CN103777799A - Method for forming transparent conducting layer on substrate - Google Patents
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- CN103777799A CN103777799A CN201210410586.XA CN201210410586A CN103777799A CN 103777799 A CN103777799 A CN 103777799A CN 201210410586 A CN201210410586 A CN 201210410586A CN 103777799 A CN103777799 A CN 103777799A
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Abstract
The invention provides a method for forming a transparent conducting layer on a substrate. The method comprises the steps that a conducting composition containing conducting polymer is exerted on the substrate so that the transparent conducting layer can be formed on the substrate; a patterning protective layer is formed on the transparent conducting layer so that a transparent conducting layer zone covered with the protective layer and a transparent conducting layer zone not covered with the protective layer can be defined; the transparent conducting layer zone not covered with the protective layer is etched in a wet type; the protective layer is removed and the transparent conducting layer is annealed before or after the wet-type etching operation. According to the method for forming the transparent conducting layer on the substrate, chromatic aberration generated between the etched portion of the transparent conducting layer and the non-etched portion of the transparent conducting layer can be reduced; due to the fact that the chromatic aberration does not need to be reduced through an extra optical layer, compared with a traditional method, the method is simple, convenient to use and good in economic benefit.
Description
Technical field
The present invention relates to a kind of method that forms transparency conducting layer on substrate.
Background technology
In recent years, use for the convenience of the user electronic product, the contact panel of signal being inputted to electronic product by contact screen is widely used.The development of touch technology is maked rapid progress, and at present, according to the difference of method for detecting position, contact panel roughly comprises optical mode, ultrasound wave mode, static capacity mode, resistive film mode etc.The contact panel of resistance/static capacity mode be configured to transparency conducting layer with configured by sept (spacer) subtend with the glass of transparency conducting layer.The contact panel of static capacity mode needs on demand sometimes by pattern for transparent conductive layer.Generally to utilize the mode of lithography by pattern for transparent conductive layer, but, transparency conducting layer after etching, described through etching remove transparency conducting layer place with without etching remove transparency conducting layer place between can generation thickness difference; And etching meeting destroys the electrical of conductive layer, this thickness difference all can make the optical property (as absorption, reflection etc.) of transparency conducting layer change with electrical destruction, and causes aberration to become obviously, just the outward appearance defectiveness of contact panel.Especially,, for the contact panel of static capacity mode, because transparency conducting layer is positioned at light entrance face side, described apparent defect can be more obvious.
Prior art proposes for the method for utilizing dry type sputtered indium tin oxide (ITO) to manufacture transparent conducting film the scheme addressing the aforementioned drawbacks, it is to utilize between transparency conducting layer and base material, to form at least one deck undercoat, to improve its optical property (No. I346046th, Republic of China's patent), but this method needs the extra undercoat that adds.
Other technology of utilizing dry type sputtering way to form transparency conducting layer for example comprises: Japanese Patent 4364938, TOHKEMY 2011-17795; Other technology of utilizing wet type coating method to form transparency conducting layer for example comprises: TOHKEMY 2011-44145, TOHKEMY 2003-80624 and US 7,083,851, these patents all need to utilize extra optical layers, and (these patents are all utilized two-layer optical layers, d1 and d2), solve the aberration problem that the transparency conducting layer thickness difference that causes because of etching produces.But it can increase technologic difficulty, and its effect of improving outward appearance is still limited; Also easily have the problem of embrittlement using ITO as conductive membrane, and process costs is higher.
In recent years, due to the lifting of conducting polymer aspect electrically with in the improvement aspect processability, its economic benefit obtains attention gradually.
US 2011/0059232 just discloses a kind of utilization and comprises polyase 13, and the organic conductive composition of 4-ethylidene dioxy base thiophene (PEDOT)/PSS (PSS) forms the method for transparent organic electrode; Ai Kefa (Agfa) also proposes a kind of mode (advanced material (Adv.Mater.) 2006,18,1307-1312 that utilizes lithography patterning for conducting polymer; With large molecule wall bulletin (Macromol.Rapid Commun.) 2005,26,238-246); But, conductive polymer applications also can be produced to the problem of the aberration producing as the aforementioned thickness difference because of transparency conducting layer (as because of the etch process patterning person of causing) in transparency conducting layer, and the not good problem of product appearance causing because of described aberration.Adjust the refractive index of blooming by adding the mode of optical layers although there are at present many technology, for example reduce in the mode of adding optical cement (OCA glue) the aberration problem that line pattern is caused, but its production run needs many one technique, and the space that is still improved of its optical property.
In view of above-mentioned, in industry, still need to seek a kind of method that improves above-mentioned formation transparency conducting layer.
Summary of the invention
One object of the present invention is to provide a kind of method that forms transparency conducting layer on substrate, and it can solve at least one the problems referred to above.Particularly, an object of the present invention is to provide a kind of extra optical layers that do not need, just can reduce the method for the aberration problem producing after pattern for transparent conductive layer.
According to the present invention, the described method that forms transparency conducting layer on substrate comprises: the electrically conductive composition that comprises conducting polymer is put on to substrate, to form transparency conducting layer on described substrate; On described transparency conducting layer, form the protective seam of patterning, to define the transparency conducting layer district covering through described protective seam and the transparency conducting layer district covering without described protective seam; The transparency conducting layer district covering without protective seam is carried out to Wet-type etching; And remove described protective seam, wherein before or after Wet-type etching, described transparency conducting layer is carried out to annealing in process.
The method of formation transparency conducting layer of the present invention, can reduce the aberration of transparency conducting layer and adjacent domain.Particularly, reduce the optical property (as absorption, reflection etc.) causing because of transparency conducting layer difference in thickness traditionally and change the aberration causing.In addition, reduce aberration because the inventive method does not need to utilize extra optical layers, the inventive method is easier and compared with tool economic benefit.
Accompanying drawing explanation
Figure 1A shows an embodiment of the method for transparency conducting layer formed according to the present invention to 1C.
Embodiment
Below to illustrate that to 1C the present invention forms the specific embodiment of the method for transparency conducting layer by means of Figure 1A.
Figure 1A demonstration puts on the electrically conductive composition that comprises conducting polymer on substrate 4, to form transparency conducting layer 2 thereon.
Conducting polymer used in the present invention can be formed by the combination of the monomer of the group that selects free pyrroles (pyrrole), thiophene (thiophene), aniline (aniline) and composition thereof to form and its derivant, oligomer and its derivant or above-mentioned any material.
Described " oligomer " has cognitive in the technical field of the invention general significance herein, for example, refer to the compound being made up of limited aforementioned monomer.For instance, refer to dipolymer, trimer, tetramer or the pentamer etc. of the monomer that can produce conducting polymer.
The general significance of described " derivant of monomer " known to having in the technical field of the invention, for example, refers to the aforementioned monomer being substituted herein.
The general significance of described " derivant of oligomer " known to having in the technical field of the invention, for example, refers to the aforementioned oligomer being substituted herein.
For instance, " pyrroles " and " pyrroles's derivant " all refers to, after polymerization, can produce the monomer of the conducting polymer with similar pyrrole structure.
Can be used for azole derivatives of the present invention, for example, include but not limited to: 3-alkyl pyrroles, as 3-hexyl pyrroles; 3,4-dialkyl group pyrroles, as 3,4-dihexyl pyrroles; 3-alkoxy pyrroles, as 3-methoxyl pyrroles; And 3,4-dialkoxy pyrroles, as 3,4-dimethoxy pyrroles.
Can be used for thiophene derivant of the present invention, for example, include but not limited to: 3,4-ethylidene dioxy base thiophene and derivatives; 3-alkylthrophene, as 3-hexyl thiophene; And 3-alkoxy thiophene, as 3-methoxythiophene.
Can be used for anil of the present invention, for example, include but not limited to: 2-alkyl benzene amine, as 2-aminotoluene; And 2-alkoxyl aniline, as 2-aminoanisole.
According to a particular embodiment of the invention, the monomer using is 3,4-ethylidene dioxy base thiophene (poly-3,4-ethylenedioxythiophene, PEDOT) or derivatives thereof, for example, include but not limited to: 3,4-(1-alkyl) ethylidene dioxy base thiophene, as 3,4-(1-hexyl) ethylidene dioxy base thiophene.In the case, electrically conductive composition of the present invention can further comprise that PSS (polystyrene sulfonate, PSS) is to arrange in pairs or groups with PEDOT.
The amount of conducting polymer that the inventive method is used is restriction especially not.But, if obtain acceptable electric conductivity, the amount of described conducting polymer in composition be approximately 1 % by weight to approximately 50 % by weight, be preferably approximately 20 % by weight to approximately 30 % by weight.
Electrically conductive composition of the present invention can comprise solvent.The solvent can be used in the present invention is preferably selected from the solvent that can reach with described conducting polymer acceptable compatible effect.Described solvent can be the organic solvent of water (being preferably deionized water), organic solvent or mixed water.Organic solvent comprises: alcohols, as methyl alcohol, ethanol and isopropyl alcohol (IPA); Arene, as benzene, toluene and dimethylbenzene; Fat hydrocarbon, as hexane; And aprotic polar solvent, as DMF, dimethyl sulfoxide (DMSO), acetonitrile and acetone.Above-mentioned organic solvent can be used alone or merges use.Solvent preferably comprises at least one in water, alcohol organic solvent and aprotic polar solvent, and it preferably selects to comprise the potpourri of potpourri, ethanol and water and the potpourri of dimethyl sulfoxide (DMSO) and water of water, ethanol, dimethyl sulfoxide (DMSO), water and isopropyl alcohol.
Electrically conductive composition of the present invention can comprise cementing agent, in order to improve the cohesive force of electrically conductive composition of the present invention.Applicable cementing agent is known in the technical field of the invention cementing agent, for example, include but not limited to: the low-molecular-weight cementing agent of water dissolvable, the high molecular cementing agent of water dissolvable or its combination.
Electrically conductive composition of the present invention can comprise viscosity modifier, in order to regulate the viscosity of electrically conductive composition of the present invention, puts on substrate so that it is suitable in the mode of printing.If the viscosity of electrically conductive composition too by force or too, is all unsuitable for putting on substrate with mode of printing.Selecting of viscosity modifier is according to selected mode of printing.The mode of printing conductive composition for example comprises ink jet printing, wire mark, intaglio printing and offset printing.According to selected mode of printing, applicable viscosity modifier is known in the technical field of the invention viscosity modifier.
Electrically conductive composition of the present invention can comprise electric conductivity intensive (conductivity enhancer), in order to strengthen the electric conductivity of transparency conducting layer of the present invention.Applicable electric conductivity intensive can be in the technical field of the invention known electric conductivity intensive, for example dimethyl sulfoxide (DMSO).
Electrically conductive composition of the present invention can comprise stabilizing agent, in order to improve the stability of transparency conducting layer.Applicable stabilizing agent can be known in the technical field of the invention stabilizing agent, for example tannic acid, gallic acid or its combination.
There is no particular restriction for the material of substrate 4, and it can be made up of any material, as long as transparency conducting layer can be easily formed thereon.In addition, substrate 4 other element known to can comprising in the technical field of the invention itself, for example, measuring sensor, electrode wires or the optical layers etc. of capacitance variations while touching contact panel for measuring user's hand.If substrate of the present invention separately comprises an optical layers, transparency conducting layer so of the present invention can be formed thereon.According to purposes, substrate 4 can be made up of coloured or colourless material.In the time that substrate 4 is used as the display plane of display device, substrate 4 can be made up of transparent material.For instance, substrate 4 can be by for example polyethylene terephthalate (polyethylene terephthalate, PET), polycarbonate (polycarbonate), polycarbonate (polycarbonate), polymethylmethacrylate (polymethyl methacrylate), Polyethylene Naphthalate (polyethylene naphthalate, PEN), polyethersulfone (polyether sulfone, PES), cyclic olefin polymer (cyclic olefin polymer, and analog COC), glass, tempered glass) and analog form.
According to the present invention, transparent water white transparency, colored transparent, translucent, the coloured translucent and similar situation of comprising.
Described electrically conductive composition can be by known in the technical field of the invention any method, for example coating or print process and put on substrate 4, according to a concrete aspect of the present invention, be to put on substrate 4 by coating process, for example, include but not limited to the modes such as rotary coating (spin coating), line rod coating (bar coating), dipping formula coating (dip coating), slit coating (slot coating) or volume to volume coating (roll to roll coating).
With reference to Figure 1B, it is presented on transparency conducting layer 2 and forms patterned protective seam 6, to define the transparency conducting layer 2-A district covering through protective seam and the transparency conducting layer 2-B district covering without protective seam.The transparency conducting layer district 2-B covering without protective seam exposes follow-up transparency conducting layer and needs through etching, destroys electrical part.
Protective seam 6 can first for example, put on transparency conducting layer 2 with known in the technical field of the invention any method (coating or print process); according to a concrete aspect of the present invention; put on transparency conducting layer 2 with printing process; afterwards; recycle known in the technical field of the invention mode; for example light lithography etching (lithography and etching) mode patterning, or can utilize printing (for example wire mark) mode directly the protective seam of patterning 6 to be formed on transparency conducting layer 2.
The material of protective seam can obtain by known in the technical field of the invention mode; for example can be purchased from (the H.C.Starck GmbH of H.C. Starck GmbH & Co. KG of Ge Silaer; Goslar) (trade name: Clevios SET G, heat curing-type acryl resin).
According to one embodiment of present invention; next can first carry out chemical etching for the transparency conducting layer covering without protective seam; for example it is carried out to Wet-type etching so that described transparency conducting layer is electrically destroyed; make its surface impedance for example be greater than about 80M Ω; be preferably greater than about 100M Ω, or the transparency conducting layer district 2-B covering without protective seam is removed.The etching solution using is known in the technical field of the invention etching solution, for example, include but not limited to NaClO
3aqueous solution, KMnO
4aqueous solution etc.
As shown in Figure 1 C, protective seam just can manifest patterned transparency conducting layer 8 after removing.Protective seam can utilize known in the technical field of the invention mode to remove, and the mode of removing protective seam is relevant with its material.For example, can utilize NH
4oH removes the H.C. Starck GmbH & Co. KG purchased from Ge Silaer, the protective seam of commodity Clevios SET G by name.
Removing after protective seam, just carry out annealing in process for described patterned transparency conducting layer.Wherein said annealing in process is at approximately 65 ℃ to approximately 165 ℃, preferably in the temperature range between approximately 80 ℃ to approximately 150 ℃, carries out constant temperature and processes approximately 0.5 to approximately 2 hours, and preferably after approximately 1 hour, then mode cool to room temperature for example naturally to lower the temperature.In addition, removing after the step of described protective seam, the step of cleaning described layer at transparent layer with acid can be comprised in addition, for example, H can be utilized
2sO
4clean described layer at transparent layer.Described sour cleaning step can carry out before annealing in process.
According to another embodiment of the present invention, described annealing in process can be carried out chemical etching (Wet-type etching) is front, for example, after forming transparency conducting layer, before forming protective seam thereon, carry out annealing in process for not patterned transparency conducting layer.Wherein said annealing in process is at approximately 65 ℃ to approximately 165 ℃, preferably in the temperature range between approximately 80 ℃ to approximately 150 ℃, carries out constant temperature and processes approximately 0.5 to approximately 2 hours, and preferably after approximately 1 hour, then mode cool to room temperature for example naturally to lower the temperature.
Next on described transparency conducting layer, form again the protective seam of patterning; and carry out chemical etching for the transparency conducting layer covering without protective seam; for example it is carried out to Wet-type etching so that described transparency conducting layer is electrically destroyed; make its surface impedance for example be greater than about 80M Ω; be preferably greater than about 100M Ω, or the transparency conducting layer district covering without protective seam is removed.It forms the mode of patterning protective seam and carries out the mode of chemical etching as discussed previously.
Now further illustrate the present invention with following specific embodiment party face, but it is not used in the present invention is imposed any restrictions.
Example
Example 1
0.13 gram of tannic acid is dissolved in the 0.5% conductivity water solution of 20 grams of PEDOT:PSS (H.C. Starck GmbH & Co. KG of manufacturer: Ge Silaer) after (aqueous solution is containing 25%IPA), with No. 9 line rods, formula liquid is coated to PET base material ((Toyobo) A4300 spins in Japan) upper with formation transparency conducting layer., in wire mark mode protective seam (Clevios SET G, H.C. Starck GmbH & Co. KG of manufacturer: Ge Silaer) circuit be printed in transparency conducting layer on thereafter, then with etching solution (5%NaClO
3aqueous solution) carry out conductive layer and electrically destroy (surface impedance > 100M Ω).Afterwards, with 1.5%NH
4oH removes protective seam, then with 1%H
2sO
4acid is cleaned after conductive layer surface, and the high temperature oven that is positioned over approximately 150 ℃ is dried 1 hour, afterwards, takes out and naturally cool to room temperature.And compare with the blank assay result without high-temperature heat treatment, its result is as follows:
L*, a* and b* (CIELAB) are three basic coordinates of the colour model for describing the visible all colours of human eye, it represents respectively the brightness (L* of color, L*=0 refers to black and L*=100 represents white), position between redness/magenta and green (a* negative value represent green and pinkish red on the occasion of representing), and position between yellow and blueness (b* negative value represent blueness and yellow on the occasion of representing).
Even change in L*a*b* model is corresponding to the even change in aware colors.So relative perceived differences of any two colors in L*a*b*, can be by each color treatments is similar to for a point in (having three component: L*, a*, b*) three dimensions, and calculate the Euclidean distance Δ E (being often called " Delta E ") between them.
ΔE*＝[(ΔL*)
2+(Δa*)
2+(Δb*)
2]
1/2
Example 2
Reaction process and condition be as example 1, but etching solution is 5% the Clevios etching solution that uses H.C. Starck GmbH & Co. KG's manufacturing of Ge Silaer.Its result is as follows:
Example 3
Reaction process and condition are as example 2, but etching solution is to use 10% Clevios etching solution.Its result is as follows:
Example 4
Reaction process and condition be as example 3, but be positioned over the baking oven 1 hour of 80 ℃.
Example 5
Reaction process and condition be as example 3, but be positioned over the baking oven 240 hours of 80 ℃.The result of example 3 to 5 arranges as follows:
Example 6
0.13 gram of tannic acid is dissolved in the 0.5% conductivity water solution of 20 grams of PEDOT:PSS (H.C. Starck GmbH & Co. KG of manufacturer: Ge Silaer) after (aqueous solution is containing 25%IPA), with No. 9 line rods, formula liquid is coated to PET base material (A4300 spins in Japan) upper with formation transparency conducting layer.The high temperature oven that is positioned over approximately 150 ℃ toasts 1 hour, afterwards, takes out and naturally cool to room temperature to complete annealing in process.Thereafter; in wire mark mode by protective seam (Clevios SET G; H.C. Starck GmbH & Co. KG of manufacturer: Ge Silaer) circuit is printed on transparency conducting layer, then carries out conductive layer with etching solution (5% Clevios etching solution) and electrically destroy (surface impedance > 100M Ω).Afterwards, remove protective seam with 1.5%NH4OH, then clean after conductive layer surface with 1%H28O4 acid, its result is as follows:
Relatively can be found by example 6 and example 2, if carry out annealing in process before etching, also can effectively reduce Δ b* and Δ E*, can improve the aberration problem of transparency conducting layer, even better than the effect of carrying out annealing in process after etching.
Comparative example 1
0.13 gram of tannic acid is dissolved in the 0.5% conductivity water solution of 20 grams of PEDOT:PSS (H.C. Starck GmbH & Co. KG of manufacturer: Ge Silaer) after (aqueous solution is containing 25%IPA), with No. 9 line rods, formula liquid is coated to PET base material (A4300 spins in Japan) upper with formation transparency conducting layer., go out after circuit with laser-induced thermal etching thereafter, then be positioned over approximately 150 ℃ high temperature oven dry 1 hour.Its result is as follows:
Can be found by comparative example, the present invention is not suitable for physics/dry-etching mode.
From above result, with the blank assay comparison without annealing in process, the inventive method can effectively reduce Δ b* and Δ E*, improves the aberration problem of transparency conducting layer; In addition, because the inventive method does not need to utilize extra optical layers, reduce the not good problem of product appearance that causes of pattern for transparent conductive layer, its technique is easier and compared with tool economic benefit.
Claims (13)
1. a method that forms transparency conducting layer on substrate, it comprises:
The electrically conductive composition that comprises conducting polymer is put on substrate, to form transparency conducting layer on described substrate;
On described transparency conducting layer, form the protective seam of patterning, to define the transparency conducting layer district covering through described protective seam and the transparency conducting layer district covering without described protective seam;
The described transparency conducting layer district covering without protective seam is carried out to Wet-type etching; And
Remove described protective seam,
Wherein before or after Wet-type etching, carry out annealing in process for described transparency conducting layer.
2. method according to claim 1, wherein said electrically conductive composition is to be coated with or mode of printing puts on described substrate.
3. method according to claim 2, wherein said coating method is the freely group of following composition of choosing: rotary coating, the coating of line rod, the coating of dipping formula, slit coating and volume to volume coating.
4. method according to claim 1, the protective seam of wherein said patterning is to be formed on described transparency conducting layer in wire mark mode.
5. method according to claim 1 is wherein to make the surface impedance of the described transparency conducting layer covering without protective seam be greater than about 80M Ω to the step of carrying out Wet-type etching without the transparency conducting layer of protective seam covering.
6. method according to claim 1 is wherein to make the surface impedance of the described transparency conducting layer covering without protective seam be greater than about 100M Ω to the step of carrying out Wet-type etching without the transparency conducting layer of protective seam covering.
7. method according to claim 1, wherein, removing after the step of described protective seam, utilizes H
2sO
4clean described layer at transparent layer.
8. method according to claim 1, wherein said annealing in process is in the temperature range of approximately 65 ℃ to approximately 165 ℃, to carry out after constant temperature processes approximately 0.5 to approximately 2 hours, then cool to room temperature.
9. method according to claim 1, wherein said annealing in process is in the temperature range of approximately 80 ℃ to approximately 150 ℃, to carry out after constant temperature processes approximately 0.5 to approximately 2 hours, then cool to room temperature.
10. method according to claim 9, wherein said annealing in process is to carry out constant temperature at 150 ℃ to process 1 hour.
11. methods according to claim 1, wherein said annealing in process step is to carry out after the step that forms transparency conducting layer.
12. methods according to claim 11, wherein said annealing in process step is to carry out before the step that forms protective seam.
13. methods according to claim 1, wherein said electrically conductive composition further comprises tannic acid, gallic acid or its combination.
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|---|---|---|---|---|
| US6379569B1 (en) * | 1998-02-23 | 2002-04-30 | Saint-Gobain Vitrage | Process for etching a conductive layer |
| CN101359633A (en) * | 2007-07-30 | 2009-02-04 | 徐海生 | Manufacturing method of RFID chip |
| CN101807545A (en) * | 2010-03-22 | 2010-08-18 | 中国科学院上海微系统与信息技术研究所 | Diode and producing method of resistance converting storage |
| CN102707825A (en) * | 2011-03-28 | 2012-10-03 | Smk株式会社 | Touch panel glass substrate and method for manufacturing same |
-
2012
- 2012-10-24 CN CN201210410586.XA patent/CN103777799A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6379569B1 (en) * | 1998-02-23 | 2002-04-30 | Saint-Gobain Vitrage | Process for etching a conductive layer |
| CN101359633A (en) * | 2007-07-30 | 2009-02-04 | 徐海生 | Manufacturing method of RFID chip |
| CN101807545A (en) * | 2010-03-22 | 2010-08-18 | 中国科学院上海微系统与信息技术研究所 | Diode and producing method of resistance converting storage |
| CN102707825A (en) * | 2011-03-28 | 2012-10-03 | Smk株式会社 | Touch panel glass substrate and method for manufacturing same |
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Application publication date: 20140507 |