CN111054918A - Method for accurately preparing superfine metal micro-pillar array suitable for controllable biosensor spacing - Google Patents
Method for accurately preparing superfine metal micro-pillar array suitable for controllable biosensor spacing Download PDFInfo
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- B22—CASTING; POWDER METALLURGY
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F12/00—Apparatus or devices specially adapted for additive manufacturing; Auxiliary means for additive manufacturing; Combinations of additive manufacturing apparatus or devices with other processing apparatus or devices
- B22F12/30—Platforms or substrates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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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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- 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
- G03F7/2051—Exposure without an original mask, e.g. using a programmed deflection of a point source, by scanning, by drawing with a light beam, using an addressed light or corpuscular source
- G03F7/2053—Exposure without an original mask, e.g. using a programmed deflection of a point source, by scanning, by drawing with a light beam, using an addressed light or corpuscular source using a laser
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/36—Process control of energy beam parameters
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention relates to a method for accurately preparing an ultra-fine metal micro-pillar array suitable for a biosensor with controllable space. The preparation method comprises the following steps: 1) cleaning the substrate with the nanopore array, and drying; 2) spin-coating photoresist on the surface of the substrate, and drying; 3) designing a pattern of the micron column array by using laser direct writing equipment, exposing a corresponding region according to the design, and removing photoresist in the region corresponding to the micron column array by using developing solution; 4) applying negative pressure to the bottom of the substrate, filling the metal nano slurry into the micron column array region from which the photoresist is removed, and finally grinding; 5) pressing the light transmitting sheet on the top of the base, then scanning the light transmitting sheet by laser, and sintering and solidifying the metal slurry; 6) and removing the residual photoresist to obtain the superfine metal micron column array. The method can be used for randomly designing the external appearance and array arrangement of the superfine metal micron column, the obtained superfine metal micron column has regular shape and no defect, has high size precision, and is favorable for signal enhancement and signal transmission when being used in a biosensor.
Description
Technical Field
The invention belongs to the field of micro-nano electronic science and technology, and particularly relates to a method for accurately preparing an ultra-fine metal micro-column array suitable for a biosensor with controllable spacing.
Background
When the superfine metal micro-cylinder array is irradiated by light, peripheral light waves of the superfine metal micro-cylinder array can generate obvious near-field enhancement due to local plasmon resonance, and a good resonance peak can be obtained. The unique optical phenomenon enables the superfine metal micro-column array to have good application prospect in the aspect of biosensing. In recent years, research on rapid large-area preparation of diversified ultrafine metal micro-pillars and arrays thereof has received wide attention.
The existing method for preparing the biosensor ultra-fine metal micro-column array mainly comprises a nano-imprinting method, a mold synthesis method, a focused ion beam etching method, traditional photoetching and other methods. The nano-imprinting method mainly depends on a mold, and a microstructure which is complementary with the pattern of the mold is obtained through the extrusion of a micropore mold; however, the nano-imprinting method may cause undue compressive stress, which may cause distortion of the ultra-fine metal micro-pillar array structure. The mold synthesis method is to fill the nano material into the micropores of the corresponding mold, heat and solidify the nano material, and then separate the mold, so as to obtain the corresponding superfine metal micro-column array structure; however, the ultrafine metal micro-pillar array is easy to break the array pattern in the process of separating from the mold. The focused ion beam etching method is to bombard the surface of the related material by ion beams to accurately prepare the superfine metal micro-column array; this method is slow and costly to produce. The traditional photoetching method has special advantages in the aspect of preparing ordered strip-shaped nano arrays; however, when the micro-nano scale array is prepared, due to the existence of air pressure, the nano slurry cannot be fully filled into the photoresist array groove, so that the prepared superfine metal micro-column and the array bottom thereof have more defects.
Disclosure of Invention
The invention aims to provide a method for accurately preparing an ultra-fine metal micro-cylinder array suitable for a biosensor with controllable space, the method can be used for randomly designing the appearance of the ultra-fine metal micro-cylinder and the array arrangement of the ultra-fine metal micro-cylinder, has strong flexibility and good repeatability, the shape of the obtained ultra-fine metal micro-cylinder is regular and has no defect, and the gaps among the ultra-fine metal micro-cylinders are small, so that the method is favorable for signal enhancement and signal transmission in the biosensor.
In order to solve the technical problem, the invention adopts the following scheme:
the invention provides a method for accurately preparing an ultra-fine metal micro-pillar array suitable for a biosensor with controllable spacing, which comprises the following steps:
1) cleaning the substrate with the nanopore array, and drying the substrate;
2) spin-coating photoresist on the surface of the substrate, and drying;
3) designing a pattern of the micron column array by using laser direct writing equipment, then exposing photoresist of a corresponding pattern region on the substrate, and removing the photoresist of the corresponding region of the micron column array by using developing solution;
4) applying negative pressure to the bottom of the substrate, filling the metal nano slurry into the region corresponding to the micron column array in which the photoresist is removed in the step 3), and grinding to ensure that the thickness of the metal nano slurry is consistent with that of the residual photoresist;
5) pressing the light-transmitting sheet on the area corresponding to the metal nano-slurry obtained in the step 4), then scanning the area occupied by the metal nano-slurry by laser passing through the light-transmitting sheet, and sintering and solidifying the metal nano-slurry;
6) and removing the residual photoresist to obtain the ultra-fine metal micro-pillar array with controllable space suitable for the biosensor.
According to the scheme, in the step 1), the substrate is sequentially cleaned by using acetone, absolute ethyl alcohol and deionized water.
According to the scheme, in the step 1), the substrate is Sapphire, gallium nitride and SiO2One kind of (1).
According to the scheme, in the step 1), the nanopore array on the substrate is an array formed by round holes, wherein the diameter of each round hole is 100-150 nm, and the gaps among the round holes are 100-150 nm.
According to the scheme, in the step 2), the spin-coating speed is 2000-3000 rpm, and the spin-coating time is 20-30 s; the drying temperature is 95-105 ℃, and the drying time is 2-3 min.
According to the scheme, in the step 3), the power density of the laser direct writing equipment is 100-120 mJ/cm2。
According to the scheme, in the step 3), the time for cleaning the exposure area by the developing solution is 30-45 s.
According to the scheme, in the step 3), the gap between the micron columns in the micron column array is more than or equal to 300 nm.
According to the scheme, in the step 3), the micron column is one or more of a cylinder, a triangular column, a square column and a polygonal column.
According to the scheme, in the step 4), the particle size of the metal nanoparticles is 10-20 nm; the concentration of the metal nano-slurry is 0.5-1 mg/ml.
According to the scheme, in the step 4), the metal nanoparticles are one or a mixture of more of gold, silver, iron, nickel, platinum, cobalt and tin.
According to the scheme, in the step 4), the applied negative pressure is-2000 to-1000 Pa.
According to the scheme, in the step 4), the rotating speed of the adopted grinding equipment is 30-60 rpm, and the time is set to be 0.5-1
min。
According to the scheme, in the step 5), the adopted light-transmitting sheet is rigid light-transmitting common glass with a smooth surface, and the thickness of the glass is 0.1-1 mm.
According to the scheme, in the step 5), the scanning speed of the laser is 800-1000 mm/s, the diameter of a light spot is 8-10 um, and the power of the laser is 260-365 mW.
The invention has the beneficial effects that:
1. the invention prepares the superfine metal micro-column array by the laser direct writing technology, can design the appearance and array arrangement of the superfine metal micro-column at will, accurately control the gap size of the superfine metal micro-column, simultaneously, the substrate has the nano-pore array in the preparation process, and can promote the metal nano-slurry to be fully filled in a small-size space by applying negative pressure, and the obtained superfine metal micro-column has regular shape without defects, complete structure, high size precision and uniform thickness.
2. The minimum gap of the superfine metal micro-column array obtained by the invention can reach 300nm, the signal enhancement and signal transmission requirements of almost all visible light sources (380-780 nm) and infrared light sources (780 nm-1 mm) in the biosensor are met, the shape is regular and is free of defects, and the comprehensive performance of the biosensor can be obviously improved.
3. The laser sintering method is used for sintering and curing the metal nano-slurry, so that the speed is high and the precision is high.
Drawings
FIG. 1 is a flowchart illustrating the operation of a method for precisely fabricating an array of ultra-fine metal micro-pillars with controllable pitches for biosensors according to an embodiment of the present invention;
FIG. 2 is an optical microscope image of the photoresist after developing in step 3) according to one embodiment of the present invention;
FIG. 3 is a schematic diagram of a square ultra-fine metal micro-pillar array fabricated in accordance with one embodiment of the present invention;
FIG. 4 is an optical microscope photograph showing the photoresist developed in step 3) in the second embodiment of the present invention;
FIG. 5 is a schematic view of a circular ultrafine metal micro-pillar array prepared in the second embodiment of the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and with reference to the attached drawings.
< example one >
As shown in fig. 1, this embodiment provides a method for accurately preparing an ultra-fine metal micro-pillar array suitable for a biosensor, which specifically includes the following steps:
1) selecting Sapphire as a substrate, wherein a nanopore array is arranged on the substrate and is an array formed by round holes, the diameter of each round hole is 100nm, and the gap between the round holes is 100 nm; the organic impurities on the substrate are washed with acetone, followed by washing the substrate with absolute ethanol and dissolving the acetone, followed by washing the substrate with deionized water and dissolving the ethanol. After the cleaning is finished, using N2And drying the substrate.
2) Placing the Sapphire substrate on a spin coater, dripping a plurality of drops of photoresist on the Sapphire substrate, starting the spin coater to start spin coating, and setting the rotation speed to be 3000rpm and the rotation time to be 20 s; (the photoresist used this time is negative). After the spin coating is finished, putting the substrate covered with the photoresist on a high-temperature dryer for drying, wherein the drying temperature is 95 ℃, and the drying time is 3 min;
3) after drying, the substrate covered with the photoresist is placed on an objective table of laser direct writing equipment, and the laser direct writing equipment prepares a square micrometer column array pattern according to a set program, wherein the size of the top of a square micrometer column is 2 multiplied by 2um, and the gap between the upper, lower, left and right adjacent micrometer columns is 400 nm. The laser exposure position is a gap area between the micrometer posts, and the energy density of the laser direct writing equipment is set to be 100mJ/cm2. After the photoetching is finished, transferring the exposed substrate into a developing solution for 45s, and dissolving the photoresist of the square micron column array while keeping the photoresist of the gap area between the square micron columns, wherein the corresponding structure is shown in FIG. 2;
4) filling silver nano slurry with the particle size of 10-15 nm and the concentration of 0.5mg/ml to a micro-column array region where the photoresist is removed, uniformly coating the silver nano slurry on the surface of the photoresist by using a scraper, and applying air pressure of-2000 Pa to the bottom of the substrate. Then, grinding the photoresist and the silver nano-slurry on the upper surface of the substrate by using grinding equipment, wherein the rotating speed of the grinding equipment is set to be 60rpm, and the time is set to be 30 s;
5) placing a transparent glass sheet with the thickness of 1mm on the surface of the substrate coated with the photoresist, and scanning the filled silver nano material by laser passing through the transparent glass sheet; wherein, the transparent glass sheet is placed on the photoresist, and the filled silver nano material is pressed; the adopted laser is femtosecond laser, the power of the laser is 260mW, the scanning speed is 800mm/s, and the diameter of a light spot is 8 um;
6) after the laser scanning is finished, the photoresist is dissolved by acetone, and the square ultra-fine metal micro-pillar array with controllable space suitable for the biosensor is obtained, and the specific structure is shown in figure 3.
< example two >
As shown in fig. 1, this embodiment provides a method for accurately preparing an ultra-fine metal micro-pillar array suitable for a biosensor, which specifically includes the following steps:
1) selecting Sapphire as a substrate, wherein a nano-pore array is arranged on the substrate, and the nano-pore array is an array formed by round holes, wherein the diameter of each round hole is 150nm, and the gap between the round holes is 150 nm; the organic impurities on the substrate are washed with acetone, followed by washing the substrate with absolute ethanol and dissolving the acetone, followed by washing the substrate with deionized water and dissolving the ethanol. After the cleaning is finished, using N2And drying the substrate.
2) Placing the Sapphire substrate on a spin coater, dripping a plurality of drops of photoresist on the Sapphire substrate, then starting the spin coater to start spin coating, and setting the rotation speed to be 2000rpm and the rotation time to be 30 s; (the photoresist used this time is negative). After the spin coating is finished, putting the substrate covered with the photoresist on a high-temperature dryer for drying, wherein the drying temperature is 105 ℃, and the drying time is 120 s;
3) after drying, the substrate covered with the photoresist is placed on an objective table of laser direct writing equipment, and the laser direct writing equipment prepares a circular micron column array pattern according to a set program, wherein the diameter of the circumference of the top of the circular micron column is 2 microns, and the gap between any two adjacent micron columns is 1 micron. The laser exposure position is a gap area between the micrometer posts, and the energy density of the laser direct writing equipment is set to be 120mJ/cm2. After the photoetching is finished, transferring the exposed substrate into a developing solution for 30s, and dissolving the photoresist on which the circular micron column array is located while keeping the photoresist in the gap area between the circular micron columns, wherein the corresponding structure is shown in FIG. 4;
4) filling the silver nano slurry with the particle size of 15-20 nm and the concentration of 1mg/ml to a micro-column array area where the photoresist is removed, uniformly coating the silver nano slurry on the surface of the photoresist by using a scraper, and applying the air pressure of-1000 Pa to the bottom of the substrate. Then, grinding the photoresist and the silver nano-slurry on the upper surface of the substrate by using grinding equipment, wherein the rotating speed of the grinding equipment is set to be 30rpm, and the time is set to be 60 s;
5) placing a transparent glass sheet with the thickness of 0.1mm on the surface of the substrate coated with the photoresist, and scanning the filled silver nano material by laser passing through the transparent glass sheet; wherein, the transparent glass sheet is placed on the photoresist, and the filled silver nano material is pressed; the adopted laser is femtosecond laser, the power of the laser is 365mW, the scanning speed is 1000mm/s, and the diameter of a light spot is 10 um;
6) after the laser scanning is finished, the photoresist is dissolved by acetone, and the circular ultra-fine metal micro-column array with controllable space suitable for the biosensor is obtained, and the corresponding structure is shown in fig. 5.
The above embodiments are merely illustrative of the technical solutions of the present invention. The method for preparing the patterned transparent conductive electrode by using the laser according to the present invention is not limited to the description in the above embodiments, but is subject to the scope defined by the claims. Any modification or supplement or equivalent replacement made by a person skilled in the art on the basis of this embodiment is within the scope of the invention as claimed in the claims.
Claims (10)
1. A method for accurately preparing an ultra-fine metal micro-pillar array suitable for a biosensor with controllable spacing is characterized by comprising the following steps:
1) cleaning the substrate with the nanopore array, and drying the substrate;
2) spin-coating photoresist on the surface of the substrate, and drying;
3) designing a pattern of the micron column array by using laser direct writing equipment, then exposing photoresist of a corresponding pattern region on the substrate, and removing the photoresist of the corresponding region of the micron column array by using developing solution;
4) applying negative pressure to the bottom of the substrate, filling the metal nano slurry into the region corresponding to the micron column array in which the photoresist is removed in the step 3), and grinding to ensure that the thickness of the metal nano slurry is consistent with that of the residual photoresist;
5) pressing the light-transmitting sheet on the area corresponding to the metal nano-slurry obtained in the step 4), then scanning the area occupied by the metal nano-slurry by laser passing through the light-transmitting sheet, and sintering and solidifying the metal nano-slurry;
6) and removing the residual photoresist to obtain the ultra-fine metal micro-pillar array with controllable space suitable for the biosensor.
2. The method as claimed in claim 1, wherein in the step 1), the substrate is washed sequentially with acetone, absolute ethyl alcohol and deionized water; the substrate is Sapphire, gallium nitride, SiO2One of (1); in the step 5), the light-transmitting sheet is rigid light-transmitting common glass with a smooth surface, and the thickness of the glass is 0.1-1 mm.
3. The method of claim 1, wherein in step 1), the nanopore array on the substrate is an array of circular holes, wherein the diameter of the circular holes is 100-150 nm, and the gap between the circular holes is 100-150 nm.
4. The method according to claim 1, wherein in the step 2), the spin coating speed is 2000-3000 rpm, and the spin coating time is 20-30 s; the drying temperature is 95-105 ℃, and the drying time is 2-3 min; in the step 3), the time for cleaning the exposure area by the developing solution is 30-45 s; in the step 4), the rotation speed of the grinding equipment is 30-60 rpm, and the time is set to be 0.5-1 min.
5. The method according to claim 1, wherein in the step 3), the power density of the laser direct writing device is 100-120 mJ/cm2。
6. The method as claimed in claim 1, wherein in step 3), the gap between the micropillars in the micropillar array is not less than 300 nm.
7. The method according to claim 1, wherein in the step 3), the micro-pillars are one or more of cylindrical pillars, triangular pillars, square pillars and polygonal pillars.
8. The method according to claim 1, wherein in the step 4), the metal nanoparticles have a particle size of 10 to 20 nm; the concentration of the metal nano-slurry is 0.5-1 mg/ml; the metal nano-particles are one or a mixture of more of gold, silver, iron, nickel, platinum, cobalt and tin.
9. The method according to claim 1, wherein in step 4), the negative pressure applied is between-2000 and-1000 Pa.
10. The method according to claim 1, wherein in the step 5), the scanning speed of the laser is 800-1000 mm/s, the diameter of the light spot is 8-10 um, and the power of the laser is 260-365 mW.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116140938A (en) * | 2023-03-06 | 2023-05-23 | 广东工业大学 | Processing method of macro-micro composite array wear-resistant super-hydrophobic surface and metal piece |
| CN117747455A (en) * | 2024-02-21 | 2024-03-22 | 北京大学 | Micro-bump substrate based on laser processing, preparation method and micro-bump interconnection structure |
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| CN108535967A (en) * | 2018-03-26 | 2018-09-14 | 太原理工大学 | A kind of preparation method of polymer nanocomposite column array |
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| CN116140938A (en) * | 2023-03-06 | 2023-05-23 | 广东工业大学 | Processing method of macro-micro composite array wear-resistant super-hydrophobic surface and metal piece |
| CN116140938B (en) * | 2023-03-06 | 2024-01-30 | 广东工业大学 | Processing method of macro-micro composite array wear-resistant super-hydrophobic surface and metal piece |
| CN117747455A (en) * | 2024-02-21 | 2024-03-22 | 北京大学 | Micro-bump substrate based on laser processing, preparation method and micro-bump interconnection structure |
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