CN101476109B - Preparation of flexible high-resistance multi-layer transparent conductive film - Google Patents
Preparation of flexible high-resistance multi-layer transparent conductive film Download PDFInfo
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- CN101476109B CN101476109B CN2008100304143A CN200810030414A CN101476109B CN 101476109 B CN101476109 B CN 101476109B CN 2008100304143 A CN2008100304143 A CN 2008100304143A CN 200810030414 A CN200810030414 A CN 200810030414A CN 101476109 B CN101476109 B CN 101476109B
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- pet polyester
- polyester film
- indium tin
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Abstract
The invention provides a method for preparing a flexible high resistance multi-layer transparent conductive film which includes steps as follows: forming a titanium dioxide layer, a silicon dioxide layer, an indium tin oxide layer, a zinc-aluminium oxide layer or zinc-gallium oxide layer continuously and orderly on one surface of a flexible base material PET polyester film by using a mid-frequency magnetron sputtering technique; temperature reaching to 120 DEG C or more by using heat energy generated by bombardment continuously and deposition of the high-energy particle on the PET polyester film, and controlling oxide-indium atom ratio between 1.26-1.29 for obtaining the indium tin oxide layer with crystal structure; adhibiting another side of the PET polyester with one side of the second layer PET polyester, setting a hard coating on another side of the second layer PET polyester; forming the titanium dioxide layer and the silicon dioxide layer continuously and orderly on the hard coating by using mid-frequency magnetron sputtering technique. The product has better resistance stability and durability, has advantages of short production flow, high efficiency and low cost. The product is not easy to warp in follow processing flow.
Description
Technical field
The present invention relates to the preparation method of flexible parent metal high-resistance multi-layer transparent conductive film, this film can be used for touch-screen (TP), handwriting input (PE), electroluminescent demonstration (EL), liquid-crystal display (LCD), organic light emitting display (OLED) etc.
Background technology
Existing flexible transparent conducting film, surface resistivity is more stable about 200 Ω/mouths.But along with surface resistivity raises, particularly arrived 450-500 Ω/mouth or more after the high value, then resistance value becomes very unstable, weather resistance (number of clicks that can bear) is also very poor, and occurs phenomenon such as warpage in use subsequently.Patent of invention CN1947204A has proposed technology such as the crystallization of a rhythmo structure and control ITO film and grain size number, crystal area proportion, make surface resistivity be 200-300 Ω/mouth ITO membrane stability, weather resistance be improved significantly; But it has some not enough: the one, to handle 1.5 hours at 150 ℃ after the ITO film film forming, and this obviously can influence production efficiency, improve production cost; The 2nd, medium layer silicon-dioxide (SiO
2) adopt coating and electron gun evaporation incompatible with ITO film film technique, make very numerous and diverse that technological process becomes, cause that yield rate is low, the cost raising; The 3rd, its multilayer body one side does not have moistureproof moisture barrier, in use is subjected to the high temperature moisture effect, makes this side draught tide moisture absorption, causes two-layer PET polyester film owing to the difference of shrinking percentage produces warpage, influences the carrying out of subsequent production process; And, be compositional analysis from film, transmittance also can not be done very highly.Japanese Patent HZ-194943A has proposed a modification method, promptly after the ITO film forming again long heat treatment make its crystallization, improve its stability, specifically be 150 ℃ of thermal treatments 24 hours, obviously this method inefficiency, cost are high.U.S. Pat 2003/0012955A1 then proposes at ITO film surface coverage one deck medium layer, and as SiOx or TiOx, TaOx, media such as NbOx, SnOx, consequently surface contacted resistance increases, and also can make troubles to etching.U.S. Pat 2006/003188A1 proposes with containing tindioxide (SnO
2) indium tin oxide (ITO) target less than 6% is at 90 ℃ of-170 ℃ of spatter film formings, makes the ITO film form crystalline texture, improves its performance; The shortcoming that exists is will be in film forming under the comparatively high temps, and film process will be used PEM (plasma emission) or PIC (plasma impedance control) monitoring.
Summary of the invention
The objective of the invention is, problems such as the ITO high resistance film resistance instability that exists at prior art products, poor durability, a kind of preparation method of flexible high-resistance multi-layer transparent conductive film is proposed, prepared product has good resistance stability and weather resistance when comparatively high temps (150 ℃), and the technological process of production is short, production efficiency is high, cost is low, and goods do not produce warpage in technological process subsequently.
Technical scheme of the present invention is that the preparation method of described flexible high-resistance multi-layer transparent conductive film is: adopt the medium frequency magnetron sputtering technology to form titanium dioxide layer 2, silicon dioxide layer 3, indium tin oxide layer 4, Zinc-aluminium layer or zinc gallium oxide layer 5 successively continuously in the one side of flexible parent metal PET polyester film 1;
In the film process of indium tin oxide layer 4, high energy particle bombards and is deposited on the heat energy of generation on the PET polyester film 1 continuously when utilizing described titanium dioxide layer 2 and silicon dioxide layer 3 medium frequency magnetron sputtering film forming, make temperature reach 120 ℃ or higher, thereby obtain the indium tin oxide layer 4 of crystalline texture; And control oxygen phosphide atom than (O/In) in the 1.26-1.29 scope, obtain resistance-stable indium tin oxide layer 4;
Described flexible parent metal PET polyester film 1 another side is mutually bonding with the one side of second layer PET polyester film 7 through tack coat 6, and at the another side of this second layer PET polyester film 7 hard coat 8 is set;
On hard coat 8, form titanium dioxide layer 9, silicon dioxide layer 10 successively continuously with the medium frequency magnetron sputtering technology.
Below the present invention made further specify.
Referring to Fig. 1, the structure of the flexible high-resistance multi-layer transparent conductive film that the inventive method makes is: it has flexible parent metal PET polyester film 1, has successively from the inside to the outside as anti-reflection and titanium dioxide (TiO sealing coat in the one side of this PET polyester film 1
2) layer 2, silicon-dioxide (SiO
2) layer 3, electrically conducting transparent crystal form indium tin oxide (ITO) layer 4 and top layer 5, described top layer are Zinc-aluminium (ZAO) layer or zinc gallium oxide (ZGO) layer 5; The another side of described PET polyester film 1 is mutually bonding with the one side of second layer flexible parent metal PET polyester film 7 through tack coat 6, and the another side of this second layer PET polyester film 7 is provided with hard coat 8 and from the inside to the outside successively as anti-reflection and titanium dioxide (the TiO moisture proof layer
2) layer 9, silicon-dioxide (SiO
2) layer 10.
As everyone knows, the unsettled reason of flexible high-resistance indium tin oxide (ITO) film high-temp. resistance mainly contains three: the one, and the resistivity of the indium tin oxide film that forms is at low temperatures arranged by oxygen vacancy concentration, its oxygen phosphide atom is 1.31 than the threshold value of (O/In), and the oxygen phosphide atom is than sharply increasing greater than 1.31 back resistivity.Therefore, indium tin oxide film is exposed to and can causes in the high temperature air that oxygen vacancy concentration sharply changes (increase of O/In ratio), causes resistance change; The 2nd, all be in normal temperature (20 ℃) or film forming under the low temperature more at conventional preparation indium tin oxide film on the PET polyester film, film is a non-crystalline structure, PET polyester film surface ratio is more coarse in addition, membrane structure is loose, help in the air oxygen to the rete internal divergence, quicken the increase of oxygen vacancy concentration in the rete; The 3rd, the PET polyester film is easy to adsorb steam and oxygen, and these steam and oxygen also can increase the oxygen vacancy concentration of rete to indium tin oxide rete infiltration diffusion.This situation is particularly evident when high resistant (350 Ω/mouth-550 Ω/mouths for example, this moment, resistive film was very thin, thickness only is 15-18nm).The property of the present invention is directed to taked three technical measures: the one, with existing anti-reflection effect have again the titanium dioxide layer 2 of barrier functionality and silicon dioxide layer 3 and Zinc-aluminium layer or zinc gallium oxide layer (top layer) 5 with indium tin oxide layer 4 double teams in the centre, blocks air (oxygen) or other pollute impurity diffusion in indium tin oxide (ITO) layer 4; The 2nd, adopt the medium frequency magnetron sputtering technology once to form titanium dioxide layer 2, silicon dioxide layer 3, indium tin oxide layer 4, Zinc-aluminium layer or zinc gallium oxide layer (top layer) 5 successively continuously, because high energy particle bombards continuously and is deposited on the PET polyester film 1, make its temperature reach 120 ℃, even it is higher, thereby obtain the stable indium tin oxide layer 4 of crystalline texture, and intermediate frequency sputtering technology film forming makes described each tunic Dou Hen Cause close, has more effectively stopped air (oxygen) or other impurity entering and spread to indium tin oxide layer 4; The 3rd, the oxygen room of control indium tin oxide layer 4 is not in the sensitive area, and promptly the oxygen phosphide atom is controlled at the 1.26-1.29 scope than (O/In), even aerobic enters diffusion like this, also can significantly not change the resistance value of indium tin oxide layer 4.Take such three technical measures, can make indium tin oxide layer 4 oxygen vacancy concentration maintenance at high temperature stable, thereby guaranteed the high-temperature stability of resistance.
The present invention has taked three technical measures to the weather resistance (life-span) that improves described flexible high-resistance multi-layer transparent conductive film: (1) is provided with a top layer in this flexible high-resistance multi-layer transparent conductive film structure, it is Zinc-aluminium (ZAO) layer or zinc gallium oxide (ZGO) layer 5 of a high resistant, and the surface resistivity of this layer oxide compound is controlled at greater than 1 * 10
4Ω/mouth; In this case, described top layer (ZAO or ZGO) is not more than 5% in the shunting resistance ratio with indium tin oxide layer 4 formation in parallel; Surface resistivity with indium tin oxide layer 4 is that 500 Ω/mouths are example, if the surface resistivity of top layer is controlled to be 1 * 10
4Ω/mouth, then shunting resistance is 476 Ω/mouths, the surface resistivity proportion of top layer only is 4.8%; Therefore top layer (ZAO or ZGO) is a diffusion impervious layer to indium tin oxide layer 4, it also is an attrition resistant depletion layer, (ZAO or ZGO) exhausts up to this top layer, the surface resistivity velocity of variation of indium tin oxide layer 4 can be greater than 5% yet, and this just helps improving the work-ing life of indium tin oxide layer 4; (2) titanium dioxide layer 2 of product, silicon dioxide layer 3, indium tin oxide layer 4 and top layer (ZAO or ZGO) are to adopt (once) shaping continuously successively of medium frequency magnetron sputtering method, the temperature of PET polyester film 1 reaches 120 ℃ or higher, indium tin oxide layer 4 and top layer (ZAO layer or ZGO layer) form crystalline texture, and Mo Ceng Cause is close, hardness and wear resistance improve, so its weather resistance (life-span) improves; (3) described flexible high-resistance multi-layer transparent conductive film has utilized the stress diffusion mechanism of compound basement membrane, has improved durability of products; As shown in Figure 1, be used in silicon-dioxide (SiO when masterpiece
2) when layer 10 (moisture-proof barrier) were gone up, thicker second layer PET polyester film 7 had born most of stress, then tack coat 6 again counter stress played shock absorption, and it is just very slight to be delivered to the stress of indium tin oxide layer 4 and top layer (ZAO layer or ZGO layer).Because indium tin oxide layer 4 is by titanium dioxide layer 2, silicon dioxide layer 3 and top layer (ZAO layer or ZGO layer) institute's double team; they have good adhering to and provide protection; indium tin oxide layer 4 is not directly contacted with the counter electrode (being base material usually with glass) of touch-screen, weather resistance (life-span) is improved.
Among the present invention, the thickness of described flexible parent metal PET polyester film 1 can be 30 μ m-60 μ m, and preferred thickness is 50 μ m, with the snappiness that guarantees that it is enough; As anti-reflection and titanium dioxide (the TiO blocking layer
2) layer 2 and silicon-dioxide (SiO
2) layer 3 optical thickness can be respectively 1/2 λ
0With 1/4 λ
0(λ
0=550nm), geometric thickness can be respectively 120nm-125nm and 90nm-100nm; The thickness of indium tin oxide layer 4 can be 13nm-22nm, and surface resistivity can be 350 Ω/mouth-550 Ω/mouths; Zinc-aluminium layer or zinc gallium oxide layer (top layer) 5 thickness can be 5nm-10nm, and surface resistivity is 1 * 10
4Ω/mouth-8 * 10
4Ω/mouth.
Described flexible parent metal PET polyester film 1 another side is mutually bonding with second layer PET polyester film 7 through tack coat 6, and bonding method can be carried out compound with the compounding machine of routine.The thickness of tack coat 6 can be 5 μ m-20 μ m, and preferred thickness is 10 μ m-13 μ m, to guarantee to have enough elasticity and stress buffer performance; The thickness of second layer PET polyester film 7 can be 115 μ m-155 μ m, is preferably 125 μ m, to guarantee enough physical strengths and elasticity; The thickness of the hard coat 8 of described second layer PET polyester film 7 another sides can be 3 μ m-5 μ m, and its hardness can be pencil hardness 3H, and it is one deck organism coating; And anti-reflection and moisture proof layer subsequently, be that titanium dioxide layer 9 is the same with silicon dioxide layer 3 with aforesaid titanium dioxide layer 2 with silicon dioxide layer 10, be to adopt intermediate frequency magnetic sputtering technology to form, its thickness can be respectively 120nm-125nm and 90nm-100nm, existing anti-reflection effect can prevent that again the second layer PET polyester film 7 and organic hard coatings 8 moisture absorptions are wet.
As known from the above, the present invention is a kind of flexible high-resistance multi-layer transparent conductive film, and its stability and good endurance, its surface resistivity in the high resistant scope (350 Ω/mouth-550 Ω/mouth) have good high-temperature stability (150 ℃, 30 minutes, surface resistivity changed R
T/ R
0Less than 1.1); Because two antireflection layers are arranged, visible light transmissivity is greater than 90%; Owing to adopt medium frequency magnetron sputtering technology film forming, film layer structure and performance have been improved, again owing to adopted blocking layer-high resistance transparent oxide compound top layer and multi-layer film structures such as stress dispersion, buffering, its weather resistance is fine, that uses hardness 40 contains urethanes rod (termination 7R), load is 100 grams, carries out 1,000,000 times and gets test ready, surface resistivity velocity of variation (R
T/ R
0) be 1.0, promptly get 1,000,000 times ready after, the surface resistivity no change.Also because the existence of outermost moisture proof layer has prevented PET polyester film and organic hard coatings moisture absorption, kept 1 hour under at 150 ℃, relative humidity greater than 80% condition, do not find warpage.
Description of drawings
Fig. 1 is a kind of cross section structure synoptic diagram of embodiment product, in the drawings:
The 1-PET polyester film, the 2-titanium dioxide layer, the 3-silicon dioxide layer,
The 4-indium tin oxide layer, 5-Zinc-aluminium layer or zinc gallium oxide layer (top layer),
The 6-tack coat, 7-second layer PET polyester film,
The 8-hard coat, 9-titanium dioxide layer, 10-silicon dioxide layer.
Embodiment
The inventive method comprises:
Adopt the medium frequency magnetron sputtering technology to form titanium dioxide layer 2, silicon dioxide layer 3, indium tin oxide layer 4, Zinc-aluminium layer or zinc gallium oxide layer 5 successively continuously in the one side of flexible parent metal PET polyester film 1;
In the film process of indium tin oxide layer 4, high energy particle bombards and is deposited on the heat energy of generation on the PET polyester film 1 continuously when utilizing aforementioned titanium dioxide layer 2 and silicon dioxide layer 3 medium frequency magnetron sputtering film forming, make temperature reach 120 ℃ or higher, and control oxygen phosphide atom than (O/In) in the 1.26-1.29 scope, thereby obtain the indium tin oxide layer 4 of crystalline texture;
Described flexible parent metal PET polyester film 1 another side is mutually bonding with the one side of second layer PET polyester film 7 through tack coat 6, and at the another side of this second layer PET polyester film 7 hard coat 8 is set;
On hard coat 8, form titanium dioxide layer 9, silicon dioxide layer 10 successively continuously with the medium frequency magnetron sputtering technology.
Described flexible parent metal PET polyester film 1 another side is mutually bonding with the one side of second layer PET polyester film 7 through tack coat 6, and its bonding method can be carried out compound with the compounding machine of routine.
The structure of products obtained therefrom is, has successively from the inside to the outside as anti-reflection and titanium dioxide (TiO sealing coat in the one side of PET polyester film 1
2) layer 2, silicon-dioxide (SiO
2) layer 3, electrically conducting transparent crystal form indium tin oxide (ITO) layer 4 and Zinc-aluminium layer or zinc gallium oxide layer (top layer) 5; The another side of described PET polyester film 1 is mutually bonding with the one side of second layer flexible parent metal PET polyester film 7 through tack coat 6, and the another side of this second layer PET polyester film 7 is provided with hard coat 8 and from the inside to the outside successively as anti-reflection and titanium dioxide (the TiO moisture proof layer
2) layer 9, silicon-dioxide (SiO
2) layer 10; Wherein, flexible parent metal PET polyester film 1 thickness 50 μ m, titanium dioxide layer 2 thickness 120nm, silicon dioxide layer 3 thickness 95nm; Electrically conducting transparent crystal form indium tin oxide (TTO) layer 4 thickness 15nm, surface resistivity 500 Ω/mouths; The thickness 5nm of Zinc-aluminium layer or zinc gallium oxide layer 5, surface resistivity 5 * 10
4Ω/mouth; Tack coat 6 thickness 10 μ m; Second layer PET polyester film 7 thickness 125 μ m; Hard coat 8 thickness 3 μ m; Titanium dioxide layer 9 thickness 120nm, silicon dioxide layer 10 thickness 95nm.
Claims (6)
1. the preparation method of a flexible high-resistance multi-layer transparent conductive film is characterized in that, this method is:
Adopt the medium frequency magnetron sputtering technology to form titanium dioxide layer (2), silicon dioxide layer (3), indium tin oxide layer (4), Zinc-aluminium layer or zinc gallium oxide layer (5) successively continuously in the one side of flexible parent metal PET polyester film (1);
In the film process of indium tin oxide layer (4), high energy particle bombards continuously and is deposited on PET polyester film (1) and goes up the heat energy that produces when utilizing described titanium dioxide layer (2) and silicon dioxide layer (3) medium frequency magnetron sputtering film forming, make temperature reach 120 ℃ or higher, thereby obtain the indium tin oxide layer (4) of crystalline texture; And control oxygen phosphide atom obtains resistance-stable indium tin oxide layer (4) than in the 1.26-1.29 scope;
Described flexible parent metal PET polyester film (1) another side is mutually bonding with the one side of second layer PET polyester film (7) through tack coat (6), and at the another side of this second layer PET polyester film (7) hard coat (8) is set; On hard coat (8), form titanium dioxide layer (9), silicon dioxide layer (10) successively continuously with the medium frequency magnetron sputtering technology.
2. according to the preparation method of the described flexible high-resistance multi-layer transparent conductive film of claim 1, it is characterized in that the thickness of the described flexible parent metal PET polyester film (1) of employing is 30 μ m-60 μ m.
3. according to the preparation method of the described flexible high-resistance multi-layer transparent conductive film of claim 1, it is characterized in that the described titanium dioxide layer that makes and the optical thickness of silicon dioxide layer are respectively 1/2 λ
0With 1/4 λ
0, geometric thickness is respectively 120nm-125nm and 90nm-100nm, λ
0=550nm.
4. according to the preparation method of the described flexible high-resistance multi-layer transparent conductive film of claim 1, it is characterized in that the thickness of the described indium tin oxide layer (4) that makes is 13nm-22nm, surface resistivity is 350 Ω/-550 Ω/.
5. according to the preparation method of the described flexible high-resistance multi-layer transparent conductive film of claim 1, it is characterized in that described Zinc-aluminium layer that makes or zinc gallium oxide layer (5) thickness are 5nm-10nm, surface resistivity is 1 * 10
4Ω/-8 * 10
4Ω/.
6. according to the preparation method of the described flexible high-resistance multi-layer transparent conductive film of claim 1, it is characterized in that the thickness of the described second layer PET polyester film (7) of employing is 115 μ m-155 μ m.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102034565B (en) * | 2009-10-06 | 2014-01-29 | 日油株式会社 | Transparent conductive film |
| CN102074281A (en) * | 2010-12-21 | 2011-05-25 | 苏州禾盛新型材料股份有限公司 | RF plasma transparent conductive film |
| CN102126321A (en) * | 2010-12-21 | 2011-07-20 | 苏州禾盛新型材料股份有限公司 | PET (poly(ethylene terephthalate)) transparent conductive composite panel |
| CN102324271A (en) * | 2011-10-14 | 2012-01-18 | 南昌欧菲光科技有限公司 | Crystallized type ITO (Indium Tin Oxide) transparent conductive film and preparation method thereof |
| CN102723128B (en) * | 2012-06-25 | 2015-02-18 | 深圳豪威真空光电子股份有限公司 | Flexible transparent conductive film and manufacturing method thereof and touch panel |
| CN103337279A (en) * | 2013-06-26 | 2013-10-02 | 汕头万顺包装材料股份有限公司光电薄膜分公司 | Transparent conductive film and touch panel employing same |
| CN103777814B (en) * | 2014-01-16 | 2017-06-16 | 京东方科技集团股份有限公司 | A kind of display panel and preparation method thereof and display device |
| CN109280886A (en) * | 2018-08-09 | 2019-01-29 | 滁州盛诺电子科技有限公司 | A kind of high resistance film and its preparation process and application |
| CN109725468A (en) * | 2019-03-11 | 2019-05-07 | 广州市华惠材料科技有限公司 | Light modulation film and preparation method thereof |
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|---|---|---|---|---|
| US6284382B1 (en) * | 1997-11-27 | 2001-09-04 | Sony Corporation | Antireflection film and manufacturing method thereof |
| CN1729310A (en) * | 2002-11-01 | 2006-02-01 | 艾利丹尼森公司 | Transparent conductive film for flat panel displays |
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2008
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6284382B1 (en) * | 1997-11-27 | 2001-09-04 | Sony Corporation | Antireflection film and manufacturing method thereof |
| CN1729310A (en) * | 2002-11-01 | 2006-02-01 | 艾利丹尼森公司 | Transparent conductive film for flat panel displays |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2006-32100A 2006.02.02 |
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