High-thickness and high-conductivity PEDOT film and preparation method thereof

A high-conductivity, thin-film technology, used in equipment for manufacturing conductive/semiconductive layers, cable/conductor manufacturing, circuits, etc., can solve the problems of accelerated reaction speed, low solubility, pollution, etc. High conductivity and cost reduction effect

Active Publication Date: 2017-01-04
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The second shortcoming lies in FeTos 3 and FeOtf 3 And other traditional oxidants also have the following two unstable characteristics, which limit their application: First, due to FeTos 3 and FeOtf 3 The middle anions are all strong acid ions, and the pH value of the solution is higher, which speeds up the reaction speed. Too fast reaction speed leads to the formation of structural defects and reduces the thermoelectric performance. Therefore, it is necessary to add alkaline inhibitors such as pyridine to improve the solution. pH, slows down the reaction speed, pyridine is highly toxic to humans, and its volatilization causes environmental pollution
Secondly, due to the low solubility, it is easy to crystallize and precipitate when the reaction is heated, forming defects in the film, which is not conducive to the transport of carriers, so it is necessary to add additional copolymers to inhibit crystallization, such as polyethylene glycol-propylene glycol-ethylene glycol Diol terpolymer (PEPG), the incorporation of PEPG introduces a non-conductive second phase in PEDOT, reducing the uniformity and conductivity of the film

Method used

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  • High-thickness and high-conductivity PEDOT film and preparation method thereof
  • High-thickness and high-conductivity PEDOT film and preparation method thereof
  • High-thickness and high-conductivity PEDOT film and preparation method thereof

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preparation example Construction

[0030] The present invention is prepared by synthesizing oxidant iron salt FeX 3 , Preparation of precursor solution, spin coating, polymerization, and washing processes. The invention can also effectively increase the film thickness and avoid the addition of pyridine and PEPG, while ensuring that the thermoelectric performance is not reduced.

[0031]The present invention uses doped ion sodium salt, barium salt or acid as raw material, reacts with ferric trichloride or ferric sulfate, prepares oxidant iron salt by barium sulfate precipitation method, hydrogen chloride distillation method or solution precipitation method, and then its Soluble in alcohol solvent. The solvent can be one or more of methanol, ethanol, propanol, butanol or alcohol-water mixed medium, and the concentration is between 46%-84% by mass fraction. The PEDOT synthesized based on the method provided by the present invention can be synthesized in methanol, ethanol, propanol, butanol or alcohol-water mixed...

Embodiment 1

[0041] Embodiment 1PEDOT: dodecylbenzenesulfonic acid (PEDOT: DBSA) material

[0042] Dissolve 9.00mmol ferric chloride hexahydrate and 18.00mmol sodium dodecylbenzenesulfonate in deionized water respectively, and add the ferric chloride solution dropwise to the sodium dodecylbenzenesulfonate solution under vigorous stirring , the iron dodecylbenzenesulfonate precipitate was washed 10 times with deionized water until no Cl - Check out. Then add 250mL ethanol to dissolve and evaporate to dryness in a rotary evaporator. Then re-dissolve the solid in ethanol to prepare an ethanol solution with a mass fraction of 74.3%-83.1% for future use. The above solution was spin-coated on a 18*18mm soda-lime glass substrate to form a film at a rotation speed of 5000-10000rpm and a spin-coating time of 15s. Place the spin-coated ferric dodecylbenzenesulfonate film in a double-pass flat-bottomed reaction vessel made of quartz or glass, feed nitrogen and saturated EDOT monomer vapor with a g...

Embodiment 2

[0043] Embodiment 2PEDOT: butyl naphthalene sulfonic acid (PEDOT: BNSA) material

[0044] Dissolve 9.00mmol ferric chloride hexahydrate and 18.00mmol sodium butylnaphthalene sulfonate in deionized water respectively, add the ferric chloride solution dropwise into the sodium butylnaphthalene sulfonate solution under vigorous stirring, and The ferric naphthalenesulfonate precipitate was washed 10 times with deionized water until no Cl ions were detected. Then add 250mL ethanol to dissolve and evaporate to dryness in a rotary evaporator. Then the solid was re-dissolved in ethanol to prepare an 80.1% mass fraction ethanol solution for later use, and then 5% mass fraction of butylnaphthalenesulfonic acid was added. The above solution was spin-coated on a 18*18mm soda-lime glass substrate to form a film at a rotation speed of 6000rpm and a spin-coating time of 15s. Place the spin-coated precursor film in a double-pass flat-bottomed reaction vessel made of quartz or glass, pass thr...

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Abstract

The invention relates to a high-thickness and high-conductivity PEDOT film and a preparation method thereof. The PEDOT film containing PEDOT:X is prepared from an EDOT monomer as a raw material and a weak basic anion-containing high-alcohol-solubility ferric salt FeX<3> as an oxidizing agent by adopting a gas phase method or a solution method, wherein X is high-alcohol-solubility weak basic anions, preferably, at least one of camphosulfonate ions, long-chain alkylbenzene sulfonate ions, alkyl naphthalene sulfonate ions, dialkyl naphthalene sulfonate ions and dinonyl naphthalene disulfonate ions. According to the film and the preparation method thereof, by utilizing high alcohol solubility of a ferric salt oxidizing agent solution of a precursor, the concentration and viscosity of a spin-coating solution are improved, the crystallization of the oxidizing agent in a reaction process is inhibited, and copolymer anti-crystallization inhibitors (pyridine, PEPG and the like) do not need to be added, so that a high-thickness PEDOT film is obtained.

Description

technical field [0001] The invention belongs to the field of energy materials, and specifically relates to a PEDOT film with high film thickness and high conductivity and a preparation method thereof. The product has high film thickness and high conductivity, optimizes the traditional process, and better meets the application requirements. Background technique [0002] Conductive polymer materials have better ductility, processability and lower cost than traditional inorganic bulk materials. Poly-3,4-ethylenedioxythiophene (PEDOT) is currently the most excellent conductive polymer thermoelectric material. , PSS-doped PEDOT is most commonly used due to its high conductivity and commercial production. The highest ZT value of the PEDOT film prepared by Kim et al. reached 0.42 (Nat Mater, 2013, 12, 719). In addition, the small molecule doped PEDOT prepared by solution method, gas phase method and electrochemical polymerization, such as PEDOT:Tos, has a more compact and regular s...

Claims

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Application Information

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IPC IPC(8): H01B5/14H01B13/00
CPCH01B5/14H01B13/0026
Inventor 陈立东石唯姚琴瞿三寅
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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