CN102134699A - Preparation method of multilayer transparent conductive thin film as well as prepared thin film and application thereof - Google Patents
Preparation method of multilayer transparent conductive thin film as well as prepared thin film and application thereof Download PDFInfo
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Abstract
The invention relates to the field of preparing semiconductor materials and provides a preparation method of a multilayer transparent conductive thin film as well as a prepared thin film and an application thereof. The method comprises the following steps: mixing SiO2 powder with ZnO powder and sintering to serve as an SZO target, wherein the mass ratio of the SiO2 powder to the ZnO powder is 2/199-1/6; providing an Ag target; and putting the SZO target and the Ag target into a magnetic-control sputtering cavity, orderly sputtering a first SZO layer, an Ag layer and a second SZO layer on a substrate so as to obtain an SZO-Ag-SZO transparent conductive thin film which is of a sandwich structure. The invention also provides the multilayer transparent conductive thin film obtained by using the method and the application of the film in semiconductor photoelectric devices.
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, advantage such as zinc oxide has the material cheapness, and is nontoxic, and band gap is wide becomes material commonly used.Have the material cheapness and mix silicon oxidation zinc (Si-doped ZnO, be called for short SZO film), 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 SZO 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 having the SZO film of low-resistivity.
Ultra-thin conductive metal layer also can be used as nesa coating, but its thickness is difficult to control, and light transmission is poor, is easy to external environment and reacts, and 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 SiO
2Powder and ZnO powder mix, and sintering is as the SZO target, described SiO
2The mass ratio of powder and described ZnO powder is 2/199～1/6;
Ag is provided target;
Described SZO target and described Ag target are packed in the magnetron sputtering cavity, and sputter the one SZO layer, Ag layer and the 2nd SZO layer on substrate successively obtain the SZO-Ag-SZO 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 SZO layer, Ag layer and the 2nd SZO layer, wherein, the thickness of the one SZO layer is 40nm～100nm, the thickness of Ag layer is 3nm～15nm, and the thickness of the 2nd SZO layer is 30nm～120nm.
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 SZO and Ag, 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 SZO-Ag-SZO of sandwich structure; the intermediary silver layer plays electric action; the oxide skin at two ends not only has certain conductive capability; and can play effect anti-reflection and the ultra-thin silver layer of protection, and the SZO material price is cheap, the thin film stability height of formation; the surface work function height helps improving the luminous efficiency of device.Further, be intermediate conductive layer with silver, can reach the low resistance of integral multi-layered transparent conductive film.
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 an Ag 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 1～6;
Fig. 3 is the transmitted light spectrogram of multi-layer transparent electroconductive film under ultraviolet-visible light of the embodiment of the invention 1.
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 SiO
2Powder and ZnO powder mix, and sintering is as the SZO target, described SiO
2The mass ratio of powder and described ZnO powder is 2/199～1/6;
S02: Ag is provided target;
S03: described SZO target and described Ag target are packed in the magnetron sputtering cavity, and sputter the one SZO layer, Ag layer and the 2nd SZO layer on substrate successively obtain the SZO-Ag-SZO transparent conductive film of sandwich structure.
Among the step S01, with SiO
2Powder and ZnO powder mix, and for example at 900 ℃～1350 ℃ sintering temperatures, obtain the SZO ceramic target.Preferably, SiO
2The mass ratio of powder and ZnO powder is 1/70～1/20, more preferably, and SiO
2The mass ratio of powder and ZnO powder is 1/50～1/30.In a preferred embodiment of the invention, the SZO target is selected SiO for use
2The mass ratio of powder and ZnO powder is 1/49.
Among the step S02, the Ag target can be any commercially available or self-control target, and in a preferred embodiment of the invention, the purity of Ag is 99.999% in the Ag target.
Among the step S03, the SZO-Ag-SZO transparent conductive film of sandwich structure is made up of two-layer SZO layer sandwich Ag layer.Substrate can be quartz substrate or organic flexible substrate.Organic flexible substrate comprises: polyethylene terephthalate (PET), polycarbonate (PC), PEN (PEN), polyethersulfone (PES) or the like.It is good that flexible substrate has snappiness, low cost and other advantages, but because its planarization is poor, and fusing point is low, the preparation technology of a lot of transparent conductive films should not select flexible 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 40mm～80mm.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 SZO-Ag-SZO transparent conductive film of sandwich structure, the intermediary silver layer plays electric action, and the oxide skin at two ends plays a part anti-reflection and the ultra-thin silver 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 10sccm～30sccm, be preferably 15sccm, operating pressure is 0.5Pa～5.0Pa, is preferably 1.7Pa, and the SZO-AG-SZO of sandwich structure is in sputter procedure, the power of the one SZO layer of close substrate is 30W～100W, be preferably 15W～25W, the sputtering power of Ag layer is 30W～100W, is preferably 50W～70W, the sputtering power of the 2nd SZO layer is 60W～160W, is preferably 90W～110W.The less sputtering power of the one SZO layer employing can reduce the damage to flexible substrate.The thickness of the SZO-Ag-SZO transparent conductive film of sandwich structure is extremely important.The SZO layer thickness is too big, can cause too high in resistance, but the blocked up transmittance that then can cause of Ag descends.Therefore, the transparent conductive film that obtains excellent performance need limit the thickness of each layer.Preferably, wherein a SZO layer is 40nm～100nm, more preferably, is 50nm～70nm, the thickness of Ag layer is 3nm～20nm, more preferably, the Ag layer thickness is 12nm～15nm, and the Ag layer is thin excessively, resistance is too high relatively, the thickness of the 2nd SZO layer is 30nm～120nm, and more preferably, the thickness of SZO layer is 50nm～70nm.
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 SZO layer, Ag layer and the 2nd SZO layer, wherein the thickness of a SZO layer is 40nm～100nm, the thickness of Ag layer is 3nm～20nm, and the thickness of the 2nd SZO layer is 30nm～120nm.
And the application of multi-layer transparent electroconductive film in the preparation semiconductor photoelectric device of adopting the preparation of described method, mainly be application in the transparency electrode of electroluminescent device, 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 SZO-Ag-SZO 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.SZO is with respect to other semiconductor materials, because silicon doping stability is better, and the silicon raw material is abundant relatively cheap, and advantage is more obvious in semiconductor photoelectric device, 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 SiO for use
2: ZnO=1: 49 (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 the Ag target.Then, successively use dehydrated alcohol and deionized water ultrasonic cleaning PET 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 20W of the one SZO layer, the sputtering power 60W of Ag target, the sputtering power of the 2nd SZO layer are 100W.The SZO-Ag-SZO film threeply degree that obtains is respectively 60nm, 15nm, and 60nm, square resistance are 8 Ω/, the visible light average transmittances is 90%.
Embodiment 2:
Select SiO for use
2: ZnO=1: 49 (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 the Ag target.Then, successively use dehydrated alcohol and deionized water ultrasonic cleaning PET 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 20W of the one SZO layer, the sputtering power 60W of Ag target, the sputtering power of the 2nd SZO layer are 100W.The SZO-Ag-SZO film threeply degree that obtains is respectively 75nm, 5nm, and 75nm, square resistance are 450 Ω/, the visible light average transmittances is 93%.
Embodiment 3:
Select SiO for use
2: ZnO=1: 49 (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 the Ag target.Then, successively use dehydrated alcohol and deionized water ultrasonic cleaning PET 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 20W of the one SZO layer, the sputtering power 60W of Ag target, the sputtering power of the 2nd SZO layer are 100W.The SZO-Ag-SZO film threeply degree that obtains is respectively 80nm, 12nm, and 100nm, square resistance are 50 Ω/, the visible light average transmittances is 70%.
Embodiment 4:
Select SiO for use
2: ZnO=1: 49 (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 the Ag target.Then, successively use dehydrated alcohol and deionized water ultrasonic cleaning PET 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 20W of the one SZO layer, the sputtering power 60W of Ag target, the sputtering power of the 2nd SZO layer are 100W.The SZO-Ag-SZO film threeply degree that obtains is respectively 80nm, 35nm, and 80nm, square resistance are 7 Ω/, the visible light average transmittances is 75%.
Embodiment 5:
Select SiO for use
2: ZnO=1: 49 (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 the Ag target.Then, successively use dehydrated alcohol and deionized water ultrasonic cleaning PET 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 20W of the one SZO layer, the sputtering power 60W of Ag target, the sputtering power of the 2nd SZO layer are 100W.The SZO-Ag-SZO film threeply degree that obtains is respectively 100nm, 25nm, and 150nm, square resistance are 8 Ω/, the visible light average transmittances is 70%.
Embodiment 6:
Select SiO for use
2: ZnO=1: 70 (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 the Ag target.Then, successively use dehydrated alcohol and deionized water ultrasonic cleaning PET 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 10sccm, pressure is adjusted to 0.5Pa.The sputtering power 10W of the one SZO layer, the sputtering power 30W of Ag target, the sputtering power of the 2nd SZO layer are 60W.The SZO-Ag-SZO film threeply degree that obtains is respectively 40nm, 3nm, and 30nm, square resistance are 860 Ω/, the visible light average transmittances is 95%.
Embodiment 7:
Select SiO for use
2: ZnO=1: 50 (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 the Ag target.Then, successively use dehydrated alcohol and deionized water ultrasonic cleaning PET 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 30sccm, pressure is adjusted to 5.0Pa.The sputtering power 40W of the one SZO layer, the sputtering power 100W of Ag target, the sputtering power of the 2nd SZO layer are 160W.The SZO-Ag-SZO film threeply degree that obtains is respectively 100nm, 10nm, and 120nm, square resistance are 80 Ω/, the visible light average transmittances is 89%.
Embodiment 8:
Select SiO for use
2: ZnO=1: 30 (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 the Ag target.Then, successively use dehydrated alcohol and deionized water ultrasonic cleaning PET 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 15sccm, pressure is adjusted to 2.0Pa.The sputtering power 30W of the one SZO layer, the sputtering power 40W of Ag target, the sputtering power of the 2nd SZO layer are 60W.The SZO-Ag-SZO film threeply degree that obtains is respectively 60nm, 15nm, and 60nm, square resistance are 15 Ω/, the visible light average transmittances is 80%.
Embodiment 9:
Select SiO for use
2: ZnO=1: 20 (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 the Ag target.Then, successively use dehydrated alcohol and deionized water ultrasonic cleaning PET 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 4.0Pa.The sputtering power 25W of the one SZO layer, the sputtering power 50W of Ag target, the sputtering power of the 2nd SZO layer are 50W.The SZO-Ag-SZO film threeply degree that obtains is respectively 60nm, 45nm, and 60nm, square resistance are 10 Ω/, the visible light average transmittances is 60%.
Fig. 2 is an Ag 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 1～5 preparation.Along with the increase of Ag layer thickness, the average transmittances of visible region reduces, and occurs a less rising trend again when being increased to 25nm～35nm place, for resistance, remains unchanged substantially during greater than 15nm in silver thickness.Fig. 3 is the transmitted spectrum of the multi-layer transparent electroconductive film sample of the embodiment of the invention 1 preparation, from figure, can draw, its visible light transmittance rate can reach 90%, and the square resistance of this sample is 8 Ω/ (Fig. 2), and its performance can compare favourably with the performance of commercial ito thin film.
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 SiO
2Powder and ZnO powder mix, and sintering is as the SZO target, described SiO
2The mass ratio of powder and described ZnO powder is 2/199～1/6;
Ag is provided target;
Described SZO target and described Ag target are packed in the magnetron sputtering cavity, and sputter the one SZO layer, Ag layer and the 2nd SZO layer on substrate successively obtain the SZO-Ag-SZO 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 SiO
2The mass ratio of powder and described ZnO powder is 1/70～1/20.
3. the preparation method of multi-layer transparent electroconductive film as claimed in claim 1 is characterized in that, described SiO
2The mass ratio of powder and described ZnO powder is 1/50～1/30.
4. the preparation method of multi-layer transparent electroconductive film as claimed in claim 1 is characterized in that, described substrate is organic flexible substrate.
5. the preparation method of multi-layer transparent electroconductive film as claimed in claim 1 is characterized in that, the sputtering power of a described SZO layer is 10W～40W, and the sputtering power of described Ag layer is 30W～100W, and the sputtering power of described the 2nd SZO layer is 60W～160W.
6. the preparation method of multi-layer transparent electroconductive film as claimed in claim 1 is characterized in that, the sputtering power of a described SZO layer is 15W～25W, and the sputtering power of described Ag layer is 50W～70W, and the sputtering power of described the 2nd SZO layer is 90W～110W.
7. select the preparation method of a described multi-layer transparent electroconductive film as claim 1 to 6, it is characterized in that, the process of described sputter is carried out under atmosphere of inert gases, and described inert gas flow is 10sccm～30sccm, and the operating pressure of described cavity is 0.5Pa～5.0Pa.
8. as the multi-layer transparent electroconductive film of the preparation method of the arbitrary described multi-layer transparent electroconductive film of claim 1～7 preparation, it is characterized in that, the thickness of a described SZO layer is 40nm～100nm, and the thickness of Ag layer is 3nm～45nm, and the thickness of the 2nd SZO layer is 30nm～150nm.
9. multi-layer transparent electroconductive film as claimed in claim 8 is characterized in that, the thickness of a described SZO layer is 50nm～70nm, and the thickness of Ag layer is 12～15nm, and the thickness of the 2nd SZO layer is 50nm～70nm.
10. the application of multi-layer transparent electroconductive film in semiconductor photoelectric device as claimed in claim 8 or 9.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102677012A (en) * | 2012-05-18 | 2012-09-19 | 中国科学院上海光学精密机械研究所 | Preparation method of multi-layer transparent conductive film |
| CN104834397A (en) * | 2014-02-07 | 2015-08-12 | 胜华科技股份有限公司 | Touch control device |
| CN105932172A (en) * | 2016-05-11 | 2016-09-07 | 吉林大学 | Transparent lamination electrode with quantifiably adjusting work function and preparation technology thereof |
| CN109371378A (en) * | 2018-12-20 | 2019-02-22 | 五邑大学 | A method of improving transparent conductive oxide film work function |
| CN112885503A (en) * | 2021-01-12 | 2021-06-01 | 南开大学 | Preparation method and application of ultrathin silver-based OMO (organic molybdenum oxide) composite transparent conductive film |
-
2011
- 2011-02-24 CN CN2011100447454A patent/CN102134699A/en active Pending
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| D.R.SAHU，ET AL.: "High quality transparent conductive ZnO/Ag/ZnO multilayer films deposited at room temperature", 《THIN SOLID FILMS》 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102677012A (en) * | 2012-05-18 | 2012-09-19 | 中国科学院上海光学精密机械研究所 | Preparation method of multi-layer transparent conductive film |
| CN104834397A (en) * | 2014-02-07 | 2015-08-12 | 胜华科技股份有限公司 | Touch control device |
| CN105932172A (en) * | 2016-05-11 | 2016-09-07 | 吉林大学 | Transparent lamination electrode with quantifiably adjusting work function and preparation technology thereof |
| CN109371378A (en) * | 2018-12-20 | 2019-02-22 | 五邑大学 | A method of improving transparent conductive oxide film work function |
| CN112885503A (en) * | 2021-01-12 | 2021-06-01 | 南开大学 | Preparation method and application of ultrathin silver-based OMO (organic molybdenum oxide) composite transparent conductive film |
| CN112885503B (en) * | 2021-01-12 | 2022-06-21 | 南开大学 | Preparation method and application of ultrathin silver-based OMO (organic molybdenum oxide) composite transparent conductive film |
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Application publication date: 20110727 |