CN113805433A - Manufacturing method of three-dimensional nano through hole - Google Patents
Manufacturing method of three-dimensional nano through hole Download PDFInfo
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- CN113805433A CN113805433A CN202111112640.8A CN202111112640A CN113805433A CN 113805433 A CN113805433 A CN 113805433A CN 202111112640 A CN202111112640 A CN 202111112640A CN 113805433 A CN113805433 A CN 113805433A
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/0035—Multiple processes, e.g. applying a further resist layer on an already in a previously step, processed pattern or textured surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/20—Exposure; Apparatus therefor
- G03F7/2022—Multi-step exposure, e.g. hybrid; backside exposure; blanket exposure, e.g. for image reversal; edge exposure, e.g. for edge bead removal; corrective exposure
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/70—Microphotolithographic exposure; Apparatus therefor
- G03F7/70383—Direct write, i.e. pattern is written directly without the use of a mask by one or multiple beams
- G03F7/70391—Addressable array sources specially adapted to produce patterns, e.g. addressable LED arrays
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Abstract
The invention discloses a method for manufacturing a three-dimensional nano through hole, which belongs to the technical field of photoetching, can directly manufacture the three-dimensional nano through hole with the diameter less than 100nm by combining laser direct writing with adjustable space structure light, and realizes the method for manufacturing the three-dimensional nano through hole with the controllable nano hole diameter. The manufacturing method has the advantages of simple process, low cost and short manufacturing period, can realize the controllable manufacturing of the nano through hole, and can provide an effective solution for the research in the fields of micro-nano fluidic, biomedicine, bionic functional materials and the like.
Description
Technical Field
The invention relates to the field of photoetching technology application, in particular to a method for manufacturing a three-dimensional nano through hole.
Background
The artificial nanometer through hole is a functional structure and has wide application in the fields of micro-nano fluidic, biomedicine, bionic functional materials and the like. Artificial nanopores are mainly classified into biological nanopores (regenerable ion channels, porin channels, etc.) and solid-state nanopores. The natural nano-channel has a fine structure and high sensitivity, but is too sensitive to external environment (pH value, temperature, salt concentration and the like) stimulation, so that the stability is poor and the service life is short; the solid-state nanopore overcomes the defect of poor stability of biological nanochannels, and provides a good research platform for designing and developing artificial bionic nanochannels and simulating life processes in vitro.
At present, the traditional nanopore manufacturing methods mainly include focused ion beam etching (FIB), electron beam Etching (EB), heavy particle bombardment, and nanoimprint. For example, in 2001 Li et al used a focused Ar ion beam to create 1.8nm nanopores in SiNx films; dekker et al 2003 used electron beams to produce SiO 2nm in diameter2A nanopore; in 2012, Eugenia et al processed a nanopore channel with a diameter less than 10nm by using a heavy ion bombardment technology; in 2019, Choi et al manufactured nanopores with pore diameters less than 200nm by using a nanoimprint process.
However, both FIB and EB technologies rely on expensive large-scale instruments, and the nanopore is expensive to manufacture, and slow in manufacturing speed (e.g., the EB technology takes more than 12 hours to process one nanopore); the heavy particle bombardment technology also depends on a large instrument, and heavy ion tracks are randomly distributed in a sample, so that the position and channel parameters of the nano channel are difficult to actively adjust; the difficulty in fabricating nanopores using nanoimprint techniques is that the template fabrication is expensive and time consuming, and the nanoimprint may cause contamination of the material substrate.
Therefore, how to provide a method for manufacturing a diameter-controllable nano-via by using space-structured light and laser direct writing is a problem to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the present invention provides a method for manufacturing a three-dimensional nano through hole, which is capable of directly manufacturing a three-dimensional nano through hole with a diameter smaller than 100nm by using a laser direct writing technology in combination with an adjustable spatial structured light, and manufacturing a three-dimensional nano through hole with a controllable nano hole diameter based on a spatial structured light and a laser direct writing technology. The manufacturing method has the advantages of simple process, low cost and short manufacturing period, can realize the controllable manufacturing of the nano through hole, and provides an effective solution for the research in the fields of micro-nano fluidic, biomedicine, bionic functional materials and the like.
In order to achieve the above purpose, the invention provides the following technical scheme:
a manufacturing method of a three-dimensional nano through hole is based on a laser direct writing system and is characterized by comprising the following steps:
preparing a substrate: preparing a substrate with micropores and coating a negative photoresist film on one surface of the substrate;
carrying out laser direct writing: carrying out multiple exposures at the position of the micron hole of the substrate;
and (3) carrying out photoresist development: and developing the negative photoresist to obtain the three-dimensional nano through hole.
Preferably, the performing the laser direct writing process includes:
modulating light field parameters in the laser direct writing system to obtain annular space structured light;
and calibrating the laser focus to the center of the micropore, so that the laser focus is positioned in the negative photoresist film for multiple exposure.
Preferably, the specific process after obtaining the annular space structured light includes:
and adjusting the outer diameter of the annular space structure light to be larger than the diameter of the micron hole on the substrate, and then gradually reducing the topological number of the space structure light until the optical size of the annular space structure light is controlled to be 1, and carrying out exposure once when each pair corresponds to a different topological number.
Preferably, the process for manufacturing the three-dimensional nano-via further comprises: and controlling the diameter of the three-dimensional nano through hole by controlling the exposure dose of the annular space structure light.
Preferably, the light intensity of the central region of the annular space structured light is zero.
Preferably, the specific process of calibrating the laser focus to the center of the micro-hole to make the laser focus located in the negative photoresist film for multiple exposures comprises: the exposure dose of the structured light in the peripheral annular space is higher than that of the structured light in the inner annular space.
Preferably, the performing the development includes: developing the negative photoresist by the developing solution, removing the photoresist corresponding to the zero light intensity area, and generating the nano through hole.
According to the technical scheme, compared with the prior art, the invention discloses the manufacturing method of the three-dimensional nano through hole, the three-dimensional nano through hole with the diameter less than 100nm can be directly manufactured by combining laser direct writing with adjustable space structure light, and the manufacturing method of the three-dimensional nano through hole with the controllable nano hole diameter is realized. The manufacturing method has the advantages of simple process, low cost and short manufacturing period, can realize the controllable manufacturing of the nano through holes, can realize the three-dimensional nano through holes with the depth of submicron to several microns, and provides an effective solution for the research in the fields of micro-nano fluidic, biomedicine, bionic functional materials and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic view of the preparation process provided in example 1;
fig. 2 is a Scanning Electron Microscope (SEM) image of the micropores provided in example 2.
FIG. 3(a) is a Scanning Electron Microscope (SEM) image of the hollow structure provided in this example 2;
fig. 3(b) is a Scanning Electron Microscope (SEM) image of the nanopore with the topology number of 1 provided in example 2.
In fig. 1: a 1-micron pore substrate; 2-micron pores; 3-a negative photoresist film; 4-annular space structured light; 5-photoresist developing structure; 6-three-dimensional nano-through holes.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to the attached drawing 1, the embodiment of the invention discloses a method for manufacturing a three-dimensional nano through hole, and the technical scheme is as follows:
first, prepare the substrate
Firstly, preparing a micron-pore substrate 1 with the diameter less than 5 mu m;
coating negative photoresist on one surface of the prepared substrate, and carrying out relevant treatment before photoresist exposure.
Secondly, preparing the diameter-controllable three-dimensional nano through hole 6 based on the combination of the two-photon direct writing technology and the annular structured light
Modulating laser parameters in the direct writing system to obtain annular space structured light 4;
fourthly, calibrating the laser focus to the center of the micropore 2, wherein the laser focus is positioned in the negative photoresist film 3;
firstly, loading a vortex phase diagram with large topological number on a spatial light modulator, generating a hollow light spot with the outer diameter larger than the outer diameter of the micropore 2, and carrying out first exposure on the photoresist to manufacture a hollow structure with the outer diameter larger than the micropore 2 of the substrate; then, the sample is kept still in the original position, the size of the space structure light is modulated, the peripheral size of the laser spot is smaller than that of the space structure light used for the first time, and meanwhile, the peripheral size of the laser spot is larger than that of a hollow structure of the space structure light used for the first time, and the second exposure is carried out; and then, by analogy, gradually reducing the size of the annular light, and continuously exposing the photoresist until the size of the annular light hollow structure reaches the minimum size, namely finishing the last exposure.
In a specific embodiment, the light intensity of the central area of the annular space structure light is zero, and the size of the zero-light-intensity area of the central area of the annular space structure light can be adjusted through spatial light modulation.
In a specific embodiment, the center position of the annular light spot is positioned in the through hole of the substrate micron in the laser direct writing process, and the annular laser focal spot is positioned in the photoresist layer.
In one embodiment, during the laser exposure, the light exposure dose of the outer spatial structure is higher than the light exposure dose of the inner spatial structure.
In a specific embodiment, the specific process after obtaining the annular space structure light further includes: the diameter of the three-dimensional nanometer through hole is controlled by controlling the exposure dose of the annular space structure light.
In one embodiment, the specific process after obtaining the annular space structure light comprises:
and adjusting the outer diameter of the light of the annular space structure to be larger than the diameter of the micron hole on the substrate, and carrying out multiple exposures until the size of the light of the annular space structure is controlled to be 1 in topological number, thus finishing the exposure.
Third, post-processing of the substrate
Sixthly, developing and processing the manufactured substrate to obtain a photoresist developing structure 5, and finally obtaining the three-dimensional nano through hole 6.
Compared with the prior art, the invention has the beneficial technical effects that:
the three-dimensional nano through hole 6 is directly prepared by utilizing a laser direct writing mode, the process is simple, the operation is easy, an expensive large instrument is not needed, the manufacturing cost is low, the manufacturing period is short, the depth of the nano hole is from submicron to several microns, and a solution is provided for the research in the fields of micro-nano fluidic, biomedicine, bionic functional materials and the like.
Example 2
The detailed process of the method provided in specific application example 1 is as follows:
first, prepare the substrate
Preparing a micron pore substrate 1 with the diameter less than 5 mu m:
first, a substrate (18mm × 18mm × 0.17mm, borosilicate glass cover glass) was immersed in an acetone solution for 30 minutes; then, taking out the substrate, and putting the substrate in absolute ethyl alcohol for ultrasonic cleaning for 30 minutes; and then, taking out the substrate, placing the substrate in deionized water, carrying out ultrasonic cleaning for 30 minutes, and finally taking out the substrate, placing the substrate on tin foil paper, and naturally airing the substrate.
The substrate was directly processed using a femtosecond laser with a center wavelength of 800nm, a repetition frequency of 1 kHz, and a pulse width of 35fs, with a single pulse energy of 2.1 muJ at the entrance pupil. The NA of the focusing objective lens is 0.7, and when the exposure times are 200 times and the single-point exposure time is 50ms, a micron through hole is processed.
Referring to FIG. 2, a Scanning Electron Microscope (SEM) image of the micropores provided in this example 2 shows that the micropores 2 have an oval shape, a major axis of the oval is 4.31 μm, a minor axis is about 3.45 μm, and a depth is about 170 μm.
And (3) placing the processed substrate in deionized water for ultrasonic cleaning for 30 minutes, and finally taking out the substrate and placing the substrate on tin foil paper for natural drying.
Secondly, coating a negative photoresist on one surface of the prepared substrate, and performing related treatment before photoresist exposure:
mu.l of DETC (7-dimethylamino-3-trifluoromethylcopper) negative photoresist was sucked up by a pipette and dropped on the glass substrate in the area of the microwell 2.
Secondly, preparing the three-dimensional nano through hole 6 with controllable diameter based on the combination of the laser direct writing technology and the annular structured light
And thirdly, calibrating the focus of the laser direct writing system to the center of the micropore 2, wherein the laser focus is positioned in the negative photoresist film 3. When the laser is manufactured, firstly, a vortex phase diagram with large topological number is loaded on a spatial light modulator, hollow light spots with the outer diameter larger than a micron through hole are generated to expose the photoresist, and a hollow structure larger than a substrate micron hole 2 is prepared; then, the sample is kept in place, the topological number of the vortex phase diagram loaded on the spatial light modulator is reduced by 1 to reduce the size of a hollow light spot, the photoresist is continuously exposed, and the inner diameter of the structure is further reduced on the basis of the initially prepared hollow structure; and repeating the hollow light spot modulation method until the topological number of the vortex phase diagram is reduced to 1.
And fourthly, developing the manufactured substrate to obtain a photoresist developing structure 5, and finally obtaining the three-dimensional nano through hole 6 through cleaning and other treatments.
And (3) placing the exposed sample in a developing solution for developing for 30 minutes, washing off the photoresist of the unexposed parts of the hollow light spots, then washing by using deionized water to remove the developing solution attached to the substrate, and finally standing and naturally airing the structure to obtain the three-dimensional nano through hole 6.
In this example 2, the laser used was 775nm wavelength picosecond laser, the laser pulse width was 650ps, and the objective NA of the laser direct writing system was 1.4. The topological number of a vortex phase diagram loaded on the spatial light modulator at the initial moment is 9, the adopted laser power at the entrance pupil is 410mW, the exposure time is 10s, and the first exposure is carried out; then, sequentially reducing the topological number of the vortex phase diagram to 4, wherein the exposure time is 10s, and carrying out multiple exposure; then, the topological number is reduced to 3, the exposure power is reduced to 154mW, and the exposure time is 10 s; the laser power is 137mW when the topological number is 2, and the exposure time is 10 s; finally, the vortex phase map topology number was reduced to 1, the laser power was 113mW, and the exposure time was 30 s. When the topological number is 9, a hollow structure having an outer diameter of about 3.5 μm can be obtained. When the topological number is reduced step by step, the outer diameter of the obtained corresponding annular structure is always smaller than the outer diameter of the annular structure obtained by the last exposure and larger than the inner diameter of the annular structure obtained by the last exposure, and therefore the annular structure obtained by each exposure can be tightly combined with the annular optical structure obtained by the last exposure. Referring to fig. 3(a), a Scanning Electron Microscope (SEM) image of the hollow structure provided in example 2 shows that the number of the topology of the hollow structure in fig. 3(a) is 9, and the outer diameter is about 3.5 μm.
In the laser exposure process, the diameter of the final three-dimensional nano-via 6 can be controlled by controlling the exposure dose of the space structure light with the topological number equal to 1. When the laser power was 113mW and the exposure time was 30s, the diameter of the nanopore was 82 nm. Referring to FIG. 3(b), a Scanning Electron Microscope (SEM) image of nanopore with a topology number of 1 is provided for this example 2, wherein the nanopore diameter is 82 nm.
According to the technical scheme, compared with the prior art, the invention discloses the manufacturing method of the three-dimensional nano through hole, the three-dimensional nano through hole with the diameter less than 100nm can be directly manufactured by combining laser direct writing with adjustable space structure light, and the manufacturing method of the three-dimensional nano through hole with the controllable nano hole diameter is realized. The manufacturing method has the advantages of simple process, low cost and short manufacturing period, can realize the controllable manufacturing of the nano through holes, can realize the three-dimensional nano through holes with the depth of submicron to several microns, and provides an effective solution for the research in the fields of micro-nano fluidic, biomedicine, bionic functional materials and the like.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. A manufacturing method of a three-dimensional nano through hole is based on a laser direct writing system and is characterized by comprising the following steps:
preparing a substrate: preparing a substrate with micropores and coating a negative photoresist film on one surface of the substrate;
carrying out laser direct writing: carrying out multiple exposures at the position of the micron hole of the substrate;
and (3) carrying out photoresist development: and developing the negative photoresist to obtain the three-dimensional nano through hole.
2. The method of claim 1, wherein the laser direct writing process comprises:
modulating light field parameters in the laser direct writing system to obtain annular space structured light;
and calibrating the laser focus to the center of the micropore, so that the laser focus is positioned in the negative photoresist film for multiple exposure.
3. The method for manufacturing three-dimensional nano through hole according to claim 2, wherein the specific process after obtaining the annular space structure light comprises:
and adjusting the outer diameter of the annular space structure light to be larger than the diameter of the micron hole on the substrate, and then gradually reducing the topological number of the space structure light until the optical size of the annular space structure light is controlled to be 1, and carrying out exposure once when each pair corresponds to a different topological number.
4. The method of claim 3, wherein the fabricating process further comprises: and controlling the diameter of the three-dimensional nano through hole by controlling the exposure dose of the annular space structure light.
5. The method as claimed in claim 3, wherein the light intensity of the central region of the annular space structure light is zero.
6. The method as claimed in claim 2, wherein the step of aligning the laser focus to the center of the micro-holes to make the laser focus in the negative photoresist film for multiple exposures comprises: the exposure dose of the structured light in the peripheral annular space is higher than that of the structured light in the inner annular space.
7. The method of claim 1, wherein the developing comprises: developing the negative photoresist by the developing solution, removing the photoresist corresponding to the zero light intensity area, and generating the nano through hole.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6577799B1 (en) * | 1998-07-03 | 2003-06-10 | The Australian National University | Laser direct writing of planar lightwave circuits |
| CN103011058A (en) * | 2012-12-13 | 2013-04-03 | 中国科学院物理研究所 | Method for preparing three-dimensional hollow micro nanometer functional structure by utilizing laser direct writing |
| CN112540457A (en) * | 2020-12-10 | 2021-03-23 | 武汉先河激光技术有限公司 | Vortex light beam generation device, system and method with adjustable topological number |
-
2021
- 2021-09-18 CN CN202111112640.8A patent/CN113805433A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6577799B1 (en) * | 1998-07-03 | 2003-06-10 | The Australian National University | Laser direct writing of planar lightwave circuits |
| CN103011058A (en) * | 2012-12-13 | 2013-04-03 | 中国科学院物理研究所 | Method for preparing three-dimensional hollow micro nanometer functional structure by utilizing laser direct writing |
| CN112540457A (en) * | 2020-12-10 | 2021-03-23 | 武汉先河激光技术有限公司 | Vortex light beam generation device, system and method with adjustable topological number |
Non-Patent Citations (2)
| Title |
|---|
| FAN LIANBIN等: "Direct CW-Laser Writing Sub-Diffraction-Limit Nanopore Array Based on the Low One-Photon Absorption of Polymer", 《RARE METAL MATERIALS AND ENGINEERING》 * |
| 王凯歌 等: "基于连续激光的纳米结构研制", 《应用光学》 * |
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