Polymerization fluid, method for producing the polymerization fluid, transparent film and transparent electrode made from the polymerization fluid

Patent metadata

Field	Value
Publication number	US-8927683-B2
Application number	US-201113582282-A
Country	US
Kind code	B2
Filing date	Mar 1, 2011
Priority date	Mar 1, 2010
Publication date	Jan 6, 2015
Grant date	Jan 6, 2015

Abstract

Disclosed is a polymerization fluid for electropolymerization which exhibits a reduced environmental burden and excellent economic efficiency and which can yield a conductive polymer film that has high conductivity and that is dense and highly transparent. The polymerization fluid includes at least one monomer selected from the group consisting of 3,4-disubstituted thiophenes which is dispersed as oil drops in surfactant-free water, and the polymerization fluid is transparent. The polymerization fluid can be produced by a method which includes: an addition step of adding the monomer to surfactant-free water to prepare a phase separation fluid where water and the monomer are phase-separated; a first dispersion step of irradiating the phase separation fluid with ultrasonic waves to make the monomer dispersed in the form of oil drops and thus prepare an opaque dispersion, and a second dispersion step of irradiating the opaque dispersion with ultrasonic waves having a frequency higher than that of the ultrasonic waves used in the first dispersion step to reduce the mean size of the oil drops of the monomer and thus prepare a transparent dispersion.

First claim

What is claimed is:

1. A polymerization fluid for electropolymerization of at least one monomer selected from the group consisting of 3,4-disubstituted thiophenes, the monomer being dispersed as oil drops in surfactant-free water, and the polymerization fluid being transparent,
wherein 90% or more of the total number of oil drops of the monomer dispersed in the polymerization fluid have a diameter of 250 nm or less.

2. The polymerization fluid according to claim 1 , wherein the monomer is 3,4-ethylenedioxythiophene.

3. The polymerization fluid according to claim 1 , further comprising at least one supporting electrolyte.

4. The polymerization fluid according to claim 3 , wherein the supporting electrolyte is at least one compound selected from a group consisting of borodisalicylic acid and borodisalicylic salts.

5. The polymerization fluid according to claim 3 , wherein the supporting electrolyte is at least one compound selected from the group consisting of a sulfonylimidic acid of the formula (I) or the formula (II)

where m is an integer from 1 to 4, n is an integer from 1 to 4, and o is an integer 2 or 3, and salts thereof.

6. A method for producing the polymerization fluid according to claim 1 , comprising:
an addition step of adding the monomer to the surfactant-free water to prepare a phase separation fluid where water and the monomer are phase-separated;
a first dispersion step of irradiating the phase separation fluid with ultrasonic waves to make the monomer dispersed in the form of oil drops and thus prepare an opaque dispersion, and
a second dispersion step of irradiating the opaque dispersion with ultrasonic waves having a frequency higher than that of the ultrasonic waves used in the first dispersion step to reduce the mean size of the oil drops of the monomer and thus prepare a transparent dispersion.

7. A method for producing the polymerization fluid according to claim 3 , comprising:
an addition step of adding the monomer to the surfactant-free water to prepare a phase separation fluid where water and the monomer are phase-separated;
a first dispersion step of irradiating the phase separation fluid with ultrasonic waves to make the monomer dispersed in the form of oil drops and thus prepare an opaque dispersion;
a second dispersion step of irradiating the opaque dispersion with ultrasonic waves having a frequency higher than that of the ultrasonic waves used in the first dispersion step to reduce the mean size of the oil drops of the monomer and thus prepare a transparent dispersion, and
a step of adding the at least one supporting electrolyte, before the first dispersion step, between the first dispersion step and the second dispersion step, or after the second dispersion step.

8. The method for producing the polymerization fluid according to claim 6 , wherein the ultrasonic waves in the first dispersion step have a frequency within the range of 15 to 200 kHz and power of 4 W/cm 2 or more, and the ultrasonic waves in the second dispersion step have a frequency within the range of 1 to 4 MHz and power of 5 W/cm 2 or more.

9. The method for producing the polymerization fluid according to claim 6 , wherein the ultrasonic irradiation period in the first dispersion step is within the range of 2 to 10 minutes and the ultrasonic irradiation period in the second dispersion step is within the range of 2 to 10 minutes.

10. The method for producing the polymerization fluid according to claim 7 , wherein the ultrasonic waves in the first dispersion step have a frequency within the range of 15 to 200 kHz and a power of 4 W/cm 2 or more, and the ultrasonic waves in the second dispersion step have a frequency within the range of 1 to 4 MHz and a power of 5 W/cm 2 or more.

11. The method for producing the polymerization fluid according to claim 7 , wherein the ultrasonic irradiation period in the first dispersion step is within the range of 2 to 10 minutes and the ultrasonic irradiation period in the second dispersion step is within the range of 2 to 10 minutes.

Assignees

• Atobe Mahito
• Nakabayashi Koji
• Machida Kenji
• Takeda Sekihiro
• Nippon Chemicon

Inventors

• Atobe Mahito
• Nakabayashi Koji
• Machida Kenji
• Takeda Sekihiro

Classifications

• H01G9/028 Primary

  Organic semiconducting electrolytes, e.g. TCNQ · CPC title

• H05B33/28

  of translucent electrodes · CPC title

• H01B1/127

  comprising five-membered aromatic rings in the main chain, e.g. polypyrroles, polythiophenes · CPC title

• C08G2261/1424

  containing ether groups, including alkoxy · CPC title

• H01G11/56

  Solid electrolytes, e.g. gels; Additives therein · CPC title