CN112635671A - Femtosecond laser modification-based resistance reduction method for conductive polymer PEDOT (PEDOT-PSS) - Google Patents
Femtosecond laser modification-based resistance reduction method for conductive polymer PEDOT (PEDOT-PSS) Download PDFInfo
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Abstract
The invention relates to a femtosecond laser modification-based resistance reduction method for conductive polymers PEDOT and PSS. Selecting materials such as glass, silicon wafers or PET as a substrate of the PEDOT PSS film, and spin-coating the clean substrate material by using a spin coater to prepare the PEDOT PSS film. 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 insulating PSS in the PEDOT/PSS film material can be reduced in a targeted manner 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 operation and short processing time. The invention is suitable for transparent conductive films.
Description
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 femtosecond laser modification-based resistance reduction method for conductive polymers PEDOT and PSS.
The technical solution for realizing the purpose of the invention is as follows:
a femtosecond laser modification-based resistance reduction method for a conductive polymer PEDOT and PSS comprises the steps of utilizing a spin coater to spin-coat a clean substrate material to prepare a PEDOT and PSS film, utilizing femtosecond laser to irradiate the PEDOT and PSS film to thin an insulating PSS shell in the PEDOT and PSS, and enhancing the conductivity of the PEDOT and PSS film material.
Further, the method specifically comprises the following steps:
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 a solution of alcohol and the like, and drying to obtain a clean substrate.
Step two: 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;
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-;
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/cm2The 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 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.
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 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, the graph (a) is the original form of PEDOT and PSS, the graph (b) is in the femtosecond laser irradiation process, and the graph (c) is after the femtosecond laser irradiation is finished.
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 is that: 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 laser pulse width and 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 of the invention, the center wavelength of the femtosecond laser is 800-.
In the fifth step of the invention, the laser power density is 50-2000mJ/cm2Laser, laserThe 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 femtosecond orders-15s), the instantaneous power is extremely high, energy can be deposited in a time scale shorter than the electron-phonon equilibrium time, and therefore the thermal effect generated by the processing can be frozen near the initial energy deposition position, and local heating is realized. Compared with a metal material, because the non-metal material has less free electrons, 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 material, when the electrostatic force is larger than the acting force between crystal lattices, coulomb explosion is generated, chemical bonds between particles are broken, and the surface material is removed in a particle spraying mode. 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. The PEDOT and PSS high polymer consists of PEDOT and PSS, wherein the PEDOT has positive charges due to oxidative polymerization, has small molecular weight, has a main structure of a ring structure, and has 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 is very conductive and insoluble in water, and the outer shell is insulating and 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. In the field of femtosecond laser intensityThe method has the advantages that different thresholds exist for the fractures of different chemical bonds, 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 the PSS layer, the process parameters of femtosecond laser for vertically irradiating the PEDOT, namely the PSS film, are adjusted, the matching relation between the laser processing process parameters and a laser scanning processing path is adjusted, the relative content of insulating 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. And (2) adsorbing a clean silicon wafer on a spin coater in vacuum, dripping 100 mu l of PEDOT (PSS) solution on the silicon wafer by using a liquid transfer machine, uniformly covering the substrate with the solution, adjusting the rotation speed of the spin coater to 3000rmp/min and the spin coating time to 45s to obtain a PEDOT (PSS) wet film, then drying the PEDOT (PSS) wet film on a constant temperature hot plate at 140 ℃ for 20min, 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/cm2The 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. PSS (PEDOT-PSS) is taken out after the processing is finishedA film material. 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 solutions such as alcohol and the like, 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 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;
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 of claim 2, wherein the substrate is selected from glass, silicon wafer, or PET, and has a size of about 20mm by 20 mm.
4. The method as claimed in claim 2, wherein in the substrate cleaning process, if rigid materials such as glass or silicon wafers are 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 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.
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 constant temperature 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/cm2The 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 during processingThe drawing delay is 100-2000 mu s, the jumping speed is 1000-10000mm/s, the jumping delay is 100-3000 mu s, the corner delay is 100-1000 mu s, the whole frame number is 1-100, the frequency division amount is 1-100, and the defocusing amount is 0-5 mm.
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| CN116693908A (en) * | 2023-07-26 | 2023-09-05 | 浙江大学 | PEDOT-PSS film with high conductivity and preparation method thereof |
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| CN104934540A (en) * | 2015-05-27 | 2015-09-23 | 湖北大学 | Plastic-based high-conductivity PEDOT: PSSS film electrode, preparation method and application thereof |
| CN111009614A (en) * | 2019-12-20 | 2020-04-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Construction method of high-sensitivity photoelectric detector based on one-dimensional fullerene material/PEDOT (Polytetrafluoroethylene)/PSS (Polytetrafluoroethylene) composite film |
| CN111682123A (en) * | 2020-06-24 | 2020-09-18 | 南京邮电大学 | Modified PEDOT PSS film and preparation method and application thereof |
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| CN101121575A (en) * | 2007-07-06 | 2008-02-13 | 中国科学院上海光学精密机械研究所 | Method for realizing selectivity metallization on glass surface by femto-second laser |
| CN104934540A (en) * | 2015-05-27 | 2015-09-23 | 湖北大学 | Plastic-based high-conductivity PEDOT: PSSS film electrode, preparation method and application thereof |
| CN111009614A (en) * | 2019-12-20 | 2020-04-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Construction method of high-sensitivity photoelectric detector based on one-dimensional fullerene material/PEDOT (Polytetrafluoroethylene)/PSS (Polytetrafluoroethylene) composite film |
| CN111682123A (en) * | 2020-06-24 | 2020-09-18 | 南京邮电大学 | Modified PEDOT PSS film and preparation method and application thereof |
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| CN116693908A (en) * | 2023-07-26 | 2023-09-05 | 浙江大学 | PEDOT-PSS film with high conductivity and preparation method thereof |
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