CN104174999A - Method for preparing surface micro-nano figure through two steps - Google Patents
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- CN104174999A CN104174999A CN201410397449.6A CN201410397449A CN104174999A CN 104174999 A CN104174999 A CN 104174999A CN 201410397449 A CN201410397449 A CN 201410397449A CN 104174999 A CN104174999 A CN 104174999A
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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
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Abstract
The invention discloses a method for preparing a surface micro-nano figure through two steps. The method comprises the following steps: (1), coating a processing region on the surface of a to-be-processed material with a photosensitive polymeric material; (2), according to a micro-nano figure prepared on the surface of the to-be-processed material, designing the shape of a focusing element, performing multiphoton polymerization processing on photosensitive polymeric material through a femtosecond laser multiphoton polymerization processing device; (3), performing laser radiation on the focusing element through the laser processing device of the surface micro-nano figure, namely obtaining the micro-nano figure on the surface of the to-be-processed material. The method has the advantages as follows: the preparation process is simple and convenient, and the resolution ratio in focusing processing process is increased, so that the preparation of the surface submicron-nano figures is realized; the laser multiphoton polymerization processing method is adopted, so that three-dimensional structures with all shapes can be prepared on the surfaces of all solid materials, therefore, the method can be widely applied to preparation of micro-nano figures with complex surfaces and can realize the preparation of large-area surface micro-nano figures.
Description
Technical field
The present invention relates to a kind of method of utilizing two-step method to prepare surperficial micro-nano graph, belong to laser surface processing technical field.
Background technology
The superficiality of material, as friction, wearing and tearing, lubricated and adhesion etc., depends primarily on the surface nature of material, and the geometry of material surface is one of key factor affecting material surface character.The preparation of material surface geometry and performance study thereof are the study hotspots of sufacing in recent years.By prepare special geometric figure (Surface Texture) at material surface, can obtain required surface nature, relevant technology has broad application prospects.According to the difference of application background, the characteristic size of Surface Texture conventionally in millimeter magnitude to micron dimension, along with the development of micro-nano technology and for the demand of micro-nano device and structure, characteristic size became the research emphasis in this field at the surface microscopic geometry of sub-micron and nanometer scale in the last few years.
The method that obtains surface geometry has a variety of, comprise machining, electric machining, Ultrasonic machining, Laser Processing etc., wherein Laser Processing is due to its higher energy density, good monochromaticjty and collimation, noncontact processing and be applicable to the advantage of any solid material, thereby there is special advantage, be widely used in Surface Engineering field.Utilize the processing method comparative maturity of Laser Processing millimeter magnitude to micron dimension characteristic size texture, conventionally utilize condenser lens directly to focus on laser, irradiate and can obtain according to predefined figure or route.But due to the optical effect of laser self, cause the resolution ratio of Laser Processing infinitely not reduce, the resolution ratio that traditional laser processing obtains is difficult to break through the restriction of selected wavelength diffraction limit.Therefore,, obtaining sub-micron to aspect the Surface Texture of Nano grade, still need special method and technology.For example: the principle of the argon ion laser that the people such as Lo and Wang utilize 488nm based near field optic uses the method for near-field scan photoetching to realize groove processing (the Near-Field photolithography by a fiber probe.Proceedings of the 2001 1st IEEE Conference on Nanotechnology of width 128nm, 2001,36-39), but utilize near field optic principle to carry out Surface Machining to be very limited aspect practical.Lu carries out laser micro/nano processing with Quartz Microsphere as focusing system, and the characteristic size of processing pattern can reach 220-700nm (Laser Material Processing and Characterization at Micro/Nano-scales.Advanced Program on 8
thchina National Conference on Laser Material Processing-CNCLMP, 2006), but microballoon is mainly used in the processing of dots structure, and the aspect such as sprawls at microballoon by assigned address and have inconvenience.The method that the people such as Shao Tianmin focus on based on optical fibers utilizes the pulse laser of wavelength 1.06 μ m, pulsewidth 10ns to prepare groove (the material surface laser micromachining methods and the device that focus on based on optical fibers: China of width 3.74 μ m at material surface, 200810008077.8[P] .2008-03-07), optical fibers focuses on processing method simply and has very high working (machining) efficiency, under the effect of individual pulse, can obtain the groove that length-width ratio is greater than 1000:1.Although optical fibers focus method can obtain the exercising result of near-field effect, the difficulty of placing in surperficial near-field region due to fine optical fiber is larger, and preparation surfacial pattern mostly be linear pattern, be difficult to realize the preparation of complex figure.
Summary of the invention
The object of this invention is to provide a kind of method of utilizing " two-step method " to prepare surperficial micro-nano graph, the present invention utilizes laser multi-photon polymerization process to prepare concentrating element, thereby and apply prepared concentrating element laser focused at material surface to be processed and obtains surperficial micro-nano graph; The present invention is the preparation method of a kind of efficient controlled surperficial sub-micron to nanoscale surfacial pattern.
The method of utilizing two-step method to prepare surperficial micro-nano graph provided by the present invention, comprises the steps:
(1) apply photopolymer materials at the machining area of material surface to be processed;
(2) according to the shape of the micro-nano graph design concentrating element of preparing at material surface to be processed, utilize femtosecond laser multiphoton polymerization processing unit (plant) to carry out multiphoton polymerization processing to described photopolymer materials, obtain described concentrating element at the machining area of material surface to be processed;
Described femtosecond laser multiphoton polymerization processing unit (plant) comprises femto-second laser;
(3) utilize the laser processing device of surperficial micro-nano graph to carry out Ear Mucosa Treated by He Ne Laser Irradiation to described concentrating element, obtain micro-nano graph at material surface to be processed;
The laser processing device of described surperficial micro-nano graph comprises pulse laser.
In above-mentioned method, in step (1), described photopolymer materials can be photosensitive polymer, organic ceramic or semi-conducting material;
Described photosensitive polymer specifically can be photoresist, dimethyl silicone polymer; Described photoresist can select code name to can be the negative photoresist of IP-L, specifically purchased from German Nanoscribe company;
Described organic ceramic specifically can be organic decoration pottery, specifically purchased from German Nanoscribe company;
Described semiconductor specifically can be chalcogenide glass, as arsenic trisulphide glass.
In above-mentioned method, in step (2), form described concentrating element taking spheroid or cylinder as processing base unit;
Described spheroid and described cylindrical diameter are all less than 5 μ m, as 200nm～300nm, 200nm～400nm, 200nm～600nm, 200nm～800nm, 300nm～800nm, 300nm～600nm, 300nm～400nm, 400nm～800nm, 400nm～600nm, 600nm～800nm, 200nm～3 μ m, 200nm～2 μ m, 200nm～1 μ m, 400nm～3 μ m, 200nm, 300nm, 400nm, 600nm, 800nm, 1 μ m, 2 μ m or 3 μ m.
In above-mentioned method, in step (2), the condition of controlling described femto-second laser is as follows:
Optical maser wavelength is selected the many times of wavelength range of levying absorbing wavelength that comprise described photopolymer materials, specifically can be 775nm～1550nm;
Pulse width can be 10fs～200fs;
Repetition rate can be 20MHz～100MHz;
Power can be 1mW～100mW.
In above-mentioned method, in step (3), the condition of controlling described pulse laser is as follows:
Wavelength is selected to comprise described photopolymer materials feature transmissivity 90% above wavelength range, specifically can be 266nm～1064nm;
Pulsewidth can be nanosecond, picosecond or femtosecond, is correspondingly produced by nanosecond laser, picosecond laser or femto-second laser;
Can trigger single pulse mode, single pulse energy metric density can be 0.1J/cm
2～5J/cm
2, specifically can be 0.5J/cm
2～1.2J/cm
2, 0.5J/cm
2or 1.2J/cm
2.
In the inventive method, in step (2) afterwards, the described photopolymer materials of the unprocessed remnants of the most handy cleaning solvent ultrasonic cleaning, specifically selects the not corresponding cleaning solvent of described photopolymer materials of polymerization reaction take place of solubilized;
In step (3) afterwards, the most handy cleaning solvent surface cleaning material surface concentrating element of polymerization, specifically selects the solubilized corresponding cleaning solvent of described photopolymer materials of polymerization reaction take place.
Can choose as required material to be processed, select to can be solid material, as polysilicon.
Compared with prior art, the present invention has the following advantages:
(1) the present invention has adopted laser multi-photon polymerization technique, and the photopolymer materials of the Multiphoton Absorbtion characteristic with femtosecond laser is had to higher machining resolution, and can prepare minimum diameter is the concentrating element of 100nm left and right.
(2) in the present invention, photosensitive polymerization reacts the surface that directly occurs in material to be processed, therefore can produce processing effect near field at concentrating element to the focussing force link of incident laser, further improve the resolution ratio that focuses on process, thereby realize the preparation of surperficial sub-micron to Nano grade figure.
(3) because the controllability of laser multi-photon polymerization process method is strong, live width and the degree of depth of preparing pattern can regulate by the three-dimensional structure of concentrating element and for the laser parameter of follow-up focusing processing, therefore the present invention can prepare at any solid material surface the three-dimensional structure of arbitrary shape, therefore can be widely used in the preparation of surperficial complicated micro-nano graph.
(4) processing of femtosecond laser multiphoton polymerization has higher working (machining) efficiency, and prepared concentrating element characteristic size majority is in sub-micrometer scale, therefore concentrating element preparation process is easy, is easy to large area and prepares concentrating element to realize the preparation of large-area surfacial pattern.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph of the different-diameter column type concentrating element prepared of the embodiment of the present invention 1.
Fig. 2 is the electron scanning micrograph of the submicron order surfacial pattern prepared of the embodiment of the present invention 1.
Fig. 3 is the electron scanning micrograph of the different-diameter column type concentrating element prepared of the embodiment of the present invention 2.
Fig. 4 is the electron scanning micrograph of the submicron order surfacial pattern prepared of the embodiment of the present invention 2.
Detailed description of the invention
The experimental technique using in following embodiment if no special instructions, is conventional method.
Material, reagent etc. used in following embodiment, if no special instructions, all can obtain from commercial channels.
Embodiment 1, polysilicon surface use femto-second laser prepare micro-nano graph
1, utilize femtosecond laser multiphoton polymerization processing method, prepare concentrating element at polysilicon surface according to required graphics request
(1) select polysilicon as material to be processed, evenly apply IP-L photoresist (purchased from German Nanoscribe company) in its centre of surface region, the characteristic absorption wave band of IP-L photoresist is at 180nm～320nm.
(2) as required, intend preparing different in width strip groove at polysilicon surface.By calculating, (circular is as follows: utilize Finite Difference Time Domain (FDTD), the energy field of the cylinder polymeric component of calculating different in width diameter under laser action distributes, and compares and draws working width with material damage threshold value; Concrete software for calculation is the FDTD Solutions (V8.0) of Lumerical company.) optical field distribution of concentrating element after for Laser Focusing, the different cylinder polymeric component of design five diameters of polymerization.
(3) build femtosecond laser multiphoton polymerization processing unit (plant), comprise titanium sapphire femto-second laser and three-dimensional processing displacement platform.According to the shape of concentrating element, utilize above-mentioned femtosecond laser multiphoton polymerization processing unit (plant) to carry out multiphoton polymerization processing to IP-L photoresist, the operating condition of controlling titanium sapphire femto-second laser is: optical maser wavelength 780nm, pulsewidth 120fs, repetition rate 100MHz, power 5mW.Under these conditions, can trigger the Three-photon absorption of this femto-second laser is produced to polymerisation, IP-L photoresist can produce Three-photon absorption polymerization reaction take place and solidify through the region of femtosecond laser scanning.
(4) regulate three-dimensional processing displacement platform, titanium sapphire femtosecond laser, by the mode of scanning, is realized the multiphoton polymerization processing for preset shape.
Obtain different-diameter column type concentrating element, as shown in Figure 1, diameter is followed successively by 200nm, 400nm, 1 μ m, 2 μ m and 3 μ m to its electron scanning micrograph from left to right; Cylinder length is 200 μ m, and between cylinder, spacing is 50 μ m.
(5) application absolute ethyl alcohol ultrasonic cleaning 20 minutes, removes remaining uncured IP-L photoresist, obtains concentrating element.
2, carry out Ear Mucosa Treated by He Ne Laser Irradiation for the polysilicon on surface polymerization concentrating element, by concentrating element, incident laser is focused on, realize the graphical processing of polysilicon surface
(1) build the laser processing device of surperficial micro-nano graph, comprise titanium sapphire femto-second laser and three-dimensional processing displacement platform, the concentrating element of above-mentioned preparation is carried out to Ear Mucosa Treated by He Ne Laser Irradiation.
Because curing IP-L photoresist exceedes 99% for the transmissivity of the above laser wavelength of 390nm, therefore the operating condition of controlling titanium sapphire femto-second laser is as follows: wavelength 800nm, pulsewidth 120fs, pulse trigger mode, it is 1.2J/cm that adjusting energy makes single pulse energy metric density
2.
(2) focal position and the spot size of adjusting laser instrument, regulates three-dimensional processing displacement platform, applies individual pulse, obtains required surperficial micro-nano graph.
(3) application acetone ultrasonic cleaning polysilicon 20 minutes, removes curing IP-L photoresist.
Obtain the electron scanning micrograph of micro-nano graph as shown in Figure 2, obtain for IP-L cylinder concentrating element by 200nm in Fig. 1 focuses on, its width is 210nm, and the degree of depth is 30nm.
Embodiment 2, polysilicon surface use nanosecond laser prepare micro-nano graph
1, utilize femtosecond laser multiphoton polymerization processing method, prepare concentrating element at polysilicon surface according to required graphics request
(1) select polysilicon as material to be processed, evenly apply IP-L photoresist (purchased from German Nanoscribe company) in its centre of surface region, the characteristic absorption wave band of IP-L photoresist is at 180nm～320nm.
(2) as required, intend preparing different in width strip groove at polysilicon surface.By calculating, (circular is as follows: utilize Finite Difference Time Domain (FDTD), the energy field of the cylinder polymeric component of calculating different in width diameter under laser action distributes, and compares and draws working width with material damage threshold value; Concrete software for calculation is the FDTD Solutions (V8.0) of Lumerical company.) optical field distribution of concentrating element after for Laser Focusing, the different cylinder polymeric component of design five diameters of polymerization.
(3) build femtosecond laser multiphoton polymerization processing unit (plant), comprise titanium sapphire femto-second laser and three-dimensional processing displacement platform.According to the shape of concentrating element, utilize above-mentioned femtosecond laser multiphoton polymerization processing unit (plant) to carry out multiphoton polymerization processing to IP-L photoresist, the operating condition of controlling titanium sapphire femto-second laser is: optical maser wavelength 780nm, pulsewidth 120fs, repetition rate 100MHz, power 5mW.Under these conditions, can trigger the Three-photon absorption of this femto-second laser is produced to polymerisation, IP-L photoresist can produce Three-photon absorption polymerization reaction take place and solidify through the region of femtosecond laser scanning.
(4) regulate three-dimensional processing displacement platform, titanium sapphire femtosecond laser, by the mode of scanning, is realized the multiphoton polymerization processing for preset shape.
Obtain different-diameter column type concentrating element, as shown in Figure 3, diameter is followed successively by 200nm, 300nm, 400nm, 600nm and 800nm to its electron scanning micrograph from left to right; Cylinder length is 200 μ m, and between cylinder, spacing is 50 μ m.
(5) application absolute ethyl alcohol ultrasonic cleaning 20 minutes, removes remaining uncured IP-L photoresist, obtains concentrating element.
2, carry out Ear Mucosa Treated by He Ne Laser Irradiation for the polysilicon on surface polymerization concentrating element, by concentrating element, incident laser is focused on, realize the graphical processing of polysilicon surface
(1) build the laser processing device of surperficial micro-nano graph, comprise YAG nanosecoud pulse laser and three-dimensional processing displacement platform, the concentrating element of above-mentioned preparation is carried out to Ear Mucosa Treated by He Ne Laser Irradiation.
Because curing IP-L photoresist exceedes 99% for the transmissivity of the above laser wavelength of 390nm, therefore the operating condition of controlling YAG nanosecoud pulse laser is as follows: wavelength 532nm, pulsewidth 8ns, pulse trigger mode, it is 0.5J/cm that adjusting energy makes single pulse energy metric density
2.
(2) focal position and the spot size of adjusting laser instrument, regulates three-dimensional processing displacement platform, applies individual pulse, obtains required surperficial micro-nano graph.
(3) application acetone ultrasonic cleaning polysilicon 20 minutes, removes curing IP-L photoresist.
Obtain the electron scanning micrograph of micro-nano graph as shown in Figure 4, obtain for IP-L cylinder concentrating element by 200nm in Fig. 1 focuses on, its width is 129.65nm, and the degree of depth is 10nm.
Above-described embodiment is only for illustrating the present invention, and wherein the step of implementation method all can change to some extent, and every equivalents of carrying out on the basis of technical solution of the present invention and improvement, all should not get rid of outside protection scope of the present invention.
Claims (5)
1. utilize two-step method to prepare the method for surperficial micro-nano graph, comprise the steps:
(1) apply photopolymer materials at the machining area of material surface to be processed;
(2) according to the shape of the micro-nano graph design concentrating element of preparing at material surface to be processed, utilize femtosecond laser multiphoton polymerization processing unit (plant) to carry out multiphoton polymerization processing to described photopolymer materials, obtain described concentrating element at the machining area of material surface to be processed;
Described femtosecond laser multiphoton polymerization processing unit (plant) comprises femto-second laser;
(3) utilize the laser processing device of surperficial micro-nano graph to carry out Ear Mucosa Treated by He Ne Laser Irradiation to described concentrating element, obtain micro-nano graph at material surface to be processed;
The laser processing device of described surperficial micro-nano graph comprises pulse laser.
2. method according to claim 1, is characterized in that: in step (1), described photopolymer materials is photosensitive polymer, organic ceramic or semi-conducting material.
3. method according to claim 1 and 2, is characterized in that: in step (2), form described concentrating element taking spheroid or cylinder as processing base unit;
Described spheroid and described cylindrical diameter are all less than 5 μ m.
4. according to the method described in any one in claim 1-3, it is characterized in that: in step (2), the condition of controlling described femto-second laser is as follows:
Optical maser wavelength is 775nm～1550nm;
Pulse width is 10fs～200fs;
Repetition rate is 20MHz～100MHz;
Power is 1mW～100mW.
5. according to the method described in any one in claim 1-4, it is characterized in that: in step (3), the condition of controlling described pulse laser is as follows:
Wavelength is 266nm～1064nm;
Pulsewidth is nanosecond, picosecond or femtosecond;
Can trigger single pulse mode, single pulse energy metric density is 0.1J/cm
2～5J/cm
2.
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| CN109362239A (en) * | 2016-03-23 | 2019-02-19 | 南非大学 | The method that micro-nano contraction structure is prepared on YBa2Cu3O7-X superconducting thin film based on femtosecond laser |
| CN110456614A (en) * | 2019-07-18 | 2019-11-15 | 北京工业大学 | A kind of femtosecond laser inside photopolymerization direct write processing method of methacrylic acid gelatin hydrogel |
| CN112756777A (en) * | 2020-12-29 | 2021-05-07 | 华中科技大学 | Laser blackening treatment method for metal surface |
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