CN113210871B - Preparation method of polyimide film with periodic micro-nano structure - Google Patents

Preparation method of polyimide film with periodic micro-nano structure Download PDF

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CN113210871B
CN113210871B CN202110473265.3A CN202110473265A CN113210871B CN 113210871 B CN113210871 B CN 113210871B CN 202110473265 A CN202110473265 A CN 202110473265A CN 113210871 B CN113210871 B CN 113210871B
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polyimide film
laser
sample
nano structure
excimer laser
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CN113210871A (en
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赵嵩卿
谢玄
庄振国
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China University of Petroleum Beijing
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China University of Petroleum Beijing
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/352—Working by laser beam, e.g. welding, cutting or boring for surface treatment
    • B23K26/355—Texturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
    • B23K26/06—Shaping the laser beam, e.g. by masks or multi-focusing
    • B23K26/064—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
    • B23K26/06—Shaping the laser beam, e.g. by masks or multi-focusing
    • B23K26/064—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms
    • B23K26/0643—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms comprising mirrors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
    • B23K26/06—Shaping the laser beam, e.g. by masks or multi-focusing
    • B23K26/064—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms
    • B23K26/066—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms by using masks
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/60—Preliminary treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/70—Auxiliary operations or equipment
    • B23K26/702—Auxiliary equipment
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B27/00—Optical systems or apparatus not provided for by any of the groups G02B1/00 - G02B26/00, G02B30/00
    • G02B27/09—Beam shaping, e.g. changing the cross-sectional area, not otherwise provided for
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B27/00—Optical systems or apparatus not provided for by any of the groups G02B1/00 - G02B26/00, G02B30/00
    • G02B27/09—Beam shaping, e.g. changing the cross-sectional area, not otherwise provided for
    • G02B27/0927—Systems for changing the beam intensity distribution, e.g. Gaussian to top-hat

Abstract

The invention provides an optical path system of an excimer laser and a preparation method of a polyimide film with a periodic micro-nano structure, wherein the optical path system of the excimer laser comprises the excimer laser for emitting laser, an energy attenuator, a light homogenizer and a sample platform which are sequentially arranged along the conducting direction of the optical path of the laser, and the energy attenuator is used for adjusting the energy of the laser; the dodging device is used for uniformly distributing the energy of the laser emitted from the energy attenuator; the sample platform is used for bearing a sample to be irradiated by laser, and the sample is placed on one side of the sample platform, which faces the light homogenizer. The light path system of the excimer laser can ensure that excimer laser irradiates the surface of the polyimide film after a specific parameter range is determined by utilizing the periodic surface structure of a laser-induced material, and a periodic micro-nano structure is formed on the surface of the polyimide film.

Description

Preparation method of polyimide film with periodic micro-nano structure
Technical Field
The invention belongs to the technical field of excimer laser, and particularly relates to a preparation method of a polyimide film with a periodic micro-nano structure.
Background
In recent decades, the use of laser technology to form periodic structures on the surface of materials to improve certain properties of the materials has attracted great interest. These materials include metallic materials, inorganic non-metallic materials, polymers, and composites thereof. Polyimides have unique advantages over other polymeric materials: firstly, the material contains a large amount of nitrogen-containing five-membered heterocyclic rings and aromatic rings, which causes the rigidity of molecular chains of the material to be large and the intermolecular force to be strong; and secondly, due to the conjugated effect of the aromatic heterocycle, the polyimide has high heat resistance, thermal stability and high mechanical property. These advantages allow for broader applications of polyimides compared to other polymers. However, the development of a periodic structure on the surface of a polyimide film by a laser technique is almost blank.
Disclosure of Invention
Aiming at the defects or shortcomings in the prior art, the invention provides a preparation method of a polyimide film with a periodic micro-nano structure, which can form the periodic structure on the surface of polyimide by utilizing a laser technology so as to improve the physical properties of the polyimide film.
In order to achieve the above object, the present invention provides a method for preparing a polyimide film having a periodic micro-nano structure, wherein the preparation of the periodic micro-nano structure on the surface of the polyimide film is performed by using an optical path system of an excimer laser, the optical path system of the excimer laser comprises an excimer laser for emitting laser and a plurality of optical paths sequentially arranged along a conducting direction of the laser, the method comprises the following steps:
the energy attenuator is used for adjusting the energy of the laser;
the dodging device is used for uniformly distributing the energy of the laser emitted from the energy attenuator;
the sample platform is used for bearing a sample to be subjected to laser irradiation, and the sample is placed on one side, facing the light homogenizer, of the sample platform; the preparation method of the polyimide film with the periodic micro-nano structure comprises the following steps:
s1: preparing a polyimide film sample;
s3: fixing a polyimide film sample on a sample platform;
s2: setting pulse laser parameters;
s4: opening an excimer laser, and irradiating the polyimide film sample for a preset time;
s5: and (5) closing the excimer laser to obtain the polyimide film sample with the periodic micro-nano structure.
In an embodiment of the present invention, the step of preparing a polyimide film sample comprises:
s11: cutting the polyimide film into a shape with a preset size;
s12: placing the cut polyimide film in absolute ethyl alcohol, and ultrasonically cleaning for 10-15 minutes at room temperature;
s13: placing the polyimide film cleaned by the absolute ethyl alcohol in deionized water, and ultrasonically cleaning for 10-15 minutes at room temperature;
s14: and taking out the polyimide film and putting the polyimide film into a thermostat for drying to obtain a polyimide film sample.
In an embodiment of the invention, the pulsed laser parameters include laser frequency, fluence and irradiation time.
In the embodiment of the present invention, the laser frequency is 10Hz, and the energy density is in the range of 5mJ/cm-2～20mJ/cm-2The irradiation time is 5 min-30 min.
In an embodiment of the present invention, the optical path system of the excimer laser further comprises an optical path changing assembly located between the excimer laser and the energy attenuator, the optical path changing assembly comprising a plurality of spaced apart totally reflecting mirrors, the plurality of totally reflecting mirrors cooperating to change the optical path angle of the laser light emitted from the excimer laser.
In the embodiment of the invention, a mask is arranged between the sample platform and the light homogenizer, an irradiation port is arranged on the mask, and the laser emitted from the light homogenizer passes through the irradiation port to be irradiated on the sample.
In the embodiment of the invention, the position of the irradiation port corresponding to the sample is provided, the area of the irradiation port is larger than that of the sample, and the orthographic projection of the sample is completely projected in the irradiation port.
In an embodiment of the invention, the light homogenizer comprises a first plano-convex mirror and a light homogenizing plate positioned between the first plano-convex mirror and the energy attenuator, the plane side of the first plano-convex mirror is arranged towards the light homogenizing plate, and the central line of the light homogenizing plate is coincided with the focus of the first plano-convex mirror.
In the embodiment of the invention, a second plano-convex mirror is also arranged between the first plano-convex mirror and the mask, and the focus of the second plano-convex mirror and the focus of the first plano-convex mirror are positioned on the same straight line.
Through the technical scheme, the optical path system of the excimer laser provided by the embodiment of the invention has the following beneficial effects:
firstly, an excimer laser for emitting laser is installed, and then an energy attenuator, a light homogenizer and a sample platform are sequentially arranged along the conducting direction of the light path of the laser, so that the assembly of the light path system of the excimer laser is completed. The energy attenuator is used for adjusting the energy of the laser; the dodging device is used for uniformly distributing the energy of the laser emitted from the energy attenuator; after all the devices are assembled, a sample to be subjected to laser irradiation is placed on one side, facing the light homogenizer, of the sample platform, and excimer laser irradiation can be carried out on the sample by starting the excimer laser. The light path system of the excimer laser can ensure that excimer laser irradiates the surface of the polyimide film after a specific parameter range is determined by utilizing the periodic surface structure of a laser-induced material, and a periodic micro-nano structure is formed on the surface of the polyimide film.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide an understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view of the construction of an optical path system of an excimer laser according to the present invention.
Description of the reference numerals
1 excimer laser 42 first plano-convex mirror
2 optical path changing assembly 43 second plano-convex mirror
21 total reflection mirror 5 sample platform
3 energy attenuator 6 mask
4 light uniformizer 61 irradiation port
41 slide 7 sample
Detailed Description
The following detailed description of specific embodiments of the invention refers to the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative and explanatory of the invention and are not restrictive thereof.
An optical path system of an excimer laser according to the present invention is described below with reference to the drawings.
Referring to fig. 1, in the embodiment of the present invention, an optical path system of an excimer laser is provided, the optical path system of the excimer laser includes an excimer laser 1 for emitting laser light, and an energy attenuator 3, a dodging device 4 and a sample platform 5 which are sequentially arranged along an optical path conducting direction of the laser light, the energy attenuator 3 is used for adjusting the energy of the laser light; the dodging device 4 is used for uniformly distributing the energy of the laser emitted from the energy attenuator 3; the sample platform 5 is used for bearing a sample 7 to be irradiated by laser, and the sample 7 is placed on one side of the sample platform 5 facing the light homogenizer 4. The excimer laser is a laser that is generated when a molecule formed of a mixed gas of an inert gas and a halogen gas excited by an electron beam is transited to a ground state thereof.
When assembling the optical path system of the excimer laser, firstly, the excimer laser 1 is installed at a preset position, the excimer laser 1 emits laser, and the energy attenuator 3, the dodging device 4 and the sample platform 5 are sequentially arranged along the conduction direction of the laser optical path. The purpose of the energy attenuator 3 is to reduce the energy of the original laser pulse and to adjust the energy of the pulse laser by changing the angle of the internal mirror of the attenuator. The laser with the attenuated energy enters the light homogenizer 4 along the light path direction, the light homogenizer 4 converts laser pulses with Gaussian distribution into high flat waves, the laser with the uniformly distributed energy is emitted from the light emitting side of the light homogenizer 4, then the laser uniformly irradiates a sample 7 on the sample platform 5, and after the sample 7 is irradiated for a certain time, the sample 7 is induced to generate a periodic surface structure. The light path system of the excimer laser can ensure that excimer laser irradiates the surface of the polyimide film after a specific parameter range is determined by utilizing the periodic surface structure of a laser-induced material, and a periodic micro-nano structure is formed on the surface of the polyimide film.
In an embodiment of the present invention, the optical path system of the excimer laser further comprises an optical path changing assembly 2 located between the excimer laser 1 and the energy attenuator 3, the optical path changing assembly 2 comprising a plurality of totally reflecting mirrors 21, the plurality of totally reflecting mirrors 21 cooperating to change the optical path angle of the laser light emitted from the excimer laser 1. The number of the total reflection mirrors 21 is preferably two, and the two total reflection mirrors 21 cooperate to change the optical path of the laser by 180 degrees. Two total reflection mirrors 21 are arranged along vertical interval in the up-down direction, the focus of the total reflection mirror 21 that is located the top coincides with the central line of excimer laser 1 along the horizontal direction, the focus of the total reflection mirror 21 that is located the top coincides with the focus of the total reflection mirror 21 that is located the below along the vertical direction, so that the laser that sends from excimer laser 1 enters into the total reflection mirror 21 of below perpendicularly after the horizontal direction reflects through this total reflection mirror 21 and reflects, the total reflection mirror 21 of below becomes the laser reflection of vertical direction into during the horizontal direction enters into energy attenuator 3, change the light path direction through adopting two total reflection mirrors 21 in this embodiment, thereby can save the horizontal space of whole device.
In the embodiment of the present invention, a mask 6 is further disposed between the sample stage 5 and the light homogenizer 4, an irradiation port 61 is opened on the mask 6, and the laser light emitted from the light homogenizer 4 is irradiated onto the sample 7 through the irradiation port 61.
In the embodiment of the present invention, the irradiation port 61 is opened at a position corresponding to the sample 7, and the area of the irradiation port 61 is larger than the area of the sample 7, and the orthographic projection of the sample 7 is completely projected into the irradiation port 61. The laser light emitted from the second plano-convex mirror 43 is directly irradiated onto the sample 7 through the irradiation port 61 without any loss.
In the embodiment of the present invention, the light homogenizer 4 comprises a first planoconvex lens 42 and a light homogenizing sheet 41 located between the first planoconvex lens 42 and the energy attenuator 3, the planar side of the first planoconvex lens 42 is disposed toward the light homogenizing sheet 41, and the center line of the light homogenizing sheet 41 coincides with the focal point of the first planoconvex lens 42. A light evener 4 is arranged behind the energy attenuator 3, the light evener 4 consists of a light evener 41 and a flat convex mirror, and the function of the light evener is to change laser pulses with Gaussian distribution into high flat waves so that the energy distribution of the laser is more uniform. The horizontal center line of the dodging sheet 41 is coincident with the focus of the first plano-convex mirror, so that the laser light emitted from the dodging sheet 41 is more uniformly distributed and then reflected from the first plano-convex mirror.
In the embodiment of the present invention, a second plano-convex mirror 43 is further disposed between the first plano-convex mirror 42 and the mask 6, and a focal point of the second plano-convex mirror 43 and a focal point of the first plano-convex mirror 42 are located on the same line. The convex side of the second plano-convex mirror 43 is arranged toward the mask 6, the laser emitted by the first plano-convex mirror 42 is converged at the focal point of the second plano-convex mirror 43, and then emitted from the convex side of the second plano-convex mirror 43 to the mask 6, and the second plano-convex mirror 43 is used for re-dispersing the original laser after converging, so as to ensure the uniformity of the laser reaching the sample 7. In addition, by replacing the first plano-convex mirror 42 and the second plano-convex mirror 43 with different focal lengths, the size of the light spot emitted from the second plano-convex mirror 43 can be adjusted to meet the requirements on the size of the light spot of the sample under different experimental conditions.
The invention also provides a preparation method of the polyimide film with the periodic micro-nano structure, the preparation of the periodic micro-nano structure on the surface of the polyimide film adopts the optical path system of the excimer laser, and the preparation method of the polyimide film with the periodic micro-nano structure comprises the following steps:
s1: preparing a polyimide film sample 7;
s3: fixing a polyimide film sample 7 on a sample platform 5;
before irradiation, a polyimide film sample 7 with a certain size and shape is prepared, and then the prepared polyimide film sample 7 is fixed at a specific installation position on one side of the sample platform 5 facing the light homogenizer 4 in a bonding or clamping manner to wait for laser irradiation.
S2: setting pulse laser parameters;
s4: opening the excimer laser 1, and irradiating the polyimide film sample 7 for a preset time;
after the polyimide film sample 7 is fixed, the laser frequency of the excimer laser 1 is adjusted, the energy attenuator 3 is rotated to adjust the energy density, and the preset laser irradiation time is set in the excimer laser 1. And after the laser parameters are set, opening the excimer laser 1 to irradiate the sample 7.
S5: and (3) closing the excimer laser 1 to obtain the polyimide film sample 7 with the periodic micro-nano structure.
The operation method is simple, and a periodic micro-nano structure can be generated on the surface of the polyimide film by only constructing an optical path system according to the figure 1, fixing a prepared sample 7 to the sample platform 5 and adjusting an attenuator and setting laser parameters. Furthermore, the desired pattern can be generated by controlling the sample platform 5. The periodic micro-nano structure on the surface of the polyimide film prepared by the invention has a period of about 200nm and a ripple depth of 12-40 nm. The roughness and the hydrophilicity of the polyimide material are greatly improved, the roughness is improved to be different from the original 0.844nm to 1.218nm to 16.279nm, the hydrophilicity of the polyimide film can be enhanced, and the water contact angle is reduced to be close to 0 degree from the original 86 degree. Due to the existence of the periodic micro-nano structure, the film can be used as a substrate for surface enhanced Raman scattering. And other physical properties are improved, so that the polyimide film can be more excellent in the original application field.
In an embodiment of the invention, the pulsed laser parameters include laser frequency, fluence and irradiation time.
In the embodiment of the present invention, the laser frequency is 10Hz, and the energy density is in the range of 5mJ/cm-2～20mJ/cm-2The irradiation time is 5 min-30 min. The shape and size of the polyimide film sample 7 can be set according to actual needs, and are not limited to the size and shape in the following examples.
In an embodiment of the present invention, the step of preparing polyimide film sample 7 includes:
s11: cutting the polyimide film into a shape with a preset size;
s12: placing the cut polyimide film in absolute ethyl alcohol, and ultrasonically cleaning for 10-15 minutes at room temperature;
s13: placing the polyimide film cleaned by the absolute ethyl alcohol in deionized water, and ultrasonically cleaning for 10-15 minutes at room temperature;
s14: and taking out the polyimide film and putting the polyimide film into a thermostat for drying to obtain a polyimide film sample 7.
In order to prevent the irradiation effect from being affected by the excessively high moisture content of the polyimide film during the laser irradiation, the cleaned polyimide film needs to be placed in a thermostat for drying treatment. The temperature of the incubator can be set according to the actual situation, for example, the temperature can be 40 ℃ to 50 ℃, as long as the drying temperature does not damage the performance of the polyimide. After the polyimide film was dried, the polyimide film sample 7 was taken out from the oven.
Specific examples of the present invention are given below to illustrate a method for preparing polyimide having a periodic micro-nano structure.
First embodiment
Step 1: an optical path system matched with the excimer laser 1 is set up according to the figure 1, the laser frequency is adjusted to be 10Hz, and the energy density is adjusted to be 14.01mJ/cm by the rotational energy attenuator 3-2。
Step 2: cutting the polyimide film into square sheets with the side length of 15mm, and then soaking the cut polyimide film in absolute ethyl alcohol for ultrasonic cleaning for 10 minutes at room temperature. Then the polyimide film is fished out and put into deionized water to be ultrasonically cleaned for 10 minutes at room temperature. And finally, putting the polyimide film into a thermostat and drying.
And step 3: and (3) fixing the sample 7 prepared in the step (2) on a sample platform 5 in the optical path system built in the step (1), opening the excimer laser 1, setting the irradiation time to be 20min, and closing the excimer laser 1 after the irradiation is finished to obtain the polyimide film with the periodic micro-nano structure on the surface.
In the embodiment, the polyimide film prepared by the steps has a periodic micro-nano structure on the surface, the period of the periodic micro-nano structure is about 200nm, the surface roughness is 14.870nm, and the corrugation depth is 40 nm.
Second embodiment
Step 1: an optical path system matched with the excimer laser 1 is set up according to the graph 1, the laser frequency is adjusted to be 10Hz, and the energy density is adjusted to be 7.71mJ/cm by the rotation energy attenuator 3-2。
And 2, step: cutting the polyimide film into square sheets with the side length of 15mm, and then soaking the cut polyimide film in absolute ethyl alcohol for ultrasonic cleaning for 10 minutes at room temperature. Then the polyimide film is fished out and is put into deionized water for ultrasonic cleaning for 10 minutes at room temperature. And finally, putting the polyimide film into a thermostat and drying.
And step 3: and (3) fixing the sample 7 prepared in the step (2) on a sample platform 5 in the optical path system built in the step (1), opening the excimer laser 1, setting the irradiation time to be 20min, and closing the excimer laser 1 after the irradiation is finished to obtain the polyimide film with the periodic micro-nano structure on the surface.
In the embodiment, the polyimide film prepared by the steps has a periodic micro-nano structure on the surface, the period of the periodic micro-nano structure is about 200nm, the surface roughness is 5.693nm, and the corrugation depth is 16 nm.
Third embodiment
Step 1: an optical path system matched with the excimer laser 1 is set up according to the graph 1, the laser frequency is adjusted to be 10Hz, and the energy density is adjusted to be 9.86mJ/cm by rotating an attenuator-2。
Step 2: cutting the polyimide film into a square sheet with the side length of 15mm, and then soaking the cut polyimide film in absolute ethyl alcohol for ultrasonic cleaning for 10 minutes at room temperature. Then the polyimide film is fished out and put into deionized water to be ultrasonically cleaned for 10 minutes at room temperature. And finally, putting the polyimide film into a thermostat and drying.
And step 3: and (3) fixing the sample 7 prepared in the step (2) on a sample platform 5 in the optical path system built in the step (1), opening the excimer laser 1, setting the irradiation time to be 15min, and closing the excimer laser 1 after the irradiation is finished to obtain the polyimide film with the periodic micro-nano structure on the surface. The surface roughness of the film is 6.945nm, the corrugation depth is 18nm, and the corrugation period is about 200 nm.
In the embodiment, the polyimide film prepared by the steps has a periodic micro-nano structure on the surface, the period of the periodic micro-nano structure is about 200nm, the surface roughness is 6.945nm, and the corrugation depth is 18 nm.
Fourth embodiment
Step 1: an optical path system matched with the excimer laser 1 is built according to the graph 1, the laser frequency is adjusted to be 10Hz, and the energy density is adjusted to be 11.88mJ/cm by rotating an attenuator-2。
Step 2: cutting the polyimide film into square sheets with the side length of 15mm, and then soaking the cut polyimide film in absolute ethyl alcohol for ultrasonic cleaning for 10 minutes at room temperature. Then the polyimide film is fished out and put into deionized water to be ultrasonically cleaned for 10 minutes at room temperature. And finally, putting the polyimide film into a thermostat and drying.
And 3, step 3: and (3) fixing the sample 7 prepared in the step (2) on a sample platform 5 in the optical path system built in the step (1), opening the excimer laser 1, setting the irradiation time to be 20min, and closing the excimer laser 1 after the irradiation is finished to obtain the polyimide film with the periodic micro-nano structure on the surface.
In the embodiment, the polyimide film prepared by the steps has a periodic micro-nano structure on the surface, the period of the periodic micro-nano structure is about 200nm, the surface roughness is 14.870nm, and the corrugation depth is 40 nm.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; may be mechanically coupled, may be electrically coupled or may be in communication with each other; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (9)

1. The preparation method of the polyimide film with the periodic micro-nano structure is characterized in that the preparation of the periodic micro-nano structure on the surface of the polyimide film is carried out by adopting an optical path system of an excimer laser, and the optical path system of the excimer laser comprises an excimer laser (1) for emitting laser and a plurality of optical paths which are sequentially arranged along the conduction direction of the laser:
an energy attenuator (3), wherein the energy attenuator (3) is used for adjusting the energy of the laser;
a light homogenizer (4), the light homogenizer (4) being used for uniformly distributing the energy of the laser light emitted from the energy attenuator (3);
the preparation method of the polyimide film with the periodic micro-nano structure comprises the following steps of:
s1: preparing a polyimide film sample (7);
s3: fixing the polyimide film sample (7) on the sample platform (5);
s2: setting pulse laser parameters;
s4: opening the excimer laser (1), and irradiating the polyimide film sample (7) for a preset time;
s5: and closing the excimer laser (1) to obtain a polyimide film sample (7) with a periodic micro-nano structure.
2. The method for preparing a polyimide film with a periodic micro-nano structure according to claim 1, wherein the step of preparing a polyimide film sample (7) comprises:
s11: cutting the polyimide film into a shape with a preset size;
s12: placing the cut polyimide film in absolute ethyl alcohol, and ultrasonically cleaning for 10-15 minutes at room temperature;
s13: placing the polyimide film cleaned by the absolute ethyl alcohol in deionized water, and ultrasonically cleaning for 10-15 minutes at room temperature;
s14: and taking out the polyimide film and putting the polyimide film into a thermostat for drying to obtain a polyimide film sample (7).
3. The method for preparing the polyimide film with the periodic micro-nano structure according to claim 1, wherein the pulse laser parameters comprise laser frequency, energy density and irradiation time.
4. The preparation method of the polyimide film with the periodic micro-nano structure according to claim 3, wherein the laser frequency is 10Hz, and the energy density is within a range of 5mJ/cm-2～20mJ/cm-2The irradiation time ranges from 5min to 30 min.
5. The method for preparing the polyimide film with the periodic micro-nano structure according to claim 1, wherein the optical path system of the excimer laser further comprises an optical path changing component (2) positioned between the excimer laser (1) and the energy attenuator (3), the optical path changing component (2) comprises a plurality of totally reflecting mirrors (21) arranged at intervals, and the plurality of totally reflecting mirrors (21) are matched for changing the optical path route angle of the laser emitted from the excimer laser (1).
6. The preparation method of the polyimide film with the periodic micro-nano structure according to claim 1, wherein a mask (6) is further arranged between the sample platform (5) and the light homogenizer (4), the mask (6) is provided with an irradiation port (61), and the laser emitted from the light homogenizer (4) passes through the irradiation port (61) and is irradiated on the sample (7).
7. The preparation method of the polyimide film with the periodic micro-nano structure according to claim 6, wherein the irradiation port (61) is formed at a position corresponding to the sample (7), the area of the irradiation port (61) is larger than that of the sample (7), and the orthographic projection of the sample (7) is completely projected into the irradiation port (61).
8. The method for preparing the polyimide film with the periodic micro-nano structure according to claim 6, wherein the light homogenizer (4) comprises a first plano-convex mirror (42) and a light homogenizing sheet (41) positioned between the first plano-convex mirror (42) and the energy attenuator (3), the plane side of the first plano-convex mirror (42) is arranged towards the light homogenizing sheet (41), and the central line of the light homogenizing sheet (41) is coincided with the focus of the first plano-convex mirror (42).
9. The method for preparing the polyimide film with the periodic micro-nano structure according to claim 8, wherein a second plano-convex mirror (43) is further arranged between the first plano-convex mirror (42) and the mask (6), and a focus of the second plano-convex mirror (43) and a focus of the first plano-convex mirror (42) are located on the same straight line.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104439699A (en) * 2014-10-27 2015-03-25 中国科学院理化技术研究所 System and method for preparing micro-nano array structure by means of laser light
JP2017047185A (en) * 2015-09-04 2017-03-09 キヤノン株式会社 Ultrasonic wave device
CN107414284A (en) * 2017-09-04 2017-12-01 北京工业大学 A kind of PRK aids in micro- milling method and device
CN108821262A (en) * 2018-07-10 2018-11-16 常州大学 A method of utilizing semiconductor laser induction polyimide surface carbonization preparation nanometer high-specific surface area carbon particle
CN110385530A (en) * 2019-07-15 2019-10-29 中国科学院合肥物质科学研究院 A kind of method that quasi-molecule laser etching calcium fluoride crystal forms periodic stripe
CN210024165U (en) * 2019-03-06 2020-02-07 深圳大学 Nanofabrication system for producing structural colors

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104439699A (en) * 2014-10-27 2015-03-25 中国科学院理化技术研究所 System and method for preparing micro-nano array structure by means of laser light
JP2017047185A (en) * 2015-09-04 2017-03-09 キヤノン株式会社 Ultrasonic wave device
CN107414284A (en) * 2017-09-04 2017-12-01 北京工业大学 A kind of PRK aids in micro- milling method and device
CN108821262A (en) * 2018-07-10 2018-11-16 常州大学 A method of utilizing semiconductor laser induction polyimide surface carbonization preparation nanometer high-specific surface area carbon particle
CN210024165U (en) * 2019-03-06 2020-02-07 深圳大学 Nanofabrication system for producing structural colors
CN110385530A (en) * 2019-07-15 2019-10-29 中国科学院合肥物质科学研究院 A kind of method that quasi-molecule laser etching calcium fluoride crystal forms periodic stripe

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