CN116511719A - Method and system for preparing micro-nano structure by laser-electron beam and micro-nano structure - Google Patents
Method and system for preparing micro-nano structure by laser-electron beam and micro-nano structure Download PDFInfo
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- CN116511719A CN116511719A CN202310606018.5A CN202310606018A CN116511719A CN 116511719 A CN116511719 A CN 116511719A CN 202310606018 A CN202310606018 A CN 202310606018A CN 116511719 A CN116511719 A CN 116511719A
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 183
- 238000010894 electron beam technology Methods 0.000 title claims abstract description 109
- 238000000034 method Methods 0.000 title claims abstract description 38
- 230000000737 periodic effect Effects 0.000 claims abstract description 81
- 239000000463 material Substances 0.000 claims abstract description 65
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 238000000576 coating method Methods 0.000 claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 16
- 239000010408 film Substances 0.000 claims description 48
- 230000004048 modification Effects 0.000 claims description 20
- 238000012986 modification Methods 0.000 claims description 20
- 239000012860 organic pigment Substances 0.000 claims description 17
- 230000005684 electric field Effects 0.000 claims description 13
- 230000004907 flux Effects 0.000 claims description 11
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000004132 cross linking Methods 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 230000001133 acceleration Effects 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 33
- 238000002360 preparation method Methods 0.000 abstract description 31
- 230000000694 effects Effects 0.000 abstract description 6
- 230000001678 irradiating effect Effects 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 238000003763 carbonization Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 238000001723 curing Methods 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000003550 marker Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- FWLHAQYOFMQTHQ-UHFFFAOYSA-N 2-N-[8-[[8-(4-aminoanilino)-10-phenylphenazin-10-ium-2-yl]amino]-10-phenylphenazin-10-ium-2-yl]-8-N,10-diphenylphenazin-10-ium-2,8-diamine hydroxy-oxido-dioxochromium Chemical compound O[Cr]([O-])(=O)=O.O[Cr]([O-])(=O)=O.O[Cr]([O-])(=O)=O.Nc1ccc(Nc2ccc3nc4ccc(Nc5ccc6nc7ccc(Nc8ccc9nc%10ccc(Nc%11ccccc%11)cc%10[n+](-c%10ccccc%10)c9c8)cc7[n+](-c7ccccc7)c6c5)cc4[n+](-c4ccccc4)c3c2)cc1 FWLHAQYOFMQTHQ-UHFFFAOYSA-N 0.000 description 1
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- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000001227 electron beam curing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Classifications
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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
- B23K26/346—Working by laser beam, e.g. welding, cutting or boring in combination with welding or cutting covered by groups B23K5/00 - B23K25/00, e.g. in combination with resistance welding
-
- 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
- B23K26/08—Devices involving relative movement between laser beam and workpiece
- B23K26/082—Scanning systems, i.e. devices involving movement of the laser beam relative to the laser head
-
- 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
-
- 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
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- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Plasma & Fusion (AREA)
- Mechanical Engineering (AREA)
- Laser Beam Processing (AREA)
Abstract
The invention discloses a method and a system for preparing a micro-nano structure by laser-electron beams and the micro-nano structure. Coating matching materials on the surface of a substrate to form a film; focusing the laser generated by the laser on the surface of the film, and controlling the scanning direction of the laser on the surface of the film through a moving scanning platform; adjusting processing parameters of a laser, and enabling a light field to reach a unit area power density processing window for generating a periodic micro-nano structure on the surface of a film to form an erasable periodic micro-nano structure; focusing the electron beam on the erasable periodic micro-nano structure, adjusting the processing parameters of the electron beam, and enabling the electron beam to reach a processing window for modifying the erasable periodic micro-nano structure so as to form the permanent micro-nano structure. The invention combines the laser surface micro-nano preparation technology and the electron beam exposure technology, fully plays the high efficiency of laser irradiation and the high precision of electron beam irradiation, and realizes the effect of preparing the high-precision micro-nano structure in a large area.
Description
Technical Field
The invention relates to the technical field of micro-nano structure preparation, in particular to a method and a system for preparing a micro-nano structure by laser-electron beams and the micro-nano structure.
Background
The surface micro-nano structured processing may improve or impart some novel properties to the material surface, such as wettability, optical properties, frictional wear properties, catalytic properties, antimicrobial properties, etc. Various micro-nano processing technologies are developed, wherein the laser surface micro-nano preparation technology utilizes focused laser beams to directly write or directly induce micro-nano structures on the surface of a material; the electron beam exposure technology utilizes a focused electron beam with extremely short wavelength to directly act on the surface of an electron-sensitive material to prepare the micro-nano structure consistent with a scanning path.
Common laser surface micro-nano preparation technology comprises the following steps: laser direct writing technology, laser-induced periodic surface structure technology, and laser interference direct writing technology.
The laser surface micro-nano preparation technology has the advantages of wide applicable materials, flexibility, high efficiency, environmental friendliness and the like. The electron beam exposure technology has the advantages of ultrahigh resolution (limit size can reach less than 10 nm) and flexible preparation, and is a powerful way for preparing high-precision nano structures and devices.
However, the precision of the laser direct writing technique is generally limited by diffraction limit, the laser-induced periodic surface structure technique is not suitable for all materials, and the optical device required by the laser interference direct writing technique is complex and high in cost. The electron beam exposure technology has low exposure efficiency and complex control, is only suitable for materials sensitive to electrons, and is difficult to be applied to mass production.
Disclosure of Invention
The invention provides a method, a system and a micro-nano structure for preparing a micro-nano structure by laser-electron beams, which are used for solving the technical problems that the precision of a micro-nano preparation technology on a laser surface is limited by diffraction limit, the application range is limited, an optical device is complex, the cost is high, the exposure efficiency of an electron beam exposure technology is low, the control is complex, the method and the system are only suitable for materials sensitive to electrons and are difficult to apply to mass production, and realizing the common promotion of the whole high efficiency and the local high precision, the preparation efficiency and the preparation precision of the micro-nano structure.
In order to solve the above technical problems, in a first aspect, an embodiment of the present invention provides a method for preparing a micro-nano structure by using a laser-electron beam, where the method includes:
coating matching materials on the surface of a substrate to form a film;
placing the substrate coated with the matching material on a motion scanning platform, focusing laser generated by a laser on the surface of the film, and controlling the scanning direction of the laser on the surface of the film through the motion scanning platform;
adjusting the processing parameters of the laser, and enabling the light field to reach a processing window of unit area power density for generating a periodic micro-nano structure on the surface of the film so as to form an erasable periodic micro-nano structure;
focusing an electron beam on the erasable periodic micro-nano structure, adjusting processing parameters of the electron beam, and enabling the electron beam to reach a processing window for modifying the erasable periodic micro-nano structure so as to form a permanent micro-nano structure;
and ultrasonically cleaning the permanent micro-nano structure, and ultrasonically cleaning the permanent micro-nano structure to remove the remained matching material and the erasable periodic micro-nano structure.
In a further embodiment, the matching material is an organic pigment having partially transmissive, partially absorbing laser properties.
In a further embodiment, the processing parameters of the laser include pulse width in the range of 10ns-50ns, effective pulse number in the range of 20-20000, laser fluence and repetition rate in the range of 0.381J/cm 2 -1.651J/cm 2 The repetition frequency ranges from 1kHz to 40kHz.
In a further embodiment, the output pulse of the laser generates a periodic electric field and a temperature field at the surface of the film, the peak electric field strength of the periodic electric field and the peak temperature of the temperature field both being within a damage threshold range, the damage threshold range being determined by the damage threshold of the substrate and the matching material.
In a further embodiment, the electron beam processing parameters include an acceleration voltage in the range of 0.1-30kV and an irradiation time of 10s and above.
In a further embodiment, the organic pigment is partially carbonized by continuous laser irradiation to form erasable periodic micro-nano structures when the optical field reaches a power density processing window per unit area that produces periodic micro-nano structures at the surface of the thin film.
In a further embodiment, the adjusting the processing parameters of the electron beam to achieve the electron beam to a processing window that modifies the erasable periodic micro-nano structure to form a permanent micro-nano structure includes:
and adjusting the processing parameters of the electron beam, and enabling the energy of the electron beam to achieve chemical bond fracture and/or crosslinking reaction of the polymer in the organic pigment so as to modify and solidify the erasable periodic micro-nano structure into a permanent micro-nano structure.
In a second aspect, the micro-nano structure in the embodiment of the invention is prepared by the method of any claim of the invention.
In a further embodiment, the periodic micro-nano structure is a micro-nano grating with a period range of
950nm-1020nm。
In a third aspect, an embodiment of the present invention provides a system for preparing a micro-nanostructure by using a laser-electron beam, the system comprising:
the system comprises: a coating unit, a laser processing unit, an electron beam modification unit and an ultrasonic cleaning unit, wherein,
the coating unit is used for coating matching materials on the surface of the substrate to form a film;
the laser processing unit comprises a laser, a focusing lens and a motion scanning platform;
the laser is used for generating laser and focusing on the surface of the film; adjusting the processing parameters of the laser, and enabling the light field to reach a unit area power density processing window for generating a periodic micro-nano structure on the surface of the film so as to form a first periodic micro-nano structure; the focusing lens is used for focusing laser generated by the laser on the surface of the film; the motion scanning platform is used for bearing a substrate coated with a matching material so as to control the scanning direction of laser on the surface of the film;
the electron beam modification unit is used for focusing an electron beam on the erasable periodic micro-nano structure, adjusting processing parameters of the electron beam, and enabling the electron beam to reach a processing window for modifying the erasable periodic micro-nano structure so as to form a permanent micro-nano structure;
the ultrasonic cleaning unit is used for carrying out ultrasonic cleaning on the permanent micro-nano structure to remove the remained matching material and the erasable periodic micro-nano structure.
The embodiment of the invention provides a method and a system for preparing a micro-nano structure by laser-electron beams and the micro-nano structure. Firstly, irradiating a film formed by a matching material coated on a base material by using a laser beam, performing preliminary carbonization modification on the film to form an erasable periodic micro-nano structure, and irradiating the erasable periodic micro-nano structure by using an electron beam so as to enable a polymer in the organic pigment to generate chemical bond fracture and/or crosslinking reaction, so that the erasable periodic micro-nano structure is modified and solidified into a permanent micro-nano structure. According to the invention, the laser surface micro-nano preparation technology and the electron beam exposure technology are combined, and after the erasable periodic micro-nano structure is generated by laser irradiation, the finer micro-nano structure is prepared by using the electron beam, so that the high efficiency of the laser irradiation and the refinement of the electron beam irradiation are fully exerted, and the effect of preparing the high-precision micro-nano structure in a large area is realized.
Drawings
FIG. 1 is a schematic diagram of steps of a method for preparing a micro-nano structure by using a laser-electron beam according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of a method for preparing a micro-nano structure by using a laser-electron beam according to an embodiment of the present invention;
FIG. 3 is a comparative diagram of a permanent micro-nano structure obtained by curing an erasable micro-nano structure using a laser and an electron beam according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of a system for preparing micro-nano structures by using a laser-electron beam according to an embodiment of the present invention;
fig. 5 is a diagram of a scanning electron microscope for preparing a micro-nano structure on a gold surface by using the method for preparing a micro-nano structure by using a laser-electron beam provided by the embodiment of the invention.
Detailed Description
The following examples are given for illustrative purposes only and are not to be construed as limiting the invention, as embodiments of the invention are specifically illustrated by the accompanying drawings, which are included by reference and description only, and do not limit the scope of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1, in an embodiment of the present invention, a method for preparing a micro-nanostructure by using a laser-electron beam includes the following steps S1-S5:
s1, coating a matching material on the surface of the substrate to form a film.
S2, placing the substrate coated with the matching material on a motion scanning platform, focusing laser generated by a laser on the surface of the film, and controlling the scanning direction of the laser on the surface of the film through the motion scanning platform.
And S3, adjusting the processing parameters of the laser, and enabling the light field to reach a unit area power density processing window for generating the periodic micro-nano structure on the surface of the film so as to form the erasable periodic micro-nano structure.
S4, focusing the electron beam on the erasable periodic micro-nano structure, adjusting the processing parameters of the electron beam, and enabling the electron beam to reach a processing window for modifying the erasable periodic micro-nano structure so as to form a permanent micro-nano structure.
S5, carrying out ultrasonic cleaning on the permanent micro-nano structure, and removing the left matching material and the erasable periodic micro-nano structure.
Referring to fig. 1 and 2, in an embodiment of the present invention, in order to solve the contradiction between the existing preparation efficiency and preparation accuracy of the laser surface micro-nano preparation technology and the electron beam exposure technology, the laser surface micro-nano preparation technology and the electron beam exposure technology are combined. The laser beam acts on the film formed by the matching material coated on the surface of the base layer to enable the matching material to be partially carbonized and modified, and the periodic micro-nano structure formed at the moment is an erasable micro-nano structure and can be erased by a specific solvent. In order to improve the precision of micro-nano structure preparation, the electron beam is adopted to irradiate the erasable periodic micro-nano structure, so that the micro-nano structure which is finer than the micro-nano structure prepared by adopting a laser surface micro-nano preparation technology can be prepared in a shorter time.
In an embodiment of the invention, the matching material is an organic pigment having partially transmissive, partially absorbing laser properties. The laser is partially transmitted on the interface of the substrate and the film, the generated plasmons and interference effects determine the periodic electric field distribution, and then a periodic temperature field is generated, the electric field intensity peak value of the periodic electric field and the temperature peak value of the temperature field are both in the damage threshold range, the damage threshold range is determined by the damage threshold of the substrate and the matching material, and the irradiation of the film can be realized under the condition of not damaging the surface of the substrate. The matching material absorbs part of laser energy, and heats, melts, vaporizes and modifies under the condition that the electric field intensity peak value or the temperature peak value of the periodic electric field and the temperature field exceeds the damage threshold value of the matching material, so that the periodic micro-nano structure is etched on the film, and at the moment, the matching material is partially carbonized under the action of laser, but the solubility of the matching material is not changed, and the formed micro-nano structure can be erased through a special solvent. In the embodiment of the invention, aniline black is taken as an example for illustration and picture display.
The matching material is coated on the surface of the substrate to form a film, and the film formed by the matching material on the substrate is used as a material layer for preparing the micro-nano structure by laser, so that the micro-nano structure can be prepared without damaging the substrate. The type of the substrate is not limited, and can be metal, semiconductor or dielectric, but the damage threshold of the matching material is smaller than that of the substrate, so that the substrate is not damaged when the film formed by the matching material is subjected to laser irradiation modification.
In particular, the method comprises the steps of,the substrate coated with the matching material is placed on a motion scanning stage that is used to control the scanning direction of the laser on the film surface. Firstly, adjusting the processing parameters of a laser, wherein the processing parameters of the laser comprise pulse width, effective pulse number, laser flux and repetition frequency, the pulse width ranges from 10ns to 50ns, the effective pulse number ranges from 20 to 20000, and the laser flux range is 0.381J/cm 2 -1.651J/cm 2 The repetition frequency ranges from 1kHz to 40kHz. Only when the laser flux range of the laser reaches a specified value, the film formed by the organic pigment can be partially carbonized under the action of an electric field and an energy field generated by laser through continuous laser irradiation, so that the erasable periodic micro-nano structure is formed.
For different base materials and matching materials, according to the damage threshold values of the base materials and the matching materials, the absorption peaks of the spectra of the matching materials determine the processing parameters such as the pulse width, the effective pulse number, the laser flux, the repetition frequency and the like of laser so as to determine the laser processing parameters of each base material and matching material combination, and the laser processing parameters are used as parameter data for mass production of the micro-nano structure disclosed by the embodiment of the invention so as to improve the quality and the efficiency of preparing the micro-nano structure by laser.
After the preparation of the erasable periodic micro-nano structure is completed, in order to improve the precision of the preparation of the micro-nano structure, the electron beam is adopted to carry out curing modification on the erasable periodic micro-nano structure, and the processing parameters of the electron beam are adjusted. And adjusting processing parameters of the electron beam, and enabling energy of the electron beam to achieve chemical bond fracture and/or crosslinking reaction of the polymer in the organic pigment, wherein the polymer in the organic pigment mainly takes the crosslinking reaction at the moment so as to modify and solidify the erasable periodic micro-nano structure into a permanent micro-nano structure.
If the erasable micro-nano structure is solidified by a laser, the period of the formed micro-nano structure is close to the wavelength level, and is limited by the wavelength (about 1 μm) of the laser, the edge of the micro-nano structure area is generally rough, and finer micro-nano structures cannot be prepared. Because the beam diameter of the focused electron beam is far smaller than the laser beam spot, the method has ultrahigh resolution (limit size can reach less than 10 nm) and preparation flexibility, can generate finer micro-nano structure, and has sharper edges. As shown in fig. 3, the permanent micro-nano structure contrast diagram obtained by curing the erasable micro-nano structure by using a laser and an electron beam has the minimum spot size, rough edge and uncontrollable fineness in the area cured by using a laser beam; the area cured by the electron beam is smaller, the edges of the cured rectangle are sharper and clearer, and the micro-nano structure is finer. This is an unattainable effect of curing erasable periodic micro-nano structures using laser modification.
In the embodiment of the invention, the matching material is an organic pigment, which is difficult to be directly subjected to partial carbonization modification by the focused electron beam of the electron microscope, and even if the energy of the electron beam is increased, the carbonization modification of the organic pigment also needs long electron beam irradiation time, so that the production efficiency is low. In the embodiment of the invention, the organic pigment selected by the invention is subjected to preliminary carbonization modification treatment by adopting laser beam irradiation so as to form an erasable periodic micro-nano structure, and then the erasable periodic micro-nano structure can be subjected to curing modification by adopting short-time irradiation of electron beams.
The micro-nano structure prepared by the method for preparing the micro-nano structure by the laser-electron beam provided by the embodiment of the invention is a micro-nano grating, and the period range of the micro-nano grating is 950-1020nm.
In the embodiment of the invention, in order to solve the technical problems that the precision of the laser surface micro-nano preparation technology is limited by diffraction limit, the application range is limited, an optical device is complex, the cost is high, the electron beam exposure technology has low exposure efficiency and complex control, and the method is only suitable for electron sensitive materials and is difficult to be applied to mass production, and the method for preparing the micro-nano structure by the laser-electron beam is provided. Firstly, irradiating a film formed by a matching material coated on a base material by using a laser beam, performing preliminary carbonization modification on the film to form an erasable periodic micro-nano structure, and irradiating the erasable periodic micro-nano structure by using an electron beam so as to enable a polymer in the organic pigment to generate chemical bond fracture and/or crosslinking reaction, so that the erasable periodic micro-nano structure is modified and solidified into a permanent micro-nano structure. According to the invention, the laser surface micro-nano preparation technology and the electron beam exposure technology are combined, and after the erasable periodic micro-nano structure is generated by laser irradiation, the finer micro-nano structure is prepared by using the electron beam, so that the high efficiency of laser irradiation and the high precision of electron beam irradiation are fully exerted, and the effect of preparing the high-precision micro-nano structure in a large area is realized.
Example two
Accordingly, as shown in fig. 4, based on a method for preparing a micro-nano structure by using a laser-electron beam, the embodiment of the invention further provides a system for preparing a micro-nano structure by using a laser-electron beam, which comprises: a coating unit 1, a laser processing unit 2, an electron beam modification unit 3 and an ultrasonic cleaning unit 4, wherein,
the coating unit 1 is used for coating matching materials on the surface of a substrate to form a film;
the laser processing unit 2 comprises a laser 201, a focusing lens 202 and a motion scanning platform 203;
the laser 201 is used for generating laser and focusing on the surface of the film; adjusting the processing parameters of the laser, and enabling the light field to reach a unit area power density processing window for generating a periodic micro-nano structure on the surface of the film so as to form an erasable periodic micro-nano structure; the focusing lens 202 is used for focusing the laser generated by the laser on the surface of the film; the motion scanning platform 203 is used for bearing the substrate coated with the matching material so as to control the scanning direction of the laser on the surface of the film;
the electron beam modification unit 3 is configured to focus an electron beam on the erasable periodic micro-nano structure, adjust a processing parameter of the electron beam, and reach the electron beam to a processing window of the modified erasable periodic micro-nano structure to form a permanent micro-nano structure;
the ultrasonic cleaning unit 4 is used for performing ultrasonic cleaning on the permanent micro-nano structure to remove the remained matching material and the erasable periodic micro-nano structure.
As a preferable scheme of the embodiment, the laser 201 selects a YAG infrared nanosecond laser with a wavelength of 1064nm, a pulse width of 10ns-50ns, a repetition frequency of 1kHz-10kHz and a laser flux of 0.381J/cm 2 -1.651J/cm 2 (II), (III), (V), (; the focal length of the focusing lens 202 is 15cm, and the diameter of the focused light spot is 100 μm; the period of the prepared micro-nano structured grating is about 1 mu m, and is particularly 950-1020nm. The motion scanning platform 203 is a stepping motor, the moving speed range of the stepping motor is 0.1mm/s-0.6mm/s, the filling interval range is 0.1mm-0.2mm, and the stepping motor can be replaced by a galvanometer system to prepare a large-area micro-nano structure. The electron beam modification unit 3 is an electron beam generated by a Schottky field emission filament in a scanning electron microscope, the accelerating voltage range is 0.1-30kV, and the beam current range is 0-100nA, and is continuously adjustable.
The laser beam is expanded by a beam expander to improve the quality of the beam, and after the expanded laser beam passes through a focusing lens 202 to be focused on the surface of the film, the processing parameters of the laser 201 such as pulse width, effective pulse number, laser flux, repetition frequency and the like are adjusted so that the output laser flux range of the laser 201 reaches 0.381J/cm 2 -1.651J/cm 2 To produce an erasable micro-nano structure. Focusing the electron beam on the erasable periodic micro-nano structure, adjusting the accelerating voltage and the irradiation time of the electron beam, and enabling the energy of the electron beam modification unit 3 to achieve the chemical bond breaking and/or crosslinking reaction of the polymer in the organic pigment so as to modify and solidify the erasable periodic micro-nano structure into a permanent micro-nano structure.
For specific limitations regarding a system for preparing micro-nano structures by using a laser-electron beam, reference may be made to the above-mentioned limitations on the method for preparing micro-nano structures by using a laser-electron beam, and details thereof will not be repeated herein. Those of ordinary skill in the art will appreciate that the various modules and steps described in connection with the disclosed embodiments of the invention may be implemented in hardware, software, or a combination of both. Whether such functionality is implemented as hardware or software depends upon the particular application and design constraints imposed on the solution. Skilled artisans may implement the described functionality in varying ways for each particular application, but such implementation decisions should not be interpreted as causing a departure from the scope of the present invention.
Example III
According to the method and the system for preparing the micro-nano structure on the surface of the matching layer by the laser-electron beam, disclosed by the embodiment of the invention, the laser-electron beam composite processing of the grating micro-nano structure is realized on the surface of the metal gold as the base material.
The coating method is a manual coating method, the coating tool is a marker pen, the base material is metal gold, and the matching material is marker pen ink with the main component comprising nigrosine. YAG infrared nanosecond laser with wavelength of 1064nm, pulse width of 50ns, repetition frequency of 1kHz, linearly polarized light, focal length of focusing lens 202 of 15cm, diameter of focusing spot of 100 μm, laser flux of 1.4J/cm, and laser processing parameters 2 The number of effective pulses is selected to be 250. In the electron beam processing parameters, the accelerating voltage is selected to be 5kV, and the irradiation time is selected to be 120s. The specific solvent is absolute ethanol.
Coating the alcoholic marker ink containing nigrosine on the surface of a gold substrate to prepare a film, placing the coated sample on a motion scanning platform 203, adjusting the pulse width, the effective pulse number, the laser flux and the repetition frequency of a laser 201, expanding the laser emitted by the laser 201 by using a beam expander, focusing the laser after the beam expansion on the surface film of the gold substrate which is coated, and continuously irradiating to generate an erasable periodic micro-nano structure, wherein a plasmon (approximate sinusoidal electric field distribution) of a laser-induced metal interface is carved on the ink to form a grating structure, and the matching material is not completely carbonized and modified and can be still dissolved in absolute ethyl alcohol, as shown by a light-colored area in a central circular spot of an upper left graph of fig. 5. And then adjusting the accelerating voltage and the irradiation time of the electron beam, irradiating a white dotted line rectangular area in the center, modifying the erasable micro-nano structure into a permanent micro-nano structure, and generating chemical bond fracture or cross-linking reaction on a polymer in the matched material to become the permanent micro-nano structure insoluble in absolute ethyl alcohol. As shown in the upper right diagram of fig. 5, only the permanent micro-nano structure in the rectangular area irradiated by the electron beam is left after the ultrasonic cleaning by absolute ethyl alcohol, and the erasable micro-nano structure and the matching layer material which is not irradiated by the laser are all removed. As shown in the lower left diagram of fig. 5, the erasable micro-nano structure is generated in the irradiation range of the laser spot, but the edge is rough, and the irregular state is presented. As shown in the lower right graph of FIG. 5, the edge of the rectangular area modified by the electron beam is sharp, the fineness is high, the substrate is not damaged by the influence of laser and electron beam irradiation, and the period of the grating micro-nano structure prepared by the embodiment is about 1 μm and is between 9500nm and 1020nm.
In the embodiment of the invention, the Mark pen is directly used for coating the matching layer on the surface of the noble metal, the film is convenient to prepare, the comprehensive cost is low, and the micro-nano structure produced by the method and the system for preparing the micro-nano structure on the surface of the matching layer by using the laser-electron beam provided by the invention has the grating characteristic. The method can be applied to the preparation of composite micro-nano structures, and can be used for preparing large-area erasable periodic micro-nano structures by utilizing laser, preparing high-precision permanent micro-nano structures by utilizing electron beam curing modified erasable periodic micro-nano structures, and preparing multi-scale composite micro-nano structures.
In summary, the preparation technology of the micro-nano structure combines the laser and electron beam, and compared with the preparation technology of the micro-nano structure prepared by single laser or electron beam, the preparation technology of the composite micro-nano structure has the advantages of large-area preparation and high precision, and the preparation technology of the composite micro-nano structure is flexible.
The embodiment provides a method, a system and a micro-nano structure for preparing a micro-nano structure by laser-electron beams, which aim at the technical problem that the preparation efficiency and the preparation precision of the existing laser surface micro-nano preparation technology or electron beam exposure technology are contradictory. Firstly, irradiating a film formed by a matching material coated on a base material by using a laser beam, performing preliminary carbonization modification on the film to form an erasable periodic micro-nano structure, and irradiating the erasable periodic micro-nano structure by using an electron beam so as to enable a polymer in the organic pigment to generate chemical bond fracture and/or crosslinking reaction, so that the erasable periodic micro-nano structure is modified and solidified into a permanent micro-nano structure. According to the invention, the laser surface micro-nano preparation technology and the electron beam exposure technology are combined, and after the erasable periodic micro-nano structure is generated by laser irradiation, the finer micro-nano structure is prepared by using the electron beam, so that the high efficiency of laser irradiation and the high precision of electron beam irradiation are fully exerted, and the effect of preparing the high-precision micro-nano structure in a large area is realized.
The foregoing examples represent only a few preferred embodiments of the present invention, which are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that modifications and substitutions can be made by those skilled in the art without departing from the technical principles of the present invention, and such modifications and substitutions should also be considered to be within the scope of the present invention. Therefore, the protection scope of the patent of the invention is subject to the protection scope of the claims.
Claims (10)
1. A method of preparing a micro-nanostructure with a laser-electron beam, the method comprising:
coating matching materials on the surface of a substrate to form a film;
placing the substrate coated with the matching material on a motion scanning platform, focusing laser generated by a laser on the surface of the film, and controlling the scanning direction of the laser on the surface of the film through the motion scanning platform;
adjusting the processing parameters of the laser, and enabling the light field to reach a processing window of unit area power density for generating a periodic micro-nano structure on the surface of the film so as to form an erasable periodic micro-nano structure;
focusing an electron beam on the erasable periodic micro-nano structure, adjusting processing parameters of the electron beam, and enabling the electron beam to reach a processing window for modifying the erasable periodic micro-nano structure so as to form a permanent micro-nano structure;
and ultrasonically cleaning the permanent micro-nano structure, and removing the residual matching material and the erasable periodic micro-nano structure.
2. The method of preparing micro-nano structure according to claim 1, wherein the matching material is an organic pigment having characteristics of partial transmission and partial absorption of laser light.
3. The method of preparing micro-nano structure according to claim 2, wherein the processing parameters of the laser include pulse width, effective pulse number, laser flux and repetition rate, the pulse width is in the range of 10ns-50ns, the effective pulse number is in the range of 20-20000, and the laser flux is in the range of 0.381J/cm 2 -1.651J/cm 2 The repetition frequency ranges from 1kHz to 40kHz.
4. The method of claim 3, wherein the output pulse of the laser produces a periodic electric field and a temperature field at the surface of the thin film, the peak electric field strength of the periodic electric field and the peak temperature of the temperature field both being within a damage threshold range, the damage threshold range being determined by the damage threshold of the substrate and the matching material.
5. The method of preparing micro-nano structure according to claim 2, wherein the electron beam processing parameters include an acceleration voltage and an irradiation time, the acceleration voltage is in the range of 0.1-30kV, and the irradiation time is 10s and above.
6. The method for preparing micro-nano structure according to claim 2, wherein the method comprises the steps of,
and when the light field reaches a unit area power density processing window for generating the periodic micro-nano structure on the surface of the film, the organic pigment is partially carbonized through continuous laser irradiation to form the erasable periodic micro-nano structure.
7. The method of claim 2, wherein adjusting the processing parameters of the electron beam to achieve the processing window of the modified erasable periodic micro-nanostructure comprises:
and adjusting the processing parameters of the electron beam, and enabling the energy of the electron beam to achieve chemical bond fracture and/or crosslinking reaction of the polymer in the organic pigment so as to modify and solidify the erasable periodic micro-nano structure into a permanent micro-nano structure.
8. A micro-nano structure, characterized in that it is prepared by the method according to any one of claims 1 to 7.
9. The micro-nano structure of claim 8, wherein the periodic micro-nano structure is a micro-nano grating with a period ranging from 950nm to 1020nm.
10. A system for laser-electron beam fabrication of micro-nano structures, the system comprising: a coating unit, a laser processing unit, an electron beam modification unit and an ultrasonic cleaning unit, wherein,
the coating unit is used for coating matching materials on the surface of the substrate to form a film;
the laser processing unit comprises a laser, a focusing lens and a motion scanning platform;
the laser is used for generating laser and focusing on the surface of the film; adjusting the processing parameters of the laser, and enabling the light field to reach a unit area power density processing window for generating a periodic micro-nano structure on the surface of the film so as to form an erasable periodic micro-nano structure; the focusing lens is used for focusing laser generated by the laser on the surface of the film; the motion scanning platform is used for bearing a substrate coated with a matching material so as to control the scanning direction of laser on the surface of the film;
the electron beam modification unit is used for focusing an electron beam on the erasable periodic micro-nano structure, adjusting processing parameters of the electron beam, and enabling the electron beam to reach a processing window for modifying the erasable periodic micro-nano structure so as to form a permanent micro-nano structure;
the ultrasonic cleaning unit is used for carrying out ultrasonic cleaning on the permanent micro-nano structure to remove the remained matching material and the erasable periodic micro-nano structure.
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