CN112635671B - Resistance reduction method for conductive polymer PEDOT (PEDOT-PSS) based on femtosecond laser modification - Google Patents

Resistance reduction method for conductive polymer PEDOT (PEDOT-PSS) based on femtosecond laser modification Download PDF

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CN112635671B
CN112635671B CN202011512381.3A CN202011512381A CN112635671B CN 112635671 B CN112635671 B CN 112635671B CN 202011512381 A CN202011512381 A CN 202011512381A CN 112635671 B CN112635671 B CN 112635671B
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李晓鹏
周嘉悦
彭勇
周琦
王克鸿
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Nanjing University of Science and Technology
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Abstract

The invention relates to a femtosecond laser modification-based resistance reduction method for conductive polymers PEDOT and PSS. The PEDOT PSS film is prepared by spin-coating a clean substrate material with a spin coater, wherein the substrate material is glass, silicon wafer or PET and the like. The method adopts femtosecond laser to focus on the surface of the PEDOT/PSS film, adjusts the matching relation between laser processing technological parameters and a laser scanning processing path, and utilizes the characteristic that the stability of PSS molecules is inferior to that of the PEDOT molecules to reduce the relative content of insulating PSS under the condition of not causing great damage to conductive PEDOT, so that the PSS shell in the PEDOT/PSS is thinned, and the conductivity of the PEDOT/PSS film material is enhanced. By adopting the method, the relative content of the insulated PSS in the PEDOT/PSS film material can be specifically reduced under the conditions that a polar solvent or an alcohol solvent is not added for modification and the light transmittance of the film material is not influenced, so that the conductivity of the PEDOT/PSS film material is enhanced. Has the advantages of simple and convenient operation and short processing time. The invention is suitable for transparent conductive films.

Description

Resistance reduction method for conductive polymer PEDOT (PEDOT-PSS) based on femtosecond laser modification
Technical Field
The invention relates to the technical field of femtosecond laser processing, relates to processing of a conductive polymer PEDOT/PSS film material by femtosecond laser, and particularly relates to a resistance reduction method of the conductive polymer PEDOT/PSS based on femtosecond laser modification.
Background
The PEDOT PSS solution is a high molecular polymer aqueous solution and is composed of PEDOT and PSS. PEDOT (also called poly (3, 4-ethylenedioxythiophene)) is a polymer of EDOT (3, 4-ethylenedioxythiophene monomer) and is a conductive polymer material, but intrinsic PEDOT has poor solubility, so that the application of the PEDOT is limited, PSS is polystyrene sulfonate, the solubility of the PEDOT is greatly improved by combining the PEDOT and the PSS suspension, and the obtained PEDOT suspension is coated on materials such as glass, silicon wafers or PET to obtain a transparent conductive film with high conductivity and good light transmittance, so that the PEDOT suspension can be widely applied to organic optoelectronic products such as solar cells, LED lamps, liquid crystal panels, touch screens and the like.
But the conductivity of the PEDOT: PSS film is limited to some extent by the presence of the insulating PSS. At present, the traditional method for enhancing the conductivity of the PEDOT/PSS thin film is mainly to add a certain amount of polar solvent or alcohol solvent into a PEDOT/PSS solution for doping, or use some alcohols or acids for carrying out post-treatment on the PEDOT/PSS thin film, and use a metal implantation method for enhancing the conductivity, but most methods inevitably introduce other components, so that the preparation process of the conductive thin film is more complicated and longer, and the cost is increased, so that the development of a novel method for enhancing the conductivity of the PEDOT/PSS conductive thin film is imperative.
Disclosure of Invention
The invention aims to provide a resistance reducing method of a conductive polymer PEDOT (PEDOT-PSS) based on femtosecond laser modification.
The technical solution for realizing the purpose of the invention is as follows:
a resistance reducing method for a conductive polymer PEDOT (PSS) based on femtosecond laser modification is characterized in that a spin coater is used for spin-coating a PEDOT PSS film on a clean substrate material, the PEDOT PSS film is irradiated by femtosecond laser to thin an insulating PSS shell in the PEDOT PSS, and the conductivity of the PEDOT PSS film material is enhanced.
Further, the method specifically comprises the following steps:
the method comprises the following steps: cleaning the base material: and selecting a substrate of a PEDOT PSS film, carrying out ultrasonic treatment on the substrate material in a solution of alcohol and the like, and drying to obtain a clean substrate.
Step two: preparation of PEDOT PSS film: fixing a clean substrate on a spin coater, taking a proper amount of PEDOT (PSS) solution by using a liquid transfer machine, dripping the solution on the substrate, uniformly covering the substrate with the solution, adjusting the rotating speed of the spin coater and the spin coating time to obtain a PEDOT (PSS) wet film, then placing the PEDOT (PSS) wet film on a constant-temperature hot plate, and drying to obtain a PEDOT (PSS) film sample with uniform thickness;
step three: assembling: horizontally placing a PEDOT PSS film sample on an objective table of a processing system, adjusting a light path to enable femtosecond laser to vertically irradiate the surface of the sample, and focusing the laser on the surface of the PEDOT PSS film;
step four: setting parameters of the femtosecond laser: selecting a near-infrared femtosecond laser and setting laser pulse width and laser repetition frequency; the wavelength range of the near infrared femtosecond laser is 800nm-1064 nm.
Step five: scanning PEDOT by femtosecond laser irradiation, PSS film: introducing a preprocessed processing program into integrated software, determining a laser processing path, adjusting the matching relation between the laser processing path and technological parameters such as laser power density, scanning speed, scanning delay, jumping speed, jumping delay, corner delay, whole amplitude, frequency division, defocusing and the like, reducing the relative content of insulating PSS, and enhancing the conductivity of the PSS film material PEDOT;
step six: and taking out PEDOT (PSS) film material after the processing is finished.
Furthermore, the substrate can be made of glass, silicon wafers or PET and the like, and the size of the substrate is about 20mm by 20 mm.
Further, if rigid materials such as glass or silicon wafers are selected as the substrate in the substrate cleaning process, the substrate needs to be sequentially soaked in ethanol and acetone for ultrasonic cleaning for 10-20min, then placed on a constant temperature hot plate for drying at the temperature of 100-200 ℃ for 10-20min, and finally placed in an ozone processor for treatment for 10-20 min; if a flexible material such as PET is selected as a substrate, the flexible material is cut into a proper size, soaked in ethanol and distilled water, ultrasonically cleaned for 5-20min, and dried for use.
Further, the rotation speed of the spin coater is 1000-4000rmp/min, the spin coating time is 10-60s, the temperature of the constant temperature hot plate is 100-200 ℃, the drying time is 10-30min, and the thickness of a PEDOT (polyethylene glycol terephthalate) (PSS) film sample is 30-100 nm;
furthermore, the center wavelength of the femtosecond laser in the fourth step is 800-.
Further, the laser power density in the fifth step is 50-2000mJ/cm 2 The laser processing scanning path is an S-shaped path. The diameter of the laser spot can be measured to be 10-500 mu m by properly adjusting the defocusing amount. In order to make the laser processing scanning path completely cover the PEDOT PSS film, the distance between two adjacent processing paths needs to be adjusted, and the distance ranges from 0.005 mm to 0.1 mm. The scanning speed during processing was 10 μmThe/s-1000 mm/s, the scanning delay is 100-.
Compared with the prior art, the invention has the following remarkable advantages:
(1) according to the modification method, the femtosecond laser is adopted to irradiate the PEDOT (PSS) film, and the characteristic that the stability of PSS molecules is inferior to that of the PEDOT molecules is utilized, so that the relative content of insulating PSS can be reduced under the condition that the conductive PEDOT is not greatly damaged, and the conductivity of the PEDOT (PSS) film material is enhanced;
(2) the modification method can reduce the square resistance of the PEDOT/PSS film by 1-2 orders of magnitude;
(3) the modification method of the invention belongs to nondestructive modification, and the transmittance of the PEDOT PSS film before and after modification is not obviously changed;
(4) the modification method of the invention does not need to add polar solvent or alcohol solvent for modification, and does not need to introduce other components such as metal wires, and the like, and has simple and convenient operation and short processing time.
The present invention is described in further detail below with reference to the attached drawing figures.
Drawings
FIG. 1 is a schematic diagram of PSS (modified polymer) of conductive polymer PEDOT modified by femtosecond laser according to the present invention; wherein, FIG. 1(a) shows the original form of PEDOT: PSS, FIG. 1(b) shows the course of femtosecond laser irradiation, and FIG. 1(c) shows the completion of femtosecond laser irradiation.
FIG. 2 is a schematic diagram of a femtosecond laser processing path according to the present invention.
Detailed Description
The invention will be further explained with reference to the drawings
The invention provides a resistance reducing method of a conductive polymer PEDOT (polymer substrate) PSS based on femtosecond laser modification, which reduces the relative content of insulating PSS without causing great damage to the conductive PEDOT.
As shown in figure 1, the resistance reduction method of the conductive polymer PEDOT PSS based on femtosecond laser modification comprises the steps of cleaning a substrate material, preparing a PEDOT PSS film, and irradiating the modified PEDOT PSS film by femtosecond laser 3.
And irradiating the PEDOT PSS film by using femtosecond laser to thin an insulating PSS shell in the PEDOT PSS, so that the conductivity of the PEDOT PSS film material is enhanced.
A femtosecond laser modification-based resistance reduction method for conductive polymers PEDOT and PSS comprises the following steps:
the first step is as follows: cleaning the base material: selecting a substrate of a PEDOT PSS film, carrying out ultrasonic treatment on the substrate material in a solution of alcohol and the like, and drying to obtain a clean substrate.
The second step: preparation of PEDOT PSS films: fixing a clean substrate on a spin coater, taking a proper amount of PEDOT (PSS) solution by using a liquid transfer machine, dripping the solution on the substrate, uniformly covering the substrate with the solution, adjusting the rotating speed of the spin coater and the spin coating time to obtain a PEDOT (PSS) wet film, then placing the PEDOT (PSS) wet film on a constant-temperature hot plate, and drying to obtain a PEDOT (PSS) film sample with uniform thickness;
the third step: assembling: horizontally placing a PEDOT PSS film sample on an objective table of a processing system, adjusting a light path to enable femtosecond laser to vertically irradiate the surface of the sample, and focusing the laser on the surface of the PEDOT PSS film;
the fourth step: setting parameters of the femtosecond laser: selecting a near-infrared femtosecond laser and setting a laser pulse width and a laser repetition frequency;
the fifth step: scanning PEDOT by femtosecond laser irradiation, PSS film: introducing a preprocessed processing program into integrated software, determining a laser processing path, adjusting the matching relation between the laser processing path and technological parameters such as laser power density, scanning speed, scanning delay, jumping speed, jumping delay, corner delay, whole amplitude, frequency division, defocusing and the like, reducing the relative content of insulating PSS, and enhancing the conductivity of the PSS film material PEDOT;
and a sixth step: and taking out PEDOT (PSS) film material after the processing is finished.
In the first step of the invention, the substrate can be made of glass, silicon wafers or PET and the like, and the size of the substrate is about 20mm by 20 mm.
In the first step of the invention, if rigid materials such as glass or silicon wafers are selected as a substrate, the substrate is required to be sequentially soaked in ethanol and acetone for ultrasonic cleaning for 10-20min, then the substrate is placed on a constant temperature hot plate and dried at the temperature of 100-200 ℃ for 10-20min, and finally the substrate is placed in an ozone processor for treatment for 10-20 min; if a flexible material such as PET is selected as a substrate, the flexible material is cut into a proper size, soaked in ethanol and distilled water, ultrasonically cleaned for 5-20min, and dried for use.
In the second step, the rotation speed of the spin coater is 1000-;
in the fourth step, the center wavelength of the femtosecond laser is 800-1064nm, the laser pulse width is 50-1000fs, and the laser repetition frequency is 200-1000 KHz.
In the fifth step of the invention, the laser power density is 50-2000mJ/cm 2 The laser machining scan path is an S-shaped path, as shown in fig. 2. The diameter of the laser spot can be measured to be 10-500 mu m by properly adjusting the defocusing amount. In order to make the laser processing scanning path completely cover the PEDOT PSS film, the distance between two adjacent processing paths needs to be adjusted, and the distance ranges from 0.005 mm to 0.1 mm. The scanning speed is 10 mu m/s-1000mm/s, the scanning delay is 100-2000 mu s, the jump speed is 1000-10000mm/s, the jump delay is 100-3000 mu s, the corner delay is 100-1000 mu s, the whole number of times is 1-100, the frequency division amount is 1-100, and the defocusing amount is 0-5 mm.
The principle of the invention is as follows: the femtosecond laser operates in a pulse mode, has a small focusing diameter and a duration of 10 femtoseconds -15 s), the instantaneous power is extremely high, and energy can be deposited in a time scale shorter than the electron-phonon equilibrium time, so that the thermal effect generated by processing can be frozen near the initial energy deposition position, and local heating is realized. Compared with metal materials, because of less free electrons in the nonmetal materials, electrons bound around atoms can become free electrons under the excitation of a strong laser field, an electrostatic field is formed on the surface of the materials, when the electrostatic force is larger than the acting force between crystal lattices, coulomb explosion is generated, and particles are separated from each otherThe chemical bonds are broken and the surface material is removed in the form of sprayed particles. The femtosecond laser acts on the surface of the substance in a way of destroying the lattice structure of the substance by melting, gasifying and coulomb explosion, so that the substance is removed or modified. PEDOT, namely PSS high polymer consists of PEDOT and PSS, wherein the PEDOT has small molecular weight due to positive charge brought by oxidative polymerization, and has a main structure of a ring structure with good stability. PSS has sulfite with negative charge and larger molecular weight, and has some single bonds such as C-C single bond, C-H single bond and the like besides a cyclic structure, so that the stability of PSS is inferior to PEDOT. The PEDOT and PSS are tightly combined in aqueous solution by means of ionic bonds to form spherical double-layer PEDOT, namely PSS colloidal particles, wherein the inner part of the spherical double-layer PEDOT is very conductive but insoluble in water, and the outer shell of the spherical double-layer PEDOT is insulating but hydrophilic PSS. And spin-coating and drying the PEDOT PSS solution to obtain the PEDOT PSS conductive film. The spin-coating method is used for preparing PEDOT, namely a PSS film with the PSS layer on the uppermost end of the surface. Different thresholds exist for the fractures of different chemical bonds under the femtosecond laser intensity field, so that by utilizing two conditions that the stability of the PSS is inferior to that of the PEDOT and the highest end of the surface of the film is a PSS layer, the process parameters of the femtosecond laser which vertically irradiates the PEDOT, namely the PSS film, are adjusted, and the matching relation between the laser processing process parameters and a laser scanning processing path is adjusted, the relative content of the insulated PSS can be reduced under the condition that the conductive PEDOT is not greatly damaged, the PSS shell in the PEDOT, namely the PSS, is thinned, and the conductivity of the PEDOT, namely the PSS film material is enhanced.
In the embodiment 1, a 20mm by 20mm monocrystalline silicon wafer is selected as a substrate of the PEDOT PSS film, the silicon wafer is soaked in ethanol and ultrasonically cleaned for 15min and then soaked in acetone and ultrasonically cleaned for 15min and then taken out, the ultrasonically treated silicon wafer is placed on a constant temperature hot plate and dried for 15min at 150 ℃, then naturally cooled for 5min, then the silicon wafer is placed in an ozone processor for treatment for 15min to remove redundant organic matters on the surface of the silicon wafer, and finally the clean silicon wafer is obtained and used as the substrate of the PEDOT PSS film. Vacuum adsorbing clean silicon wafer on spin coater, applying 100 μ l of PEDOT (PSS) solution onto the silicon wafer by pipette, uniformly covering the substrate with the solution, and adjusting the spin coater at 3000rmp/min for 45s to obtainAnd obtaining a PEDOT PSS wet film, then placing the PEDOT PSS wet film on a constant temperature hot plate, drying for 20min at 140 ℃, and finally obtaining a PEDOT PSS film sample with the thickness of 56 nm. And horizontally placing the PEDOT PSS film sample on an object stage of a microscope processing system, adjusting a light path to enable femtosecond laser to vertically irradiate the surface of the sample, and focusing the laser on the surface of the PEDOT PSS film. The parameters of the femtosecond laser are adjusted, the central wavelength of the laser adopted in the experiment is 1035nm, the pulse width of the laser is 300fs, and the repetition frequency of the laser is 1000 KHz. And (3) introducing a preprocessed processing program into the integrated software, wherein the laser processing scanning path is an S-shaped array, the array is a square, the length and the width of the array are both 20mm, the length of a corner is 0.01mm, and the distance between two adjacent scanning paths is 0.01 mm. The laser power density adopted by the experiment is 255mJ/cm 2 The scanning speed is 1000mm/s, the scanning delay is 1000 mus, the jumping speed is 7000mm/s, the jumping delay is 1000 mus, the corner delay is 100 mus, the whole frame number is 1, the frequency division is 1, and the defocusing amount is 0 during femtosecond laser processing. And taking out PEDOT (PSS) film material after the processing is finished. Tests prove that the square resistance of the PEDOT and PSS film is reduced from 81819 omega/sq to 5314 omega/sq after modification, and the effect is obvious; besides, the transmittance of the PEDOT and PSS film is not obviously changed before and after modification, so that the PEDOT and PSS film is subjected to lossless modification and meets the requirements.

Claims (7)

1. The femtosecond laser modification-based resistance reduction method for the conductive polymer PEDOT PSS is characterized in that a spin coater is used for spin-coating a clean substrate material to prepare a PEDOT PSS film, and the femtosecond laser is used for irradiating the PEDOT PSS film to thin an insulating PSS shell in the PEDOT PSS, so that the conductivity of the PEDOT PSS film material is enhanced.
2. The method according to claim 1, characterized in that it comprises in particular the steps of:
the method comprises the following steps: cleaning the base material: selecting a substrate of a PEDOT (PSS) film, carrying out ultrasonic treatment on the substrate material in an alcohol solution, and drying to obtain a clean substrate;
step two: preparation of PEDOT PSS films: fixing a clean substrate on a spin coater, taking a PEDOT (PSS) solution by using a liquid transfer machine, dripping the solution on the substrate, uniformly covering the substrate with the solution, adjusting the rotating speed of the spin coater and the spin coating time to obtain a PEDOT (PSS) wet film, then placing the PEDOT (PSS) wet film on a constant-temperature hot plate, and drying to obtain a PEDOT (PSS) film sample with uniform thickness;
step three: assembling: horizontally placing a PEDOT PSS film sample on an object stage of a processing system, adjusting a light path to enable femtosecond laser to vertically irradiate the surface of the sample, and focusing the laser on the surface of the PEDOT PSS film;
step four: setting parameters of the femtosecond laser: selecting a near-infrared femtosecond laser and setting laser pulse width and laser repetition frequency;
step five: scanning PEDOT by femtosecond laser irradiation, PSS film: introducing a preprocessed processing program into integrated software, determining a laser processing path, adjusting the matching relation between the laser power density, the scanning speed, the scanning delay, the jumping speed, the jumping delay, the corner delay, the whole frame times, the frequency division amount and the defocusing amount process parameters and the laser processing path, reducing the relative content of insulating PSS, and enhancing the conductivity of the PEDOT PSS film material;
step six: and taking out PEDOT (PSS) film material after the processing is finished.
3. The method according to claim 2, wherein the substrate is selected from glass, silicon wafer or PET material, and the size of the substrate is 20mm by 20 mm.
4. The method as claimed in claim 2, wherein in the substrate cleaning process, if a glass or silicon chip rigid material is selected as the substrate, the substrate is sequentially soaked in ethanol and acetone for ultrasonic cleaning for 10-20min, then placed on a constant temperature hot plate for drying at 100-200 ℃ for 10-20min, and finally placed in an ozone processor for treatment for 10-20 min; if the PET flexible material is selected as the substrate, the PET flexible material is cut into a proper size, soaked in ethanol and distilled water, ultrasonically cleaned for 5-20min, and dried for use.
5. The method as claimed in claim 2, wherein the spin rate of the spin coater is 1000-4000rmp/min, the spin coating time is 10-60s, the temperature of the thermostatic hot plate is 100-200 ℃, the drying time is 10-30min, and the thickness of the PEDOT: PSS film sample is 30-100 nm.
6. The method as claimed in claim 2, wherein the center wavelength of the femtosecond laser in the fourth step is 800-1064nm, the pulse width of the laser is 50-1000fs, and the repetition frequency of the laser is 200-1000 KHz.
7. The method of claim 2, wherein the laser power density in the fifth step is 50-2000mJ/cm 2 The laser processing scanning path is an S-shaped path; the diameter of a laser spot can be measured to be 10-500 mu m by properly adjusting the defocusing amount; PSS film, the interval between two adjacent processing paths needs to be adjusted, and the range of the interval is 0.005-0.1 mm; the scanning speed is 10 mu m/s-1000mm/s, the scanning delay is 100-2000 mu s, the jump speed is 1000-10000mm/s, the jump delay is 100-3000 mu s, the corner delay is 100-1000 mu s, the whole number of times is 1-100, the frequency division amount is 1-100, and the defocusing amount is 0-5 mm.
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