CN100517517C - Flexible composite transparent conductive film and Manufacturing method - Google Patents
Flexible composite transparent conductive film and Manufacturing method Download PDFInfo
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- CN100517517C CN100517517C CNB2006100705099A CN200610070509A CN100517517C CN 100517517 C CN100517517 C CN 100517517C CN B2006100705099 A CNB2006100705099 A CN B2006100705099A CN 200610070509 A CN200610070509 A CN 200610070509A CN 100517517 C CN100517517 C CN 100517517C
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Abstract
The invention relates to a flexible, combined, transparent conducting film and the preparing method thereof, provided in turn with passivation layer, metal oxide layer, metal conducting layer and metal oxide layer on an organic flexible substrate, where the passivation layer is prepared by radio sputtering passivation target material in argon atmosphere, the metal oxide layer is prepared by radio sputtering metal oxide target material in argon atmosphere, and the metal conducting layer is prepared by DC sputtering metal target material in argon atmosphere. And its advantages: no need of heating substrate, simple manufacturing process, low cost, nontoxicity, no environmental pollution, and good photoelectric performance and stability.
Description
(1) technical field:
The present invention relates to a kind of flexible composite transparent conductive film and preparation method thereof, belong to the optoelectronic information technical field of function materials.
(2) background technology:
Nesa coating is meant the film low to light transmission rate height, the resistance of visible light.Transparent conductive film has a wide range of applications in electronics industry as a kind of important functional material, and it can be used as the transparency electrode of LCD, electroluminescent display, non-crystal silicon solar cell; Do the antifrost antifogging film of visible observation at aspects such as automobile, locomotive, aircraft, freezer, instrument and meters; Utilize its good micro-wave screening effect, be used for computer floor, radar shielding protection etc.The transparent conductive film for preparing on the hard glass substrate has reached higher application level.The transparent conductive film that on organic flexible parent metal, prepares have deflection, in light weight, should not be broken, be easy to large tracts of land production, be convenient to distinct advantages such as transportation, be expected to become the renewal product of hard glass substrate transparent conductive film.
Find that by retrieval the composite transparent conductive film for preparing has ITO/Ag/TO, is disclosed Chinese patent " metal indium-stannic oxide compound transparent electricity conductive film and preparation method thereof " among the CN1257135A referring to publication number on organic flexible parent metal to existing document; ZAO/ITO/ZAO number is disclosed Chinese patent among the CN2539375Y " a kind of flexible and transparent conductive composite membrane of high stable " referring to Granted publication.The composite transparent conductive film for preparing on the hard substrate has TiO
2/ Ag/TiO
2And ZnS/Ag/ZnS, be that disclosed Chinese patent among the CN1442872A " multi-layer nano nesa coating and preparation method thereof " and publication number are that disclosed Chinese patent among the CN1648693A " improves the method for Ag base composite transparent conductive film stability " referring to publication number; Dielectric/silver alloy/dielectric is disclosed Chinese patent among the CN85104006B " dielectric/silver alloy/dielectric type nesa coating " referring to publication number.
The conductivity and the light transmission of ITO/Ag/ITO for preparing on organic flexible parent metal and ZAO/ITO/ZAO composite transparent conductive film are better, but most ITO (In
2O
3: Sn) target dependence on import, In is a precious metal, and the ito thin film cost is higher, and In is poisonous, and it is contaminated environment not only, but also can work the mischief to health.The TiO that on the hard substrate, prepares
2/ Ag/TiO
2Have good optical property and electric property with money base composite transparent conductive films such as ZnS/Ag/ZnS, but the poor stability of money base composite transparent conductive film.Silver can produce white point or white fouling product under the environment of humidity, humidity causes that the part of silver is migrated at the interface, causes silver-colored interface binding power to descend, even causes the wrinkling of top film and come off.When getting involved, silver-colored film is easy to lump and is agglomerated into the discontinuous film of island when outside energy (as heating, illumination), and not only electric conductivity reduces greatly, and deterioration can take place the transmitance of visible light, and it is used because stability problem is restricted.People attempt to adopt silver alloy film to replace silverskin or at metal layer A g film and bottom TiO
2Add the stability that plating Ti layer improves silverskin between the film.The result shows the electric property and the optical property of but having sacrificed the money base composite transparent conductive film when improving stability.In addition, Ag is a precious metal, the cost height of money base composite transparent conductive film.As everyone knows, organic flexible parent metal is very responsive to humidity and oxygen, and organic flexible parent metal is than the easy absorption of glass substrate and infiltrate more humidity and oxygen.In film deposition process, these remaining compositions diffuse into film formation and are led or scattering center, the photoelectric properties of infringement film.Adopt above-mentioned technology to address these problems.
(3) summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of flexible composite transparent conductive film and preparation method thereof is provided, make simple, with low cost, nontoxic, free from environmental pollution, the made nesa coating of its manufacturing process conductivity and optical transmittance height, thickness evenness is good, photoelectric properties are stable.
Purpose of the present invention can reach by following measure: a kind of flexible composite transparent conductive film, it is characterized in that it has organic flexible parent metal, and be provided with passivation layer, metal oxide layer, metal conducting layer and metal oxide layer on organic flexible parent metal successively.
In order further to realize purpose of the present invention, wherein passivation layer is SiO
2Film or A1
2O
3Film, thickness 40-200nm, preferred 100nm; Metal oxide layer is ZnO film or TiO
2Film, thickness 20-100nm, preferred 50nm; Metal conducting layer is the Cu film, thickness 3-8nm, preferred 5nm.It is one of following that organic flexible parent metal is selected from: transparent polyester film, transparent polyethylene terephthaldehyde ester film, transparent polycarbonate film, transparent polypropylene film, transparent polyimide film, transparent polypropylene two ester films.
A kind of preparation method of flexible composite transparent conductive film, it is to adopt the non-reactive sputtering plated film of vacuum magnetic control to make on flexible parent metal, promptly radio frequency sputtering passivation target prepares passivation layer in argon atmosphere, radio frequency sputtering metal oxide target prepares metal oxide layer in argon atmosphere, the direct current sputtering metal targets prepares metal conducting layer in argon atmosphere, and flexible parent metal rotates to guarantee that base material is in the relevant position of different targets during alternating sputtering.All films adopt the mode of the non-reactive sputtering of vacuum to form, and working gas is an argon gas, makes in this way when the plating oxide membranous layer, has avoided the oxidation of metal conducting layer.
In order further to realize purpose of the present invention, preparation technology's concrete steps of the present invention are as follows:
1, highly purified passivation target is installed in the radio frequency negative electrode target groove of a water-cooled in the sputtering chamber of magnetic control sputtering device, highly purified metal oxide target is installed in the radio frequency negative electrode target groove of another water-cooled in the sputtering chamber, highly purified metal targets is installed in the direct current negative electrode target groove of the water-cooled in the sputtering chamber, the washed flexible base material is put into substrate frame, in the media disk in the substrate frame insertion sputtering chamber, the adjustment target-substrate distance is 40-80mm;
2, sputtering chamber and gas pipeline are bled, the base vacuum that makes sputtering chamber is less than 1.0 * 10
-3Pa, the back charges into the high-purity gas argon gas in sputtering chamber, adjust rate of air sucked in required, and the gas pressure intensity that makes sputtering chamber is 0.5-3Pa;
3, at first open the radio-frequency power supply of passivation target, treat that radio frequency glow discharge is stable after, flexible parent metal is gone to passivation target correspondence position carries out the sputtering sedimentation passivation layer; The radio-frequency power supply of opening metal oxide target material again, treat that radio frequency glow discharge is stable after, flexible parent metal is gone to metal oxide target correspondence position carries out the sputtering sedimentation metal oxide layer; The DC power supply of opening metal target then, treat that direct current glow discharge is stable after, flexible parent metal is gone to the metal targets correspondence position carries out the sputtering sedimentation metal conducting layer; Turn round flexible parent metal to metal oxide target correspondence position at last and carry out the sputtering sedimentation metal oxide layer, make flexible composite transparent conductive film, the film thickness in the film deposition process is monitored in real time by the film thickness monitoring instrument of magnetic control sputtering device.
For further realization purpose of the present invention, the sputtering power of described passivation target: 100-500W, the sputtering power of metal oxide target: 20-100W, the sputtering power of metal targets: 10-50W, sputter temperature is room temperature.
Under preferred processing condition, promptly the sputtering chamber base vacuum 4.0 * 10
-4Pa, target-cardinal distance 50mm, working gas pressure 0.9Pa; Passivation layer SiO
2The commodity SiO of rf magnetron sputtering purity 99.99WT% is adopted in the preparation of film
2Target, sputtering power 120W; The commodity ZnO target of rf magnetron sputtering purity 99.99WT%, sputtering power 48W are adopted in the preparation of metal oxide layer ZnO film; The commodity Cu target of magnetically controlled DC sputtering purity 99.99WT%, sputtering power 20W are adopted in the preparation of metal conducting layer Cu film; The sputter temperature room temperature, the rete parameter adopts SiO
2(100nm)/during ZnO (50nm)/Cu (5nm)/ZnO (50nm), the square resistance of flexible composite transparent conductive film is that 10 Ω/, visible light transmissivity (550nm) are higher than 88%.Membrane structure and photoelectric properties are stable, combine firmly with organic flexible parent metal.
The experiment proved that above-mentioned passivation layer SiO
2Film can be used Al
2O
3Film replaces, and the metal oxide layer ZnO film can be used TiO
2Film replaces, and the optical characteristics of flexible composite transparent conductive film and electrology characteristic are also very good.
The present invention can produce following good effect compared with the prior art: substrate of the present invention does not need to heat, manufacturing process is simpler, with low cost, nontoxic, free from environmental pollution, the conductivity of made nesa coating and optical transmittance height, thickness evenness is good, photoelectric properties are stable, combine firmly with organic flexible parent metal.
(4) embodiment:
Below the specific embodiment of the present invention is elaborated:
Embodiment 1:100nm SiO
2/ 50nm ZnO/5nm Cu/50nm ZnO
Flexible parent metal adopts the transparent polyester film of thickness 125 μ m, cleans with sonochemistry.Commodity SiO with purity 99.99WT%
2Target is installed in the radio frequency negative electrode target groove of a water-cooled in the sputtering chamber of magnetic control sputtering device, the commodity ZnO target of purity 99.99WT% is installed in the radio frequency negative electrode target groove of another water-cooled in the sputtering chamber of magnetic control sputtering device, the commercial metal Cu target of purity 99.99WT% is installed in the direct current negative electrode target groove of water-cooled of sputtering chamber of magnetic control sputtering device, the above-mentioned flexible parent metal that cleaned is put into substrate frame, substrate frame is inserted in the media disk of sputtering chamber, adjustment target-cardinal distance is 50mm; Sputtering chamber and gas pipeline are bled, and the base vacuum that makes sputtering chamber is less than 1.0 * 10
-3Pa, the back charges into the argon gas of purity 99.99% in sputtering chamber, adjust rate of air sucked in required, and the gas pressure intensity that makes sputtering chamber is 0.9Pa; At first open SiO
2The radio-frequency power supply of target, treat that radio frequency glow discharge is stable after, flexible parent metal is gone to SiO
2The target correspondence position carries out sputtering sedimentation passivation layer SiO
2Film, sputtering power: 120W; Open the radio-frequency power supply of ZnO target again, treat that radio frequency glow discharge is stable after, flexible parent metal is gone to ZnO target correspondence position carries out the sputtering sedimentation ZnO film, sputtering power: 48W; Open the DC power supply of Cu target then, treat that direct current glow discharge is stable after, flexible parent metal is gone to Cu target correspondence position carries out sputtering sedimentation Cu film, sputtering power: 20W; Turn round flexible parent metal to ZnO target correspondence position at last and carry out the sputtering sedimentation ZnO film, sputtering power: 48W.Media disk is rotated to guarantee that flexible parent metal is in the relevant position of different targets during alternating sputtering, and sputter temperature is room temperature, and film thickness is monitored in real time by the film thickness monitoring instrument in the film deposition process, makes flexible composite transparent conductive film.The square resistance of flexible composite transparent conductive film is that 10 Ω/, visible light transmissivity (550nm) are higher than 88%.Membrane structure and photoelectric properties are stable, combine firmly with organic flexible parent metal.
Embodiment 2:40nm SiO
2/ 20nm ZnO/5nm Cu/20nm ZnO
Preparation technology is described with embodiment 1 substantially, and different is the transparency polycarbonate film that flexible parent metal adopts thickness 175 μ m, and target-cardinal distance is 40mm, and the gas pressure intensity of sputtering chamber is 0.5Pa, radio frequency sputtering SiO
2The sputtering power 100W of target, the sputtering power 20W of radio frequency sputtering ZnO target, the sputtering power 10W of direct current sputtering Cu target.The square resistance of flexible composite transparent conductive film is that 10 Ω/, visible light transmissivity (550nm) are higher than 86%.Membrane structure and photoelectric properties are stable, combine firmly with flexible parent metal.
Embodiment 3:200nm SiO
2/ 100nm ZnO/5nm Cu/100nm ZnO
Preparation technology is described with embodiment 1 substantially, and different is the clear polyimides film that flexible parent metal adopts thickness 75 μ m, and the gas pressure intensity of sputtering chamber is 3Pa, radio frequency sputtering SiO
2The sputtering power 500W of target, the sputtering power 100W of radio frequency sputtering ZnO target, the sputtering power 25W of direct current sputtering Cu target.The square resistance of flexible composite transparent conductive film is that 10 Ω/, visible light transmissivity (550nm) are higher than 85%.Membrane structure and photoelectric properties are stable, combine firmly with flexible parent metal.
Embodiment 4:100nm Al
2O
3/ 50nm ZnO/3nm Cu/50nm ZnO
Preparation technology is described with embodiment 1 substantially, and different is transparent polypropylene two ester films that flexible parent metal adopts thickness 125 μ m, the passivation target commodity Al of purity 99.99WT%
2O
3Target, target-cardinal distance are 55mm, the gas pressure intensity 1.3Pa of sputtering chamber, radio frequency sputtering Al
2O
3The sputtering power 180W of target, the sputtering power 60W of radio frequency sputtering ZnO target, the sputtering power 10W of direct current sputtering Cu target.The square resistance of flexible composite transparent conductive film is that 25 Ω/, visible light transmissivity (550nm) are higher than 80%.Membrane structure and photoelectric properties are stable, combine firmly with flexible parent metal.
Embodiment 5:100nm SiO
2/ 50nm ZnO/8nm Cu/50nm ZnO
Preparation technology is described with embodiment 1 substantially, and different is the transparent polypropylene film that flexible parent metal adopts thickness 75 μ m, and target-cardinal distance is 80mm, the sputtering power 50W of direct current sputtering Cu target.The square resistance of flexible composite transparent conductive film is that 5 Ω/, visible light transmissivity (550nm) are higher than 72%.Membrane structure and photoelectric properties are stable, combine firmly with flexible parent metal.
Embodiment 6:100nm SiO
2/ 50nm TiO
2/ 5nm Cu/50nm TiO
2
Preparation technology is described with embodiment 1 substantially, and different is the transparent polyethylene terephthaldehyde ester film that flexible parent metal adopts thickness 125 μ m, the metal oxide target commodity TiO of purity 99.99WT%
2Target.The square resistance of flexible composite transparent conductive film is that 10 Ω/, visible light transmissivity (550nm) are higher than 86%.Membrane structure and photoelectric properties are stable, combine firmly with flexible parent metal.
Claims (9)
1, a kind of flexible composite transparent conductive film is characterized in that it has organic flexible parent metal, is provided with passivation layer, metal oxide layer, metal conducting layer and metal oxide layer on organic flexible parent metal successively, and described metal oxide layer is ZnO film or TiO
2Film.
2, a kind of flexible composite transparent conductive film according to claim 1, the thickness that it is characterized in that described passivation layer is 40-200nm, and the thickness of metal oxide layer is 20-100nm, and the thickness of metal conducting layer is 3-8nm.
3, a kind of flexible composite transparent conductive film according to claim 2, the thickness that it is characterized in that described passivation layer is 100nm; The thickness of metal oxide layer is 50nm; The thickness of metal conducting layer is 5nm.
4, according to claim 1 or 2 or 3 described a kind of flexible composite transparent conductive films, it is characterized in that described passivation layer is SiO
2Film or Al
2O
3Film.
5,, it is characterized in that described metal conducting layer is the Cu film according to claim 1 or 2 or 3 described a kind of flexible composite transparent conductive films.
6, a kind of flexible composite transparent conductive film according to claim 1 is characterized in that described organic flexible parent metal is a kind of in transparent polyester film, polyethylene terephthaldehyde ester film, polycarbonate film, polypropylene film, polyimide film, polypropylene two ester films.
7, the preparation method of the described a kind of flexible composite transparent conductive film of claim 1, it is characterized in that it is to adopt the non-reactive sputtering plated film of vacuum magnetic control to make on flexible parent metal, promptly radio frequency sputtering passivation target prepares passivation layer in argon atmosphere, radio frequency sputtering metal oxide target prepares metal oxide layer in argon atmosphere, the direct current sputtering metal targets prepares metal conducting layer in argon atmosphere, the sputtered metal oxide target prepares metal oxide layer, and flexible parent metal rotates to guarantee that base material is in the relevant position of different targets during alternating sputtering.
8, the preparation method of a kind of flexible composite transparent conductive film according to claim 7 is characterized in that it specifically comprises the steps:
A, the passivation target of purity 99.99WT% is installed in the radio frequency negative electrode target groove of a water-cooled in the sputtering chamber of magnetic control sputtering device, the metal oxide target of purity 99.99WT% is installed in the radio frequency negative electrode target groove of another water-cooled in the sputtering chamber, the metal targets of purity 99.99WT% is installed in the direct current negative electrode target groove of the water-cooled in the sputtering chamber, the washed flexible base material is put into substrate frame, in the media disk in the substrate frame insertion sputtering chamber, the distance of adjusting between target and the organic flexible parent metal is 40-80mm;
B, sputtering chamber and gas pipeline are bled, the base vacuum that makes sputtering chamber is less than 1.0 * 10
-3Pa, the back charges into the gas argon gas of purity 99.99% in sputtering chamber, adjust rate of air sucked in required, and the gas pressure intensity that makes sputtering chamber is 0.5-3Pa;
C, at first open the radio-frequency power supply of passivation target, treat that radio frequency glow discharge is stable after, flexible parent metal is gone to passivation target correspondence position carries out the sputtering sedimentation passivation layer; The radio-frequency power supply of opening metal oxide target material again, treat that radio frequency glow discharge is stable after, flexible parent metal is gone to metal oxide target correspondence position carries out the sputtering sedimentation metal oxide layer; The DC power supply of opening metal target then, treat that direct current glow discharge is stable after, flexible parent metal is gone to the metal targets correspondence position carries out the sputtering sedimentation metal conducting layer; Turn round flexible parent metal to metal oxide target correspondence position at last and carry out the sputtering sedimentation metal oxide layer, make flexible composite transparent conductive film, the film thickness in the film deposition process is monitored in real time by the film thickness monitoring instrument of magnetic control sputtering device.
9, the preparation method of a kind of flexible composite transparent conductive film according to claim 8, the sputtering power that it is characterized in that described passivation target: 100-500W, the sputtering power of metal oxide target: 20-100W, the sputtering power of metal targets: 10-50W, sputter temperature: room temperature.
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|---|---|---|---|
| CNB2006100705099A CN100517517C (en) | 2006-11-22 | 2006-11-22 | Flexible composite transparent conductive film and Manufacturing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100705099A CN100517517C (en) | 2006-11-22 | 2006-11-22 | Flexible composite transparent conductive film and Manufacturing method |
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|---|---|
| CN1979695A CN1979695A (en) | 2007-06-13 |
| CN100517517C true CN100517517C (en) | 2009-07-22 |
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Families Citing this family (15)
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| CN101582304A (en) * | 2008-05-13 | 2009-11-18 | 日东电工株式会社 | Transparent conductive film and method for production thereof |
| CN102157575A (en) * | 2011-03-28 | 2011-08-17 | 天津师范大学 | Novel transparent conducting oxide thin film with multi-layer film structure and manufacturing method thereof |
| CN102418096B (en) * | 2011-12-07 | 2013-08-07 | 天津大学 | Kapton/Al2O3 surface nanometer composite membrane and application |
| CN104616726B (en) * | 2014-12-17 | 2017-10-24 | 青岛墨烯产业科技有限公司 | One kind is without indium transparency electrode and preparation method thereof |
| CN104701437A (en) * | 2015-03-09 | 2015-06-10 | 武汉大学 | Three-dimensional LED luminescent device |
| CN105039911B (en) * | 2015-08-14 | 2019-01-22 | 陕西师范大学 | A kind of transparent conductive film and preparation method thereof |
| CN111204988B (en) * | 2018-11-21 | 2023-09-29 | 中国建筑材料科学研究总院有限公司 | Flexible film type thermal control coating and preparation method thereof |
| CN109887746B (en) * | 2019-03-06 | 2021-01-01 | 无锡鑫聚电子科技有限公司 | Metallized film for high-reliability high-power capacitor and preparation method thereof |
| CN111916523A (en) * | 2019-05-07 | 2020-11-10 | 君泰创新（北京）科技有限公司 | Heterojunction solar cell, assembly thereof and preparation method |
| CN110205588A (en) * | 2019-06-11 | 2019-09-06 | 贵州优宝泰光电有限责任公司 | A kind of PVD flexible conductive film, preparation method and its method for generating microcircuit through nano effect |
| CN111053298B (en) * | 2019-12-20 | 2022-03-15 | 深圳麦克韦尔科技有限公司 | Flexible heating element and manufacturing method thereof, flexible heating assembly and aerosol generator |
| CN112941464B (en) * | 2021-01-28 | 2022-09-16 | 山东省科学院能源研究所 | Multilayer transparent conductive film and preparation method and application thereof |
| CN112951930B (en) * | 2021-01-29 | 2022-11-04 | 山东省科学院能源研究所 | Titanium dioxide/silver/titanium dioxide transparent conductive film and preparation method and application thereof |
| CN114737153B (en) * | 2022-03-22 | 2023-07-18 | 洛阳理工学院 | Strontium titanate/gold/silicon dioxide structured flexible transparent electrode and preparation method thereof |
| CN114753150A (en) * | 2022-05-12 | 2022-07-15 | 广东欣丰科技有限公司 | Conductive fabric and manufacturing method and application thereof |
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