CN101697289A - Transparent conducting film and preparation method thereof - Google Patents
Transparent conducting film and preparation method thereof Download PDFInfo
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- CN101697289A CN101697289A CN200910152788A CN200910152788A CN101697289A CN 101697289 A CN101697289 A CN 101697289A CN 200910152788 A CN200910152788 A CN 200910152788A CN 200910152788 A CN200910152788 A CN 200910152788A CN 101697289 A CN101697289 A CN 101697289A
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Abstract
The invention discloses a transparent conducting film. A first Ga-doped n type ZnO thin film, a metal layer and a second Ga-doped n type ZnO thin film are orderly deposited on an organic polymer substrate. The transparent conducting film is prepared by a magnetron sputtering method which is simple. The transparent conducting film of the invention is good in electric performance, has a square resistance of 2 to 5 Omega/sq and the advantages of light weight, foldability, non-fragility, easy large-area production, convenient transportation, low cost and the like, can be applied to the manufacture of a flexible luminous apparatus, a plastic liquid crystal display and a flexible substrate amorphous silicon solar cell and can be used as a transparent electromagnetic shield, a touch-sensitive covering layer and the like as well as a transparent thermal-insulation heat-preservation material for a vinyl house.
Description
Technical field
The present invention relates to a kind of nesa coating and preparation method thereof.
Background technology
In recent years, zinc oxide (ZnO) nesa coating has obtained very extensive studies.Zinc-oxide film has advantages such as abundant raw materials, nontoxic, the conductivity can improve film of mixing and stability for indium tin oxide (ITO).As a kind of important optoelectronic information material, the good photoelectric characteristic of zinc oxide transparent conducting film makes it be widely used in fields such as solar cell, LCD, hot mirrors.The nesa coating of sandwich construction deposits the first ZnO film layer, metal level and the second ZnO film layer successively on substrate at present, and first, second ZnO film layer of this nesa coating does not all mix, its resistance height, and electric property is relatively poor.
In order to obtain more excellent electric property, can carry out the doping of ZnO usually, mainly be the III major element.In all doped chemicals, Ga and Zn atomic radius are the most approaching, and the bond distance of Ga-O key and Zn-O key is more approaching, so behind the Ga atom replacement Zn atom, the ZnO distortion of lattice that causes is little, helps mixing of Ga, and compares with Al, and Ga is difficult for oxidation.So Ga is considered to the most promising doped chemical.
Oxide/metal/oxide multilayered structure on the basis that is not very remarkable reduction visible light transmissivity, can improve the electric property of single layer oxide greatly.The selection of metal level mainly contains Ag, Cu and Al, because the Ag cost is higher, and the easy oxidation of Al, so Cu is best selection.
Organic substrate nesa coating not only has the photoelectric characteristic of glass substrate nesa coating, and many distinct advantages are arranged.It can be used as the transparency electrode of collapsible LCD, non-crystal silicon solar cell, also can be used as Pasting formula vehicle glass frost protection film, on transparency electromagnetic wave shield and collapsible reflection heat mirror, also be widely used, provide a kind of new thinking for developing flexible full impregnated funerary objects spare.
Summary of the invention
The purpose of this invention is to provide good nesa coating of a kind of electric property and preparation method thereof.
Nesa coating of the present invention deposits the first ZnO film layer, metal level and the second ZnO film layer successively on substrate, it is characterized in that substrate is an organic polymer, and the first ZnO film layer and the second ZnO film layer are Ga doped n type ZnO film, and metal level is a copper.
Above-mentioned organic polymer can be polyethylene terephthalate (PET), poly-carbonic acid dead drunk (PC), polymethyl methacrylate (PMMA) or PEN (PEN).
The preparation method of nesa coating may further comprise the steps:
1) pure ZnO and the Ga of weighing
2O
3Powder, wherein the Ga molar content is 4%, with above-mentioned powder ball milling mix, compression moulding, then at 1200 ℃ of sintering temperatures, make the ZnO ceramic target of mixing Ga;
2) adopting radio-frequency magnetron sputter method, is target with the ZnO ceramic target of mixing Ga, deposition one deck Ga doped n type ZnO film on the organic polymer substrate, and sputtering condition: the distance between target and the substrate remains 4～6cm, and growth room's vacuum degree is evacuated to 3 * 10 at least
-3Pa, the growth room feeds pure argon and purity oxygen, and control pressure is 0.1～3.0Pa, Ar: O
2=1: 0～0: 1, sputtering power 100W～300W;
3) adopting dc reactive magnetron sputtering technique, is metal targets with pure Cu, in step 2) deposition Cu film on the Ga doped n type ZnO film that makes, sputtering condition: the distance between target and the substrate remains 4～6cm, and growth room's vacuum degree is evacuated to 3 * 10 at least
-3Pa, the growth room feeds pure argon, and control pressure is 0.5～3.0Pa, sputtering power 100W～200W;
4) with step 2) method, deposition one deck is mixed the n type ZnO film of Ga on the Cu layer.
The purity of above-mentioned pure argon is more than 99.99%, and the purity of purity oxygen is more than 99.99%.ZnO, Ga
2O
3The purity of powder and metal Cu piece is more than 99.99%.
The thickness of each layer of nesa coating can be decided by sedimentation time.
Advantage of the present invention is:
1) preparation method is simple, can at room temperature grow, nesa coating electric property excellence of the present invention, and square resistance is 2～5 Ω/sq.
2) sandwich construction nesa coating of the present invention, adopt flexible substrate, have light weight, collapsible, non-friable, be easy to large tracts of land production, be convenient to the transportation and low cost and other advantages, can be applicable to make flexible luminescent device, plastic liquid crystal display and flexible substrate non-crystal silicon solar cell, can be used as transparency electromagnetic wave shield and touch sensitive overlays etc., also can be used as transparent heat-insulated insulation material and be used for hot house.
Description of drawings
Fig. 1 is the transparent conductive film structure schematic diagram.
Embodiment
Further specify the present invention below in conjunction with accompanying drawing and instantiation.
With reference to Fig. 1, nesa coating of the present invention deposits the first ZnO film layer 2, metal level 3 and the second ZnO film layer 4 successively on substrate 1, and substrate is an organic polymer, and the first ZnO film layer and the second ZnO film layer are Ga doped n type ZnO film, and metal level is a copper.
Embodiment 1:
The preparation method of nesa coating may further comprise the steps:
The ZnO and the Ga of 1) weighing purity 99.99%
2O
3Powder, wherein the molar content of Ga is 4%.With load weighted ZnO and Ga
2O
3Powder is poured in the ball grinder that agate ball is housed, and ball milling is 24 hours on ball mill, and purpose is to allow evenly also refinement to a certain extent of powder.Then raw material is separated oven dry, add binding agent and grind compression moulding.The idiosome of moulding is put into sintering furnace, and row is plain through low temperature (400 ℃), makes the binding agent volatilization, is warming up to 1200 ℃ of sintering again 4 hours, obtains mixing the ZnO ceramic target of Ga.
2) the PC substrate is fixed on the sample tray after cleaning, puts into the reaction vacuum chamber.The ZnO ceramic target that to mix Ga is contained on the target frame, embeds then on the target head of magnetic control sputtering device.The distance of regulating substrate and target is 6cm, and baffle plate is placed between substrate and the target.Growth room's vacuum degree is evacuated to 3 * 10
-3Pa, the growth room feeds pure argon and purity oxygen, Ar: O
2=4: 1, control pressure is 0.14Pa, begins sputter at the power of 300W, and sputtering time is 10min, obtains the ZnO film of mixing Ga of the about 100nm of thickness.
3) take off the ZnO ceramic target of mixing Ga, pure Cu metallic target is contained on the target frame, embed then on the target head of magnetic control sputtering device.Distance between target and the substrate remains 6cm, and baffle plate is placed between substrate and the target.Growth room's vacuum degree is evacuated to 3 * 10
-3Pa, growth room feed pure argon, and control pressure is 1.0Pa, begin sputter at the power of 120W, and sputtering time is 12s, obtains the Cu layer that thickness is about 8nm.
4) take off pure Cu metallic target, change the ZnO ceramic target of mixing Ga, with step 2) method, the n type ZnO film of mixing Ga of growth one layer thickness about 100nm on the Cu layer.
All magnetron sputtering deposition processes are all at room temperature carried out.The square resistance of the nesa coating that this example makes is 4 Ω/sq, and average transmittance is higher than 70% in the visible region, and device flexible 120 ° and property retention are stable.
Embodiment 2:
Preparation process is with embodiment 1, and different is: substrate is PET, and the thickness that first, second layer mixed the ZnO film of Ga is 150nm, and the thickness of Cu layer is 12nm.When preparing first, second layer and mixing the ZnO film of Ga, Ar: O
2=5: 1.The square resistance of the nesa coating that this example makes is 2 Ω/sq, and average transmittance is higher than 60% in the visible region, and device flexible 90 ° and property retention are stable.
Claims (5)
1. nesa coating, on substrate (1), deposit the first ZnO film layer (2), metal level (3) and the second ZnO film layer (4) successively, it is characterized in that substrate is an organic polymer, the first ZnO film layer and the second ZnO film layer are Ga doped n type ZnO film, and metal level is a copper.
2. nesa coating according to claim 1 is characterized in that organic polymer is that polyethylene terephthalate, poly-carbonic acid are dead drunk, polymethyl methacrylate or PEN.
3. the preparation method of the described nesa coating of claim 1 is characterized in that may further comprise the steps:
1) pure ZnO and the Ga of weighing
2O
3Powder, wherein the Ga molar content is 4%, with above-mentioned powder ball milling mix, compression moulding, then at 1200 ℃ of sintering temperatures, make the ZnO ceramic target of mixing Ga;
2) adopting radio-frequency magnetron sputter method, is target with the ZnO ceramic target of mixing Ga, deposition one deck Ga doped n type ZnO film on the organic polymer substrate, and sputtering condition: the distance between target and the substrate remains 4～6cm, and growth room's vacuum degree is evacuated to 3 * 10 at least
-3Pa, the growth room feeds pure argon and purity oxygen, and control pressure is 0.1～3.0Pa, Ar: O
2=1: 0～0: 1, sputtering power 100W～300W;
3) adopting dc reactive magnetron sputtering technique, is metal targets with pure Cu, in step 2) deposition Cu film on the Ga doped n type ZnO film that makes, sputtering condition: the distance between target and the substrate remains 4～6cm, and growth room's vacuum degree is evacuated to 3 * 10 at least
-3Pa, the growth room feeds pure argon, and control pressure is 0.5～3.0Pa, sputtering power 100W～200W;
4) with step 2) method, deposition one deck is mixed the n type ZnO film of Ga on the Cu layer.
4. the preparation method of nesa coating according to claim 3, the purity that it is characterized in that pure argon is more than 99.99%, the purity of purity oxygen is more than 99.99%.
5. the preparation method of nesa coating according to claim 3 is characterized in that ZnO, Ga
2O
3The purity of powder and metal Cu piece is more than 99.99%.
Priority Applications (1)
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| CN200910152788A CN101697289A (en) | 2009-10-15 | 2009-10-15 | Transparent conducting film and preparation method thereof |
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| CN200910152788A CN101697289A (en) | 2009-10-15 | 2009-10-15 | Transparent conducting film and preparation method thereof |
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ID=42142389
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102097299A (en) * | 2010-11-16 | 2011-06-15 | 无锡中微晶园电子有限公司 | Saturated doping process of thick polycrystalline resistor |
| CN102174689A (en) * | 2011-04-01 | 2011-09-07 | 浙江大学 | FZO/metal/FZO transparent conductive film and preparation method thereof |
| CN102543266A (en) * | 2010-12-27 | 2012-07-04 | 迎辉科技股份有限公司 | Transparent conducting film with copper conductor |
| CN104991294A (en) * | 2015-06-18 | 2015-10-21 | 中国科学院国家天文台南京天文光学技术研究所 | Extremely-low temperature environment large-aperture reflecting-type telescope frost-prevention film system and preparing method thereof |
| CN105140311A (en) * | 2015-07-10 | 2015-12-09 | 福建铂阳精工设备有限公司 | Back electrode, manufacturing method thereof and battery assembly |
| CN105276656A (en) * | 2015-12-03 | 2016-01-27 | 安徽省蓝泰新材料有限公司 | Air-conditioning glass |
| CN105304732A (en) * | 2015-09-18 | 2016-02-03 | 河北曹妃甸汉能薄膜太阳能有限公司 | Transparent conductive oxide film preparation method and application thereof |
| CN108878058A (en) * | 2018-06-25 | 2018-11-23 | 湖北雄华科技有限公司 | Three-decker transparent conductive film and preparation method thereof for dimming glass |
| CN109671515A (en) * | 2017-10-17 | 2019-04-23 | 臻鼎科技股份有限公司 | The preparation method of flexible transparent electrode structure and the flexible transparent electrode structure |
| CN112334602A (en) * | 2018-07-05 | 2021-02-05 | 巴斯夫涂料有限公司 | Transparent conductive film |
-
2009
- 2009-10-15 CN CN200910152788A patent/CN101697289A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102097299A (en) * | 2010-11-16 | 2011-06-15 | 无锡中微晶园电子有限公司 | Saturated doping process of thick polycrystalline resistor |
| CN102097299B (en) * | 2010-11-16 | 2012-11-07 | 无锡中微晶园电子有限公司 | Saturated doping process of thick polycrystalline resistor |
| CN102543266A (en) * | 2010-12-27 | 2012-07-04 | 迎辉科技股份有限公司 | Transparent conducting film with copper conductor |
| CN102543266B (en) * | 2010-12-27 | 2014-04-02 | 迎辉科技股份有限公司 | Transparent conducting film with copper conductor |
| CN102174689A (en) * | 2011-04-01 | 2011-09-07 | 浙江大学 | FZO/metal/FZO transparent conductive film and preparation method thereof |
| CN104991294A (en) * | 2015-06-18 | 2015-10-21 | 中国科学院国家天文台南京天文光学技术研究所 | Extremely-low temperature environment large-aperture reflecting-type telescope frost-prevention film system and preparing method thereof |
| CN105140311A (en) * | 2015-07-10 | 2015-12-09 | 福建铂阳精工设备有限公司 | Back electrode, manufacturing method thereof and battery assembly |
| CN105140311B (en) * | 2015-07-10 | 2018-08-03 | 福建铂阳精工设备有限公司 | Back electrode and preparation method thereof and battery component |
| CN105304732A (en) * | 2015-09-18 | 2016-02-03 | 河北曹妃甸汉能薄膜太阳能有限公司 | Transparent conductive oxide film preparation method and application thereof |
| CN105276656A (en) * | 2015-12-03 | 2016-01-27 | 安徽省蓝泰新材料有限公司 | Air-conditioning glass |
| CN109671515A (en) * | 2017-10-17 | 2019-04-23 | 臻鼎科技股份有限公司 | The preparation method of flexible transparent electrode structure and the flexible transparent electrode structure |
| CN108878058A (en) * | 2018-06-25 | 2018-11-23 | 湖北雄华科技有限公司 | Three-decker transparent conductive film and preparation method thereof for dimming glass |
| CN108878058B (en) * | 2018-06-25 | 2019-11-22 | 湖北雄华科技有限公司 | Three-decker transparent conductive film and preparation method thereof for dimming glass |
| CN112334602A (en) * | 2018-07-05 | 2021-02-05 | 巴斯夫涂料有限公司 | Transparent conductive film |
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Open date: 20100421 |