CN114591527A - Preparation method of polymer film surface periodic structure regulated by laser wavefront - Google Patents
Preparation method of polymer film surface periodic structure regulated by laser wavefront Download PDFInfo
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- CN114591527A CN114591527A CN202210223641.8A CN202210223641A CN114591527A CN 114591527 A CN114591527 A CN 114591527A CN 202210223641 A CN202210223641 A CN 202210223641A CN 114591527 A CN114591527 A CN 114591527A
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- 230000000737 periodic effect Effects 0.000 title claims abstract description 59
- 229920006254 polymer film Polymers 0.000 title claims abstract description 27
- 230000001105 regulatory effect Effects 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 15
- 229920001721 polyimide Polymers 0.000 claims description 17
- 229920000642 polymer Polymers 0.000 claims description 15
- 230000010287 polarization Effects 0.000 claims description 13
- 239000004642 Polyimide Substances 0.000 claims description 12
- 238000002679 ablation Methods 0.000 claims description 9
- 230000003287 optical effect Effects 0.000 claims description 9
- -1 polytrimethylene terephthalate Polymers 0.000 claims description 6
- 230000001276 controlling effect Effects 0.000 claims description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 4
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 4
- 229920002215 polytrimethylene terephthalate Polymers 0.000 claims description 4
- 239000004793 Polystyrene Substances 0.000 claims description 3
- 229920000515 polycarbonate Polymers 0.000 claims description 3
- 239000004417 polycarbonate Substances 0.000 claims description 3
- 238000013519 translation Methods 0.000 claims description 3
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 230000033228 biological regulation Effects 0.000 claims 2
- 230000001939 inductive effect Effects 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 31
- 238000012545 processing Methods 0.000 abstract description 9
- 230000008859 change Effects 0.000 abstract description 4
- 238000002310 reflectometry Methods 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 6
- 239000002861 polymer material Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000002910 structure generation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/123—Treatment by wave energy or particle radiation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- Laser Beam Processing (AREA)
Abstract
The invention discloses a preparation method of a polymer film surface periodic structure regulated by laser wavefront, which comprises the following steps: the method comprises the steps of preparing a micron-order periodic stripe structure on the surface of a polymer film by using ultraviolet nanosecond laser, wherein the direction of the periodic stripe structure can be changed by shaping the wave front of the laser, and the period of the periodic stripe structure can be regulated and controlled by the energy density and the number of pulses of incident laser. The periodic stripe structure prepared on the surface of the polymer film can change the friction characteristic and reflectivity of the material, realize micron-scale morphology control, and meet the micron-scale processing requirements of parts with special requirements such as high precision, difficult processing, complex surface shape and the like.
Description
Technical Field
The invention belongs to a nanosecond laser-induced polymer material surface periodic structure preparation technology, and particularly relates to a preparation method of a polymer film surface periodic structure regulated by laser wavefront.
Background
The laser induced material surface periodic structure is a means for realizing micro-nano processing of the material surface, and the shape control of the micro-nano scale is realized through the interaction of the laser and the material, so that the physical state and the property of the material are changed. Compared with other micro-nano manufacturing modes, the laser micro-nano manufacturing method can meet the manufacturing requirements of parts with special requirements on high precision, high surface quality and the like, can process special materials such as difficult-to-machine materials, complex surface materials, micro parts and extremely-low-rigidity members, and has the advantages of non-contact, precision controllability, high efficiency, energy conservation and the like. Furthermore, the materials used for this type of processing are very wide, for example, metals, semiconductors, dielectrics as mentioned in the documents "Martin E, Bing H, FrankF, et al, Generation of laser-induced periodic Surface structures (LIPSS) in fused silica by single NIR nano-second laser pulse irradiation in applied Surface Science,2019,470: 56-62", "YuFan G, CaiYu Y, Bing H, et al, Pico-second laser-induced periodic Surface structures (LIPSS) on crystalline silicon, Surface and Interfaces,2020,100538", U.S. Pat. No. 5/0083984A 1, Wo/065356A 1. Generally, a laser induced surface periodic structure (LIPSS) is generated under laser irradiation in a certain energy density range and pulse number, the energy density threshold of laser generated by a common periodic structure is close to or slightly smaller than the ablation threshold of a material, the period is generally close to the wavelength or half of the wavelength of incident laser, and is regulated and controlled by the energy density, the pulse number and the incident angle of the laser, and the orientation of the LIPSS is determined by the polarization direction of the laser. Researchers have proposed many principles of LIPSS generation based on different materials and different processing conditions, and widely include generalized scattering and interference (Sipe) models, Surface Plasmon Polariton (SPP) assisted formation models, second harmonic models, and capillary wave models. However, there is no theory that is applicable to the characteristics of LIPSS formation, the mechanism of LIPSS formation remains worth discussion, and how to effectively and periodically regulate LIPSS remains a key point of concern.
The periodic structure is prepared on the surface of the polymer material by using laser, the mechanical property, the optical property, the wetting property and the like of the material can be changed, and the material has wide application prospect in the fields of optics, biomedicine, microelectronics, aerospace, aviation and the like. At present, the research on the laser-induced surface periodic structure of the polymer material is less, the generated structural period is mostly one half, one time or two times of the wavelength of the incident laser, and the direction of the periodic structure is only related to the polarization direction of the laser. With the advent of ultrashort pulse lasers, there has been less research on the use of nanosecond laser systems to fabricate periodic structures. However, the equipment cost of the ultrashort pulse laser is high, and the cold processing effect after the material is irradiated is different from the mechanism that the thermal effect is dominant when the nanosecond laser interacts with the substance. Therefore, the research on the periodic structure generation of the polymer surface induced by nanosecond laser irradiation still has certain scientific significance.
Disclosure of Invention
The invention aims to provide a preparation method of a polymer film surface periodic structure regulated by laser wavefront, which solves the problem that the prior art is difficult to prepare a micron-scale periodic structure on the surface of a polymer.
The technical solution for realizing the invention is as follows: a preparation method of a polymer film surface periodic structure regulated by laser wavefront comprises the following steps:
ultraviolet nanosecond laser passes through a half-wave plate and a polarization beam splitting prism, and is focused on the surface of the polymer film through a beam shrinking system combined by a concave-convex lens to form a periodic structure, wherein the number of pulses with the laser energy density higher than the ablation threshold value of the polymer film is 1-50.
Preferably, the laser fluence is 1.5-20 times the ablation threshold.
Preferably, the method for determining the single pulse energy density and the number of pulses of the ultraviolet nanosecond laser comprises the following steps:
rotating the half-wave plate, changing the included angle between the polarization direction of the emergent laser and the fast axis or the slow axis of the half-wave plate, adjusting the energy to the target by using the polarization splitting prism combination, measuring the energy to the target by using an energy meter, and determining the energy sizes corresponding to different scales of the half-wave plate and the scale value corresponding to the maximum or minimum target energy;
placing a sample on a three-dimensional translation table, rotating a half-wave plate to a position of half the maximum energy, moving the sample along a direction parallel to an optical axis, and changing the laser energy density to a target by controlling the distance position between the target and a focus;
under the condition that the energy density of the laser to the target is not changed, the number of the laser pulses to the target is changed, and the energy density threshold value and the number of pulses threshold value of the micron-scale periodic structure prepared on the surface of the polymer film are determined.
Preferably, the polymer is any one of polyimide, polystyrene, polycarbonate, polytrimethylene terephthalate and polyethylene terephthalate.
Preferably, a slit is arranged between the polymer and the beam-shrinking system, the shape of the laser wavefront is controlled through the slit, periodic structures in different directions are prepared on the surface of the polymer, and the direction of the periodic structures is perpendicular to the slit.
Preferably, the laser wavelength is in the ultraviolet band.
Preferably, the laser wavelength is 355 nm.
Preferably, the laser is linearly polarized light with a pulse width of 7ns, and the laser focal spot diameter of the polymer surface is between 90 μm and 130 μm.
Preferably, the slit width of the introduced slit is smaller than the diameter of the laser beam.
Preferably, the distance from the center of the slit to the target is greater than 0mm and less than 35 mm.
Compared with the prior art, the invention has the following remarkable advantages: 1) the invention can prepare micron-scale periodic stripe structures on parts with complex surface types, difficult processing and special requirements by a non-contact processing means; 2) the invention can control the direction of the stripes by a simple device; 3) the invention can change the optical characteristics of the material surface, realize information transmission by utilizing the material surface and improve the cell growth characteristics on the material surface with better biocompatibility; 4) the invention is suitable for micro-nano processing of various surface materials; 5) the invention is suitable for preparing grating structures on micro optical devices and optical storage devices; 6) the invention does not need vacuum experimental environment.
The present invention is described in further detail below with reference to the attached drawings.
Drawings
FIG. 1 is a schematic diagram of an experiment for generating a laser-induced periodic structure on the surface of a polymer film material with a direction controlled by a wavefront.
FIG. 2 is a graph showing the results of an optical microscope for producing LIPSS on the surface of a Polyimide (PI) film according to example 1.
FIG. 3 is a periodic distribution diagram of the periodic structure on the surface of the Polyimide (PI) film under different laser energy densities and different pulse numbers in example 1.
FIG. 4 is a schematic diagram of an experimental result of the embodiment 1 that the period of the periodic stripe structure induced on the surface of the PI film by the ultraviolet nanosecond laser changes along with the change of the laser energy density.
FIG. 5 is a schematic diagram of experimental results of embodiment 1, in which the period of the periodic fringe structure induced by the ultraviolet nanosecond laser on the surface of the PI film changes with the number of laser pulses.
FIG. 6 is a graph of experimental results of laser irradiation on a material surface to form different wavefront features by changing the slit direction.
Detailed Description
As shown in figure 1, in a method for preparing a periodic structure on the surface of a polymer film regulated by laser wavefront, a periodic stripe structure with controllable period and direction changing along with the wavefront is generated on the surface of the polymer film within a set laser parameter interval. The method specifically comprises the following steps:
ultraviolet nanosecond laser passes through a half-wave plate and a polarization beam splitting prism, and is focused on the surface of the polymer film through a beam shrinking system combined by a concave-convex lens, and the centers of all optical components are coaxial. The combination of the concave lens and the convex lens plays a role in beam shrinking, the area of a light spot is reduced, the energy density of a target is increased, the longer the focal length of the combination system is, the slower the energy density change is, the more accurately the threshold value of LIPSS can be determined, and the combination of the concave lens and the convex lens also plays a role in correcting aberration, so that the wavefront of the target is better. The combination of the half-wave plate and the polarization beam splitter prism achieves the energy adjustment.
The energy density of the single pulse of the ultraviolet nanosecond laser is higher than the ablation threshold of the polymer material, and the number of pulses is 1 to 50.
Specifically, the laser fluence is 1.5-20 times the ablation threshold.
In some embodiments, the method for determining the energy density of the single pulse and the number of pulses of the ultraviolet nanosecond laser comprises the following steps:
rotating the half-wave plate (the precision is 2 degrees), changing the included angle between the polarization direction of the emergent laser and the fast (slow) axis of the half-wave plate, adjusting the target energy by utilizing the polarization splitting prism combination, measuring the target energy by adopting an energy meter, and determining the energy sizes corresponding to different scales of the half-wave plate and the scale value corresponding to the maximum or minimum target energy.
And placing the sample on a three-dimensional translation table with the precision of 1 mu m, rotating the half-wave plate to the position of half of the maximum energy, moving the sample along the direction parallel to the optical axis, and changing the laser energy density of the target by controlling the distance position of the target and the focus, but keeping the target in front of the focus all the time.
Under the condition that the energy density of the laser to the target is not changed, the number of the laser pulses to the target is changed, and the energy density threshold value and the number of pulses threshold value of the micron-scale periodic structure prepared on the surface of the polymer film are determined.
In some embodiments, the target may be a polymer having a high absorption rate to the laser light in the ultraviolet band, such as Polyimide (PI), Polystyrene (PS), Polycarbonate (PC), polytrimethylene terephthalate (PTT), polyethylene terephthalate (PET), or the like. The laser energy density range is higher than the ablation threshold of the material, so that the temperature rise of the surface of the material is higher than the viscous flow temperature of the material, the material is converted from a glass state to a high elastic state and then to a viscous flow state, polymer molecular chains move and enter an unstable state, the material is irreversibly deformed, and then the material is cooled, and a periodic structure is formed on the surface. As shown in FIG. 2, the polymer surface acted by laser forms a periodic structure, the structure period is in micron order, the grid-like structure (stripe) has consistent orientation, and the regularity is better. As shown in fig. 3, the periodic structure is controlled by parameters including laser energy density and pulse number, and it is found through various examples that the period of the periodic stripe structure increases with the increase of the incident laser energy density, and a relation graph of the period changing with the energy density is shown in fig. 4; the graph showing the variation of the period with the laser pulse as the number of incident pulses increases is shown in fig. 5, but the periodic structure is always located at the bottom of the ablation pit until the thin film is broken.
In a further embodiment, after the generation threshold of the periodic structure is determined, a slit is introduced at a position close to the front of the experimental sample, the slit is rotated to control the laser wavefront morphology, and periodic structures in different directions can be prepared on the surface of the polymer, wherein the structure direction is always perpendicular to the slit, as shown in fig. 6. If the periodic structure is caused by laser light diffracting through the slit, the direction of the stripe should be parallel to the slit, so as to eliminate the influence of diffraction effect.
In a further embodiment, the laser wavelength in step 1 is in the ultraviolet band.
In a further embodiment, the laser wavelength is 355 nm.
In a further embodiment, the laser in step 1 is linearly polarized light with a pulse width of 7ns, and the laser focal spot diameter of the polymer surface is between 90 μm and 130 μm.
In a further embodiment, the laser has a focal spot diameter of 94 μm incident on the surface of the polymer material.
In a further embodiment, a polyimide film is used having a thickness of between 0 μm and 30 μm.
In a further embodiment, the slit width of the introduced slit is smaller than the diameter of the laser beam and is 80 μm.
In a further embodiment, the position of the slit center from the target is more than 0mm and less than 35mm, i.e. the slit is close to the target but still has a certain distance.
In a further embodiment, the polymer material film has a thickness of 30 μm.
Example 1
The technical scheme of the invention is described in detail by taking the process of preparing the periodic structure regulated by the laser wavefront on the surface of the Polyimide (PI) film material as an example.
(1) A polyimide film material having a thickness of 30 μm was used.
(2) The laser with the wavelength of 355nm and the pulse width of 7ns and linear polarization is selected as a light source and is focused on the surface of the material through a beam shrinking system.
(3) The beam-shrinking system is composed of a convex lens with a focal length f equal to 50mm and a concave lens with a focal length f equal to-25 mm, and the distance d is equal to 33 mm.
(4) The laser energy density range is 54J/cm2-586J/cm2And the number of pulses is 1-50. The spot diameter on the surface of the material is 94 μm.
(5) The slits were positioned at a distance of 28mm from the center of the material and 80 μm in width, and were arranged vertically or horizontally.
The embodiment is suitable for generating a periodic stripe structure with a period between 4 mu m and 7 mu m on the surface of the polyimide film, regulating and controlling the period of the stripe structure by changing the laser energy density and the number of pulses respectively, and introducing the slit to control the direction of the stripe, wherein the direction of the stripe is always vertical to the slit.
Claims (10)
1. A preparation method of a polymer film surface periodic structure regulated by laser wavefront is characterized by comprising the following steps:
ultraviolet nanosecond laser passes through a half-wave plate and a polarization beam splitting prism, and is focused on the surface of the polymer film through a beam shrinking system combined by a concave-convex lens to form a periodic structure, wherein the number of pulses with the laser energy density higher than the ablation threshold value of the polymer film is 1-50.
2. The method for preparing the polymer film surface periodic structure regulated by the laser wavefront as claimed in claim 1, wherein the laser energy density is 1.5-20 times of the ablation threshold.
3. The preparation method of the polymer film surface periodic structure regulated by the laser wavefront as claimed in claim 1, wherein the determination method of the ultraviolet nanosecond laser single pulse energy density and the number of pulses comprises:
rotating the half-wave plate, changing the included angle between the polarization direction of the emergent laser and the fast axis or the slow axis of the half-wave plate, adjusting the energy to the target by using the polarization splitting prism combination, measuring the energy to the target by using an energy meter, and determining the energy sizes corresponding to different scales of the half-wave plate and the scale value corresponding to the maximum or minimum target energy;
placing a sample on a three-dimensional translation table, rotating a half-wave plate to a position of half the maximum energy, moving the sample along a direction parallel to an optical axis, and changing the laser energy density to a target by controlling the distance position between the target and a focus;
under the condition that the energy density of the laser to the target is not changed, the number of the laser pulses to the target is changed, and the energy density threshold value and the number of pulses threshold value of the micron-scale periodic structure prepared on the surface of the polymer film are determined.
4. The method for preparing the polymer film surface periodic structure regulated by the laser wavefront as claimed in claim 1, wherein the polymer is any one of polyimide, polystyrene, polycarbonate, polytrimethylene terephthalate and polyethylene terephthalate.
5. The method for preparing the polymer film surface periodic structure regulated by the laser wavefront as claimed in claim 1, wherein a slit is arranged between the polymer and the beam shrinking system, the laser wavefront morphology is controlled through the slit, the periodic structures in different directions are prepared on the polymer surface, and the direction of the periodic structures is perpendicular to the slit.
6. The method for preparing the polymer film surface periodic structure modulated by the laser wavefront as claimed in claim 1, wherein the laser wavelength is in the ultraviolet band.
7. The method for preparing the polymer film surface periodic structure modulated by the laser wavefront as claimed in claim 6, wherein the laser wavelength is 355 nm.
8. The preparation method of the polymer film surface periodic structure regulated by the laser wavefront as claimed in claim 1, wherein the laser is linearly polarized light, the pulse width is 7ns, and the laser focal spot diameter of the polymer surface is between 90 μm and 130 μm.
9. The method for inducing the periodic structure of the polyimide film with the wavefront regulation in the surface direction by the nanosecond laser according to the claim 1, wherein the width of the introduced slit is smaller than the diameter of the laser beam.
10. The method for inducing the periodic structure of the polyimide film with the wavefront regulation and control in the surface direction by the nanosecond laser as claimed in claim 1, wherein the distance from the center of the slit to the target is greater than 0mm and less than 35 mm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080299408A1 (en) * | 2006-09-29 | 2008-12-04 | University Of Rochester | Femtosecond Laser Pulse Surface Structuring Methods and Materials Resulting Therefrom |
| CN103193999A (en) * | 2013-03-29 | 2013-07-10 | 西南科技大学 | Method and equipment for preparing strip structures on conjugated polymer surfaces through pulse lasers |
| CN109277692A (en) * | 2018-12-04 | 2019-01-29 | 湘潭大学 | Dimethyl silicone polymer surface micro-nano structure femtosecond double pulses regulate and control method |
| CN111168233A (en) * | 2020-02-14 | 2020-05-19 | 南京理工大学 | Method for inducing periodic structure on surface of optical glass by picosecond laser |
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- 2022-03-07 CN CN202210223641.8A patent/CN114591527A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080299408A1 (en) * | 2006-09-29 | 2008-12-04 | University Of Rochester | Femtosecond Laser Pulse Surface Structuring Methods and Materials Resulting Therefrom |
| CN103193999A (en) * | 2013-03-29 | 2013-07-10 | 西南科技大学 | Method and equipment for preparing strip structures on conjugated polymer surfaces through pulse lasers |
| CN109277692A (en) * | 2018-12-04 | 2019-01-29 | 湘潭大学 | Dimethyl silicone polymer surface micro-nano structure femtosecond double pulses regulate and control method |
| CN111168233A (en) * | 2020-02-14 | 2020-05-19 | 南京理工大学 | Method for inducing periodic structure on surface of optical glass by picosecond laser |
Non-Patent Citations (1)
| Title |
|---|
| 林素颖: "纳秒激光诱导聚酰亚胺薄膜周期性结构的产生", 《红外与激光工程》 * |
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Application publication date: 20220607 |