding 25sccm, pressure is adjusted to 1.2Pa.The sputtering power 120W of GZO target, the sputtering power 50W of Cu target.The GZO-Cu-GZO film threeply degree that obtains is respectively 120nm, 3nm, and 30nm, square resistance are 305 Ω/, the visible light average transmittances is 75%.
Embodiment 6:
Select Ga for use
2O
3: ZnO=1: 80 (mass ratio) powder, through behind the uniform mixing, 900 ℃ of high temperature sinterings become the ceramic target of Φ 60 * 2mm, and (Φ 60 * 3mm) packs in the vacuum cavity with Cu target customized.Then, successively use acetone, dehydrated alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up, put into vacuum cavity with high pure nitrogen.Is the distance setting of target and substrate 50mm.With mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 7.0 * 10
-4Pa, the argon gas of feeding 30sccm, pressure is adjusted to 1.2Pa.The sputtering power 120W of GZO target, the sputtering power 50W of Cu target.The GZO-Cu-GZO film threeply degree that obtains is respectively 20nm, 8nm, and 90nm, square resistance are 20 Ω/, the visible light average transmittances is 90%.
Embodiment 7:
Select Ga for use
2O
3: ZnO=1: 40 (mass ratio) powder, through behind the uniform mixing, 900 ℃ of high temperature sinterings become the ceramic target of Φ 60 * 2mm, and (Φ 60 * 3mm) packs in the vacuum cavity with Cu target customized.Then, successively use acetone, dehydrated alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up, put into vacuum cavity with high pure nitrogen.Is the distance setting of target and substrate 50mm.With mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 7.0 * 10
-4Pa, the argon gas of feeding 30sccm, pressure is adjusted to 1.2Pa.The sputtering power 120W of GZO target, the sputtering power 50W of Cu target.The GZO-Cu-GZO film threeply degree that obtains is respectively 40nm, 11nm, and 90nm, square resistance are 16 Ω/, the visible light average transmittances is 84%.
Embodiment 8:
Select Ga for use
2O
3: ZnO=1: 19 (mass ratio) powder, through behind the uniform mixing, 900 ℃ of high temperature sinterings become the ceramic target of Φ 60 * 2mm, and (Φ 60 * 3mm) packs in the vacuum cavity with Cu target customized.Then, successively use acetone, dehydrated alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up, put into vacuum cavity with high pure nitrogen.Is the distance setting of target and substrate 50mm.With mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 7.0 * 10
-4Pa, the argon gas of feeding 30sccm, pressure is adjusted to 1.2Pa.The sputtering power 120W of GZO target, the sputtering power 50W of Cu target.The GZO-Cu-GZO film threeply degree that obtains is respectively 60nm, 20nm, and 100nm, square resistance are 6 Ω/, the visible light average transmittances is 60%.
Fig. 2 is a Cu layer thickness and the transmittance under ultraviolet-visible light and the change curve of square resistance in the multi-layer transparent electroconductive film of the embodiment of the invention 1～4 preparation.Along with the increase of Cu layer thickness, the average transmittances of visible region reduces, and resistance also reduces.Fig. 3 is the transmitted spectrum of the multi-layer transparent electroconductive film sample of the embodiment of the invention 1 preparation, can draw from figure, and its visible light transmittance rate can reach 85%, and the square resistance of this sample is 15 Ω/ (Fig. 2), near the performance of commercial ITO.
The above only is preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of being done within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a multi-layer transparent electroconductive film is characterized in that, described method comprises the steps:
With Ga
2O
3Powder and ZnO powder mix, and sintering is as the GZO target, described Ga
2O
3The mass ratio of powder and described ZnO powder is 1/99～1/19;
Cu is provided target;
Described GZO target and described Cu target are packed in the magnetron sputtering cavity, and alternately sputter GZO layer and Cu layer on substrate obtain the GZO-Cu-GZO transparent conductive film of sandwich structure.
2. the preparation method of multi-layer transparent electroconductive film as claimed in claim 1 is characterized in that, described Ga
2O
3The mass ratio of powder and described ZnO powder is 1/80～1/40.
3. the preparation method of multi-layer transparent electroconductive film as claimed in claim 2 is characterized in that, described Ga
2O
3The mass ratio of powder and described ZnO powder is 1/70～1/60.
4. the preparation method of multi-layer transparent electroconductive film as claimed in claim 1 is characterized in that, the sputtering power of described GZO layer is 60W～160W, and the sputtering power of described Cu layer is 30W～100W.
5. the preparation method of multi-layer transparent electroconductive film as claimed in claim 1 is characterized in that, the sputtering power 90W～110W of described GZO layer, the sputtering power 50W～70W of described Cu layer.
6. select the preparation method of a described multi-layer transparent electroconductive film as claim 1 to 5, it is characterized in that, the process of described sputter is carried out under atmosphere of inert gases, and described inert gas flow is 15sccm～35sccm, and the operating pressure of described cavity is 0.2Pa～2.0Pa.
7. the multi-layer transparent electroconductive film that makes as the preparation method of the arbitrary described multi-layer transparent electroconductive film of claim 1～6, it is characterized in that, described multi-layer transparent electroconductive film comprises a GZO layer, Cu layer and the 2nd GZO layer, the thickness of a described GZO layer is 20nm～120nm, the thickness of Cu layer is 3nm～20nm, and the thickness of the 2nd GZO layer is 30nm～150nm.
8. multi-layer transparent electroconductive film as claimed in claim 7 is characterized in that, the thickness of a described GZO layer is 40nm～60nm, and the thickness of Cu layer is 9nm～11nm, and the thickness of the 2nd GZO layer is 70nm～90nm.
9. multi-layer transparent electroconductive film as claimed in claim 8 is characterized in that, the thickness of a described GZO layer is 50nm, and the thickness of Cu layer is 10nm, and the thickness of the 2nd GZO layer is 80nm.
10. as the application of the arbitrary described multi-layer transparent electroconductive film of claim 7～9 in semiconductor photoelectric device.
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Cited By (4)
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| CN102747334A (en) * | 2012-07-30 | 2012-10-24 | 中国科学院宁波材料技术与工程研究所 | Zinc-oxide-based transparent conductive film and preparation method thereof |
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| CN104894520A (en) * | 2015-05-06 | 2015-09-09 | 大连理工大学 | Metal Mg-based UVC wave band transparent conducting structure and preparation method thereof |
| CN106756799A (en) * | 2016-12-19 | 2017-05-31 | 长沙理工大学 | A kind of method for improving ZnO transparent conductive thin film adhesive force |
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2011
- 2011-02-24 CN CN201110044945XA patent/CN102134704A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103422053A (en) * | 2012-05-14 | 2013-12-04 | 海洋王照明科技股份有限公司 | Conductive film, and preparation method and applications thereof |
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| CN104894520A (en) * | 2015-05-06 | 2015-09-09 | 大连理工大学 | Metal Mg-based UVC wave band transparent conducting structure and preparation method thereof |
| CN106756799A (en) * | 2016-12-19 | 2017-05-31 | 长沙理工大学 | A kind of method for improving ZnO transparent conductive thin film adhesive force |
| CN106756799B (en) * | 2016-12-19 | 2020-10-16 | 长沙理工大学 | Method for improving adhesion of ZnO transparent conductive film |
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Application publication date: 20110727 |