KR20160116614A - Special chemical oxidizing agent for PEDOT-PSS conductive film with excellent oxidation stability and method for patterning conductivity of PEDOT-PSS conductive film using the oxidizing agent - Google Patents

Special chemical oxidizing agent for PEDOT-PSS conductive film with excellent oxidation stability and method for patterning conductivity of PEDOT-PSS conductive film using the oxidizing agent Download PDF

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KR20160116614A
KR20160116614A KR1020150044591A KR20150044591A KR20160116614A KR 20160116614 A KR20160116614 A KR 20160116614A KR 1020150044591 A KR1020150044591 A KR 1020150044591A KR 20150044591 A KR20150044591 A KR 20150044591A KR 20160116614 A KR20160116614 A KR 20160116614A
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양동연
김현
심원섭
조경인
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Abstract

The present invention relates to a chemical special oxidizer for a PEDOT-PSS conductive film containing 2.0-15.0 wt% of a sodium hypochlorite (NaOCl) aqueous solution in which a concentration of sodium hypochlorite (NaOCl) is 2.0-20.0%, 0.1-15.0 wt% of a potassium-based compound, 0.1-5.0 wt% of a pH adjusting agent indicating acidity, and 70.0-97.5 wt% of a solvent; and a conductive patterning method of a PEDOT-PSS conductive film using the same. According to the present invention, as a PEDOT-PSS conductive film is exposed to a chemical special oxidizer to lose conductivity in a chemical manner not physical corrosion, a change in optical properties such as a color difference before/after oxidation is reduced, whereby a shape of the pattern is not clear. In addition, the oxidation time for forming a conductive pattern is short within 1 minute, and excellent oxidation stability for being lasted about 30 days is obtained.

Description

TECHNICAL FIELD [0001] The present invention relates to a PEDOT-PSS conductive film, a PEDOT-PSS conductive film, and a PEDOT-PSS conductive film. conductive film using the oxidizing agent}

The present invention relates to a chemical special oxidizer for a PEDOT-PSS conductive film having excellent oxidation stability and a conductive patterning method of a PEDOT-PSS conductive film using the same. More particularly, the present invention relates to a transparent electrode material having excellent transparency, To a chemical special oxidizer for PEDOT-PSS conductive film which can be used in a chemical oxidation process for the conductive patterning of a PEDOT-PSS conductive film and a conductive patterning method of the PEDOT-PSS conductive film using the same.

Electronic communication devices are becoming increasingly smaller and lighter due to the rapid development of consumer needs and technologies, and there is a demand for devices with various functions in addition to flexibility.

To fabricate flexible electronic devices such as flexible displays, transistors, touch panels, solar cells, etc., transparent and flexible electrodes must be used, such as polyethylene terephthalate, polyethersulfone (PES), and triacetyl cellulose (TAC), which are required to have high conductivity and excellent visible light transmittance in the visible region.

Flexible materials that can be used as next-generation transparent electrodes include conductive polymers, transparent conducting oxides (TCO), silver nanowires, carbon nanotubes (CNT), graphene ) Have been actively researched. Currently, the most commonly used transparent electrode is indium tin oxide (ITO) film. However, ITO films have several disadvantages in the use of flexible materials in future electronic devices. In order to overcome the disadvantages of ITO film and to replace ITO film, research on next generation transparent electrode has been proceeding with competition of the future display industry.

In addition, a method of forming a transparent electrode film to improve the economical efficiency of the manufacturing process and the production yield, is a method of forming a transparent electrode film by using inkjet printing, spraying, gravure, Studies have been actively conducted to fabricate a transparent electrode by applying a roll-to-roll coating process such as a slot-die coating or the like.

For the transparent electrode film to be applied to the touch panel of the display, a patterning process of an electrode is required in most cases. In the patterning process of the conductive polymer, it is necessary to impart appropriate processability to the conductive polymer, and it is required that the polymer in the non-patterned portion after the patterning has a small change in electric or optical properties. It is an important point to consider. In addition, for industrial application, it is required to secure an oxidizing agent having excellent long-term stability of oxidation, not a workability and a temporary oxidation performance with an oxidation time of less than one minute.

Korean Patent Publication No. 10-2012-0077112

A problem to be solved by the present invention is to expose a PEDOT-PSS conductive film to a chemical special oxidant to lose chemical conductivity, not physical corrosion, thereby reducing variations in optical characteristics such as color difference before and after oxidation, And a method of forming a conductive pattern of a PEDOT-PSS conductive film using the same, wherein the oxidizing time is as short as one minute or less and the oxidation stability is about 30 days for forming a conductive pattern.

The present invention relates to an aqueous sodium hypochlorite solution, which comprises 2.0 to 15.0% by weight of sodium hypochlorite (NaOCl) aqueous solution having a concentration of sodium hypochlorite (NaOCl) of 2.0 to 20.0%, 0.1 to 15.0% And 70.0 to 97.5% by weight of a solvent. The present invention also provides a chemical special oxidizing agent for a PEDOT-PSS conductive film.

The sodium hypochlorite (NaOCl) aqueous solution is preferably an aqueous solution having an effective chlorine concentration of 500 to 10,000 ppm.

The potassium-based compound can be used in combination with one or more compounds selected from the group consisting of potassium chloride (KCl), potassium fluoride (KF), potassium fluoride (KHF 2 ), potassium bromide (KBr), potassium iodide (KI), potassium azide (KN 3 ) KNH 2), potassium oxide (K 2 O), potassium hydroxide (KOH), potassium peroxide (K 2 O 2), potassium carbonate (K 2 CO 3), potassium nitrate (KNO 3), potassium sulfate (K 2 SO 4 ) And potassium chromate (K 2 Cr 2 O 7 ).

The pH adjusting agent may include at least one substance selected from hydrochloric acid (HCl), nitric acid (HNO 3 ), acetic acid (CH 3 COOH), formic acid (HCOOH) and citric acid (C 6 H 8 O 7 ).

The pH of the chemical special oxidizing agent is preferably 3.5 to 6.0.

It is preferable that the solvent includes distilled water.

(B) selectively exposing the photoresist using a mask; and (c) selectively exposing the selectively exposed photoresist using a mask. (D) selectively oxidizing the exposed PEDOT-PSS conductive film using the chemical special oxidizing agent according to claim 1; and (e) exposing the exposed PEDOT-PSS conductive film to a chemical oxidizing agent. Wherein the PEDOT structure is chemically changed in the PED conductive film to lose conductivity, and (f) removing the remaining photoresist pattern to obtain a selectively oxidized PEDOT-PSS conductive film. A method of conductive patterning of a PSS conductive film is provided.

The PEDOT-PSS conductive film in step (a) preferably has a surface resistance of 20 to 4000? / ?, and the PEDOT-PSS conductive film part not exposed to the chemical special oxidant has a surface of 20 to 4,000? Resistance.

The oxidized PEDOT-PSS conductive film portion exposed to the chemical special oxidizing agent may have a surface resistance of 10 9 to 10 13 Ω / □.

According to the present invention, the PEDOT-PSS conductive film is exposed to a chemical special oxidizing agent to lose chemical conductivity, not physical corrosion, thereby reducing variations in optical characteristics such as color difference before and after oxidation, . Even when exposed to a chemical special oxidizing agent, the PEDOT-PSS conductive film does not deteriorate the distinctive blue hue, so the color difference is small and visibility is excellent.

The chemical special oxidizing agent of the present invention can be used in a chemical oxidation process for the conductive patterning of conductive PEDOT-PSS conductive film having excellent transparency and transparency in the next generation transparent electrode material and forms a conductive pattern of PEDOT-PSS conductive film And the oxidation stability is as good as about 30 days.

In addition, the use of the chemical special oxidizing agent of the present invention is advantageous in that the conductive patterning process of the PEDOT-PSS conductive film is convenient and can be performed at low cost.

1 is a cross-sectional view illustrating a conductive patterning method of a PEDOT-PSS conductive film.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, it should be understood that the following embodiments are provided so that those skilled in the art will be able to fully understand the present invention, and that various modifications may be made without departing from the scope of the present invention. It is not.

PEDOT [Poly (3,4-Ethylene Dioxythiophene)] - PSS [Poly (Styrene Sulfonate)] It is better to judge the stability of the chemical special oxidizer in the patterning process of the conductive film as the persistence of oxidation rather than precipitation.

When the oxidation time is about 20 minutes, the productivity lowers. When the oxidation stability is as short as about 5 days, it is time-limited to apply to the patterning process requiring oxidation stability for two weeks or more. ≪ / RTI >

The present invention provides a chemical special oxidizing agent for PEDOT-PSS conductive film excellent in oxidation stability. Since the PEDOT-PSS conductive film does not inhibit the peculiar blue color of the conductive film even after exposure to the chemical special oxidizing agent, the color difference is small and the visibility is excellent, the oxidation time is short within 1 minute, the oxidation stability is excellent over 30 days, The micro-conductive patterning of the stable PEDOT-PSS highly conductive film can be realized.

The chemical special oxidant for a PEDOT-PSS conductive film according to a preferred embodiment of the present invention comprises 2.0 to 15.0% by weight of an aqueous solution of sodium hypochlorite (NaOCl) having a concentration of sodium hypochlorite (NaOCl) of 2.0 to 20.0% To 15.0 wt%, 0.1 to 5.0 wt% of a pH adjusting agent showing acidity, and 70.0 to 97.5 wt% of a solvent.

The sodium hypochlorite (NaOCl) aqueous solution is preferably an aqueous solution having an effective chlorine concentration of 500 to 10,000 ppm.

The potassium-based compound can be used in combination with one or more compounds selected from the group consisting of potassium chloride (KCl), potassium fluoride (KF), potassium fluoride (KHF 2 ), potassium bromide (KBr), potassium iodide (KI), potassium azide (KN 3 ) KNH 2), potassium oxide (K 2 O), potassium hydroxide (KOH), potassium peroxide (K 2 O 2), potassium carbonate (K 2 CO 3), potassium nitrate (KNO 3), potassium sulfate (K 2 SO 4 ) And potassium chromate (K 2 Cr 2 O 7 ).

The pH adjusting agent may include at least one substance selected from hydrochloric acid (HCl), nitric acid (HNO 3 ), acetic acid (CH 3 COOH), formic acid (HCOOH) and citric acid (C 6 H 8 O 7 ).

The pH of the chemical special oxidizing agent is preferably 3.5 to 6.0.

It is preferable that the solvent includes distilled water.

 The conductive patterning method of a PEDOT-PSS conductive film according to a preferred embodiment of the present invention includes the steps of: (a) applying a photoresist on a PEDOT-PSS conductive film and drying the conductive film; and (b) Selectively exposing the resist to light; (c) immersing the selectively exposed product in a developing solution; and (d) selectively exposing the PEDOT-PSS conductive film using the chemical specialty oxidizing agent of claim 1 (E) chemically changing the PEDOT structure in the PEDOT-PSS conductive film exposed to the chemical special oxidant to lose conductivity, and (f) removing the remaining photoresist pattern to selectively oxidize the PEDOT- -PSS < / RTI > conductive film.

The PEDOT-PSS conductive film in the step (a) preferably has a surface resistance of 20 to 4000? / ?.

The oxidized PEDOT-PSS conductive film portion exposed to the chemical special oxidizing agent may have a surface resistance of 10 9 to 10 13 Ω / □.

Hereinafter, a chemical special oxidizer for a PEDOT-PSS conductive film according to a preferred embodiment of the present invention and a conductive patterning method of the PEDOT-PSS conductive film using the same will be described in more detail.

The chemical special oxidizing agent for a PEDOT-PSS conductive film according to a preferred embodiment of the present invention includes an aqueous sodium hypochlorite (NaOCl) solution, a potassium-based compound, a pH adjusting agent exhibiting acidity and a solvent.

The sodium hypochlorite (NaOCl) aqueous solution is an aqueous solution having a sodium hypochlorite (NaOCl) concentration of 2.0 to 20.0%, more preferably 5.0 to 12.0%. The effective chlorine concentration of the sodium hypochlorite (NaOCl) aqueous solution is preferably 500 to 10,000 ppm (mg / l). The aqueous solution of sodium hypochlorite (NaOCl) is decomposed with time due to its nature and changes to chlorine (Cl 2 ) gas form, so its stability is poor. In particular, since the stability of ultraviolet light (ultraviolet light) and high temperature is deteriorated rapidly, effective chlorine concentration varies depending on the time of preparation and storage state of sodium hypochlorite (NaOCl) aqueous solution.

The sodium hypochlorite (NaOCl) aqueous solution as described above is preferably contained in the chemical special oxidizing agent in an amount of 2.0 to 15.0% by weight, more preferably 3.5 to 10.0% by weight. When the content of the sodium hypochlorite (NaOCl) %, The oxidation performance may be deteriorated. If the content of the sodium hypochlorite (NaOCl) aqueous solution is higher than 15.0% by weight, the pattern shape after oxidation is clearly visible.

The potassium-based compound used in the present invention is a compound in which an element of negative +1 potassium ion and negative ion forms an ionic crystal. Most of the compound is soluble in water and completely ionized in an aqueous solution into anion of potassium ion and acid.

Examples of the potassium compound include potassium chloride (KCl), potassium fluoride (KF), potassium fluoride (KHF 2 ), potassium bromide (KBr), potassium iodide (KI), potassium azide (KN 3 ) KNH 2), potassium oxide (K 2 O), potassium hydroxide (KOH), potassium peroxide (K 2 O 2), potassium carbonate (K 2 CO 3), potassium nitrate (KNO 3), potassium sulfate (K 2 SO 4 ), Potassium dichromate (K 2 Cr 2 O 7 ) or a mixture thereof, and more preferably KCl (potassium chloride), K 2 CO 3 (potassium carbonate), KNO 3 (potassium nitrate) .

The potassium-based compound is preferably contained in the chemical specialty oxidizing agent in an amount of 0.1 to 15.0% by weight, more preferably 0.5 to 10.0% by weight. By containing the potassium-based compound in an amount of 0.1 to 15.0 wt%, the oxidizing property and the oxidation stability of the chemical special oxidizing agent for the PEDOT-PSS conductive film can be improved.

It is preferable to use an acid as the pH regulator. The pH adjusting agent may include hydrochloric acid (HCl), nitric acid (HNO 3 ), acetic acid (CH 3 COOH), formic acid (HCOOH), citric acid (C 6 H 8 O 7 ) or a mixture thereof. The acid may be in the form of a solution, and the acid solution in the form of a solution may be commercially available. For example, a hydrochloric acid solution having a hydrochloric acid concentration of 35.0% may be used, or a nitric acid solution having a nitric acid concentration of 60.0% may be used, or an acetic acid solution having an acetic acid concentration of 99.5% may be used. The pH adjusting agent is preferably contained in the chemical specialty oxidizing agent in an amount of 0.1 to 5.0% by weight, more preferably 0.5 to 3.0% by weight. It is preferable that the pH of the chemical special oxidizing agent is adjusted to about 3.5 to 6.0 by the pH adjusting agent. If the pH is lower than 3.5, the initial oxidation property may be lowered, and if the pH is higher than 6.0, the oxidation stability may be lowered.

The solvent is not particularly limited, and may be distilled water (H 2 O) or the like. The solvent is preferably contained in the chemical special oxidizing agent in an amount of 70.0 to 97.5% by weight, more preferably 75.0 to 95.0% by weight.

The above-mentioned chemical special oxidant can reduce the change of optical characteristics before and after the chemical oxidation for the PEDOT-PSS conductive film, so that the shape of the oxidized pattern can be made invisible, and the oxidation time for obtaining the pattern of the desired shape is 1 Minute, and the oxidation stability is excellent as about 30 days.

The conductive patterning method of the PEDOT-PSS conductive film (the method of selectively oxidizing the PEDOT-PSS conductive film) can utilize a photolithography process. 1 is a cross-sectional view illustrating a conductive patterning method of a PEDOT-PSS conductive film.

Referring to FIG. 1, photoresist is applied on a PEDOT-PSS conductive layer to dry the PEDOT-PSS conductive layer. The PEDOT-PSS conductive film may be formed on a substrate. The substrate may be a transparent substrate made of transparent PET (polyethylene terephthalate), PES (polyethersulfone), TAC (triacetyl cellulose), or the like. In the case of a positive photoresist, the portion to be exposed is removed and the portion where light is blocked by the shielding layer such as chrome (Cr) of the mask and is not exposed (non-exposure treatment) remains. The non-exposure process means that the photoresist pattern is left after the development so that light can not be transmitted by being shielded by the shielding layer of the mask in the exposure process. It is of course also possible to use a negative photoresist. In the case of a negative photoresist, light is blocked by a shielding layer such as chromium (Cr) in the mask, so that the unexposed portion is removed and the exposed portion remains.

A mask is used to selectively expose the photoresist (UV light exposure). The mask is a mask formed with a shielding layer defining an area to be oxidized in the PEDOT-PSS conductive film. The photoresist in the portion having no shielding layer is exposed to ultraviolet rays, and the remaining portion is shielded from ultraviolet rays by a shielding layer such as chromium (Cr) in the mask, thereby preventing exposure.

The selectively exposed product is immersed and developed in a developing solution. The photoresist is selectively removed by the development to form a photoresist pattern. As the developer, a developer that is commercially available and widely used in a semiconductor manufacturing process can be used. When a positive photoresist is used, the exposed portion is removed, and when a negative photoresist is used, the unexposed portion is removed. 1 is a view showing a case where a negative photoresist is used. The PEDOT-PSS conductive film is selectively exposed through the photoresist pattern.

The exposed PEDOT-PSS conductive film is selectively oxidized using the above-described chemical special oxidizing agent. The PEDOT-PSS conductive film protected by the photoresist pattern is not oxidized because it does not directly contact the chemical special oxidizer, and the PEDOT-PSS conductive film not protected by the photoresist pattern is in direct contact with the chemical special oxidant Oxidation is carried out.

The structure of the PEDOT: PSS conductive film is shown in the following structural formula 1.

[Structural formula 1]

Figure pat00001

The following structural formula 2 shows a chemical oxidation reaction mechanism.

[Structural formula 2]

Figure pat00002

PEDOT: When PSS conductive film is exposed to a chemical special oxidizing agent, oxidation occurs in the PEDOT part.

As the oxidation progresses, the PEDOT structure is chemically changed by over-oxidation and the conductivity is lost. In the PEDOT-PSS conductive film exposed to the chemical special oxidizing agent, the PEDOT structure is chemically changed to lose conductivity.

The remaining photoresist pattern is removed using a stripping process or the like to obtain a selectively oxidized PEDOT-PSS conductive film. Since the step of removing the photoresist pattern is a well-known process in a semiconductor manufacturing process or the like, a detailed description thereof will be omitted here.

The conductive patterning of the PEDOT-PSS conductive film of the PEDOT-PSS conductive film described above results in conductive patterning. The conductive PEDOT-PSS conductive film portion exposed to the chemical special oxidizing agent has a surface resistance of 10 < 9 > 10 13 Ω / □, and the PEDOT-PSS conductive film portion not exposed to the chemical special oxidizing agent has a surface resistance of 20 to 4000 Ω / □.

The conductive patterning method of the PEDOT-PSS conductive film described above is advantageous in that it can be applied to existing photolithography equipment without the investment of new equipment by applying the PEDOT-PSS conductive film and the chemical special oxidizing agent.

Hereinafter, the present invention will be described in more detail by way of examples and comparative examples. However, the following examples and comparative examples are for illustrative purposes only and are not intended to limit the present invention. It is to be noted that the comparative examples described below are provided merely for comparison with the characteristics of the embodiments, and are not the prior art of the present invention.

1) Manufacture of PEDOT-PSS conductive film

A conductive polymer doped with PSS [Poly (Styrene Sulfonate)] to PEDOT [Poly (3,4-Ethylene dioxythiophene)], Methanol (Methanol), Ethanol (Ethanol), N-Methylacetamide And a crosslinking agent were added and stirred at a speed of 500 rpm for 60 minutes to prepare a PEDOT-PSS conductive coating solution. Amino propyl triethoxy silane was used as the silane coupling agent. The crosslinking agent was aziridine crosslinking agent CX-100 (DSM, Neoresin).

The PEDOT-PSS conductive coating solution was coated on a PET (polyethylene terephthalate) film and cured in an oven (hot air) at about 120 ° C for about 3 minutes to prepare a PEDOT-PSS conductive film. The PEDOT-PSS conductive film had a thickness of 1 탆 or less, and a surface resistance of 20 to 4,000 Ω / □ could be achieved depending on the thickness of the PEDOT-PSS conductive film.

The conductive film used for the evaluation of the oxidative property and the oxidation stability was generally tested on the basis of a high-conductivity film of 150? /? Which is a typical surface resistance of an ITO film applied to a C-type (capacitance type) in a transparent electrode film.

2) Manufacture of chemical special oxidizing agent for PEDOT-PSS conductive film

As shown in the following Table 1, the composition and the content range of the examples were used to prepare a chemical special oxidizing agent for the PEDOT-PSS conductive film.

In the examples of the following Table 1, chemical special oxidizing agents for PEDOT-PSS conductive films were prepared by varying kinds and contents of sodium hypochlorite (NaOCl) aqueous solution, potassium compound, pH adjusting agent and distilled water. In comparative examples, Sodium (NaOCl) aqueous solution, pH adjuster and distilled water were prepared by varying kinds and contents of oxidants.

Using the 150 Ω / □ PEDOT-PSS conductive film, the oxidation and oxidation stability and the pattern visibility were evaluated by the compositions of the examples and comparative examples shown in Table 1.

2) Evaluation of Oxidation and Oxidation Stability

PEDOT-PSS conductive films were selectively oxidized by photolithography using the chemical special oxidants prepared according to the examples shown in Table 1 and the oxidants prepared according to the comparative examples to evaluate the oxidative and oxidative stability.

Specific oxidative and oxidative stability evaluations were carried out by applying a photoresist to the PEDOT-PSS conductive film to a thickness of about 2 μm and drying at a temperature of 100 ° C. for 1 minute. The photoresist was selectively exposed using a mask and developed with a developing solution to form a photoresist pattern. The photoresist pattern was used as a mask to expose the photoresist pattern to the chemical special oxidizing agent prepared in Examples and Comparative Examples to form PEDOT-PSS conductive The film was selectively oxidized. A photoresist pattern was removed using a stripping process. The selectively oxidized PEDOT-PSS conductive film was washed with distilled water, completely dried, and the surface resistance after oxidation was measured to confirm the oxidizing property.

The surface resistance before oxidation was measured using a low resistance meter (LORESTA-GP MCP-T610, Mitsubishi Chemical Co.), and the surface resistance after oxidation was measured with a high resistance meter (Monore -291, Momore). When the surface resistance after the oxidation reached the range of 10 9 to 10 13 Ω / □, it was judged to be oxidized, and evaluated as O, Δ, and X according to the oxidation time.

In addition, the oxidation stability was evaluated by observing the chemical special oxidizing agent for the PEDOT-PSS conductive film prepared according to the examples shown in Table 1 and the oxidizing agent prepared according to the comparative examples at room temperature for 5 days, The oxidative properties were evaluated according to the oxidation time.

○: 1 minute or less

△: more than 1 minute to less than 3 minutes

X: over 3 minutes

3) Pattern visibility

The pattern visibility was measured before and after the PEDOT-PSS conductive film was exposed to the chemical special oxidizer, and the transmittance at a wavelength of 550 nm was measured using a UV-Spectrometer (CM-3500d, Minolta Co.) And b * values, which are closely related to each other, were defined as good and bad according to Δb * as follows.

In addition, since the pattern visibility deteriorates with time as the oxidative property is deteriorated, the pattern visibility does not deteriorate even if the initial pattern visibility is good. Therefore, the pattern visibility was measured only once at the initial stage.

? B * < 1.5: good (pattern is not visible)

△ b *> 1.5: poor (pattern is visible)

Chemical special oxidizer NaOCl aqueous solution
(weight%) Potassium-based compound
(weight%) pH adjusting agent
(weight%) menstruum
(weight%) Comparative Example 1 NaOCl aqueous solution
(5.0) HCl (0.7) H 2 O (94.3) Comparative Example 2 NaOCl aqueous solution
(5.5) HCl (1.0) H 2 O (93.5) Comparative Example 3 NaOCl aqueous solution
(6.5) HCl (1.3) H 2 O (92.2) Comparative Example 4 NaOCl aqueous solution
(7.0) HCl (1.4) H 2 O (91.6) Comparative Example 5 NaOCl aqueous solution
(11.0) HCl (2.5) H 2 O (86.5) Comparative Example 6 NaOCl aqueous solution
(7.0) HNO 3 (2.0) H 2 O (91.0) Comparative Example 7 NaOCl aqueous solution
(7.0) CH 3 COOH (2.0) H 2 O (91.0) Example 1 NaOCl aqueous solution
(7.0) KCl (3.0) HCl (1.4) H 2 O (88.6) Example 2 NaOCl aqueous solution
(7.0) K 2 CO 3 ( 3.0) HCl (1.4) H 2 O (88.6) Example 3 NaOCl aqueous solution
(7.0) KCl (1.0), K 2 CO 3 (2.0) HCl (1.4) H 2 O (88.6) Example 4 NaOCl aqueous solution
(7.0) KCl (1.0) KNO3 ( 2.0) HCl (1.4) H 2 O (88.6) Example 5 NaOCl aqueous solution
(7.0) KCl (3.0) HCl (1.0) H 2 O (89.0) Example 6 NaOCl aqueous solution
(7.0) KCl (3.0) HCl (0.8) H 2 O (89.2) Example 7 NaOCl aqueous solution
(7.0) KCl (1.0), K 2 CO 3 (2.0) HCl (0.8) H 2 O (89.2) NaOCl aqueous solution: An aqueous solution having a sodium hypochlorite (NaOCl) concentration of 11.5%
HCl: hydrochloric acid solution having a concentration of hydrochloric acid of 35.0%
HNO 3 : nitric acid solution having a nitric acid concentration of 60.0%
CH 3 COOH: Acetic acid solution with acetic acid concentration of 99.5%
KCl: potassium chloride solution having a concentration of potassium chloride of 99.0%
K 2 CO 3 : Potassium carbonate solution with a concentration of potassium carbonate of 99.0%

The measured oxidative, oxidative stability and pattern visibility results are shown in Table 2 below.

Chemical special oxidizer Oxidation and oxidation stability Pattern visibility Early 5 days 10 days 15th 20 days 25th 30 days Comparative Example 1 O △ X Good Comparative Example 2 O △ △ X Good Comparative Example 3 O O O △ X Good Comparative Example 4 O O O O △ X Good Comparative Example 5 O O O O O O O Bad Comparative Example 6 O O △ △ X Good Comparative Example 7 O △ △ X Good Example 1 O O O O O O O Good Example 2 O O O O O O O Good Example 3 O O O O O O O Good Example 4 O O O O O O O Good Example 5 O O O O O O O Good Example 6 O O O O O O O Good Example 7 O O O O O O O Good

The oxidants prepared according to the comparative examples showed poor oxidative and oxidative stability or bad pattern visibility, whereas the chemical specialty oxidants prepared according to the examples had excellent oxidative and oxidative stability and good pattern visibility appear.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, This is possible.

Claims (9)

2.0 to 15.0% by weight of sodium hypochlorite (NaOCl) aqueous solution having a sodium hypochlorite (NaOCl) concentration of 2.0 to 20.0%;
0.1 to 15.0% by weight of a potassium compound;
0.1 to 5.0% by weight of a pH adjusting agent exhibiting acidity; And
PEDOT-PSS < / RTI > conductive film. ≪ RTI ID = 0.0 > 11. < / RTI >
The chemical special oxidant for PEDOT-PSS conductive film according to claim 1, wherein the sodium hypochlorite (NaOCl) aqueous solution is an aqueous solution having an effective chlorine concentration of 500 to 10,000 ppm.
The method of claim 1 wherein the potassium compound is potassium chloride (KCl), potassium fluoride (KF), Fluorine hydrogen potassium (KHF 2), potassium bromide (KBr), potassium iodide (KI), azide, potassium (KN 3 ), Potassium amide (KNH 2 ), potassium oxide (K 2 O), potassium hydroxide (KOH), potassium peroxide (K 2 O 2 ), potassium carbonate (K 2 CO 3 ), potassium nitrate (KNO 3 ) (K 2 SO 4 ) and potassium chromate (K 2 Cr 2 O 7 ). The chemical specialty oxidant for a PEDOT-PSS conductive film is characterized in that it comprises at least one substance selected from the group consisting of potassium (K 2 SO 4 ) and potassium chromate (K 2 Cr 2 O 7 ).
The method of claim 1, wherein the pH adjusting agent comprises at least one substance selected from the group consisting of hydrochloric acid (HCl), nitric acid (HNO 3 ), acetic acid (CH 3 COOH), formic acid (HCOOH) and citric acid (C 6 H 8 O 7 ) Wherein the PEDOT-PSS conductive film is a PEDOT-PSS conductive film.
The chemical special oxidant for PEDOT-PSS conductive film according to claim 1, wherein the pH of the chemical special oxidant is 3.5 to 6.0.
The chemical special oxidizing agent for PEDOT-PSS conductive film according to claim 1, wherein the solvent comprises distilled water.
(a) applying and drying a photoresist on a PEDOT-PSS conductive film;
(b) selectively exposing the photoresist using a mask;
(c) selectively immersing the exposed resultant in a developing solution to develop;
(d) selectively oxidizing the exposed PEDOT-PSS conductive film using the chemical special oxidizing agent according to claim 1;
(e) chemically changing the PEDOT structure in the PEDOT-PSS conductive film exposed to the chemical special oxidant to lose conductivity; And
(f) removing the remaining photoresist pattern to obtain a selectively oxidized PEDOT-PSS conductive film. < RTI ID = 0.0 > 11. < / RTI >
The method of claim 7, wherein the PEDOT-PSS conductive film of step (a) has a surface resistance of 20 to 4000? /?
Wherein the PEDOT-PSS conductive film portion not exposed to the chemical special oxidizer has a surface resistance of 20 to 4000? / ?.
The conductive patterning method of claim 7, wherein the PEDOT-PSS conductive film portion exposed to the chemical special oxidizing agent has a surface resistance of 10 9 to 10 13 Ω / □.
KR1020150044591A 2015-03-30 2015-03-30 Special chemical oxidizing agent for PEDOT-PSS conductive film with excellent oxidation stability and method for patterning conductivity of PEDOT-PSS conductive film using the oxidizing agent KR101683477B1 (en)

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PCT/KR2016/003118 WO2016159605A1 (en) 2015-03-30 2016-03-28 Specific chemical oxidant for pedot-pss conductive film, having excellent oxidation stability, and method for patterning conductivity of pedot-pss conductive film by using same

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