CN112079328A - T-shaped cantilever beam microstructure and processing method and application thereof - Google Patents
T-shaped cantilever beam microstructure and processing method and application thereof Download PDFInfo
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- CN112079328A CN112079328A CN202010844382.1A CN202010844382A CN112079328A CN 112079328 A CN112079328 A CN 112079328A CN 202010844382 A CN202010844382 A CN 202010844382A CN 112079328 A CN112079328 A CN 112079328A
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- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00134—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems comprising flexible or deformable structures
- B81C1/0015—Cantilevers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B3/00—Devices comprising flexible or deformable elements, e.g. comprising elastic tongues or membranes
- B81B3/0064—Constitution or structural means for improving or controlling the physical properties of a device
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00642—Manufacture or treatment of devices or systems in or on a substrate for improving the physical properties of a device
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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
Abstract
The invention belongs to the technical field of micro-nano processing, and discloses a T-shaped cantilever beam microstructure and a processing method and application thereof. The method is to grow SiN on the surface of a cleaned silicon substrate by adopting a low-pressure chemical vapor deposition method at 800-850 DEG C4Then spin-coating photoresist, covering the mask plate on the photoresist, and irradiating the SiN layer under ultraviolet light4Exposing and developing the photoresist on the surface of the layer to obtain a pattern; by photolithography on the silicon nitride substrate, various patterns are processed to reveal developed areas of the substrate, which are then exposed to CHF3/O2Under the condition, the developing area is etched by the plasma dry method; evaporating a noble metal film on the surface of the treated silicon nitride by using an electron beam, then immersing the gold-plated silicon nitride substrate into etching liquid for isotropic etching to obtain a microstructure with a wide top and a narrow bottom, and cleaning the surface of the microstructure to obtain the miniature T-shaped structureCantilever beam structure. The structure has super-hydrophobic and super-oleophobic properties, and can be applied to the fields of aquatic equipment, water and oil resistance, microfluidics technology or biomedical treatment and the like.
Description
Technical Field
The invention belongs to the technical field of organic semiconductors, and particularly relates to a T-shaped cantilever beam microstructure and a processing method and application thereof.
Background
Silicon is a semiconductor material widely applied to a microelectronic/nano electronic mechanical system, a super-amphiphobic surface (simultaneously has super-hydrophobic and super-oleophobic characteristics) is processed by taking silicon as a substrate, the wettability, the adhesive force, the wear resistance, the oil stain adhesion prevention performance and other performances of the surface layer of the silicon can be effectively controlled, and the silicon-based super-amphiphobic surface has wide application prospects. The research surface shows that the micro T-shaped cantilever beam structure processed on the surface of the silicon substrate meets the super-amphiphobic condition, so that super-hydrophobicity can be realized, and super-oleophobic property can be realized. However, how to process the T-shaped cantilever beam structure has great difficulty, such as:
chinese patent CN107974089A proposes a method for preparing isotropic super-hydrophobic super-oleophobic regular porous silicone rubber through an anisotropic structure, which comprises the steps of preparing silicone oil containing C ═ C double bonds, printing a catalyst and other materials, using ink, printing according to the characteristics of the anisotropic porous structure to prepare silicone rubber with a porous structure, drying and curing to obtain the isotropic super-hydrophobic super-oleophobic silicone rubber material. However, the method is complex to operate, difficult to expand production, expensive in cost, poor in mechanical durability and abrasion resistance of the super-amphiphobic surface, and extremely easy to damage or even fail due to physical abrasion.
Chinese patent CN201634414U proposes a method for processing a silicon substrate, which utilizes a laser processing method to construct a regular micron-submicron surface texture on the surface of the silicon substrate, and then implements a super-hydrophobic structure by self-assembling a molecular film. However, the microstructure processed by the method is only suitable for super-hydrophobicity, does not have super-oleophobic capability, and cannot prevent oil stain adhesion performance.
Chinese CN107346727A proposes a substrate cleaning method and a film forming method, in which a hydrophobic and oleophobic super-amphiphobic film layer is formed on a substrate by cleaning the substrate for multiple times. However, the super-amphiphobic film layer processed by the method is easy to fall off from the surface of the substrate, and the service life is greatly influenced. Therefore, a processing method of a micro T-shaped cantilever structure is urgently needed to provide, so that super-amphiphobic performance is realized, and components can be used in special occasions such as environments with high humidity, oil stains and the like.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention aims to provide a method for processing a T-shaped cantilever beam microstructure.
The invention also aims to provide the T-shaped cantilever beam microstructure prepared by the method.
The invention further provides an application of the T-shaped cantilever beam microstructure.
The purpose of the invention is realized by the following technical scheme:
a processing method of a T-shaped cantilever beam microstructure comprises the following specific steps:
s1, growing silicon nitride (SiN) on the surface of the cleaned silicon substrate by adopting a low-pressure chemical vapor deposition method at 800-850 DEG C4) Then spin-coating photoresist, covering the photoresist with a mask plate with a required pattern, and irradiating the silicon nitride SiN with ultraviolet light4Exposing and developing the photoresist on the surface of the layer to obtain a pattern; the silicon nitride substrate is patterned by photolithography to form developed regions of the substrate, which are then exposed to CHF3/O2Under the condition, the developing area is anisotropically etched by a plasma dry method;
s2, evaporating a noble metal film on the silicon nitride surface treated in the step S1 by using an electron beam to obtain a noble metal plated silicon nitride substrate;
and S3, immersing the precious metal plated silicon nitride substrate into etching liquid, stirring, performing isotropic etching to obtain a microstructure with a wide upper part and a narrow lower part, and cleaning the surface of the microstructure to obtain the T-shaped cantilever beam microstructure.
Preferably, the cleaning process in step S1 is: firstly, using a mixture of 1:1 of 91 to 96 wt% of H2SO4And 25 to 30 wt% of H2O2And treating the piranha solution at 100-110 ℃ for 10-15 min, then treating the piranha solution for 2-3 min by using 2-5 wt% of HF solution, and finally drying the piranha solution by using nitrogen.
Preferably, the time of the vapor deposition in the step S1 is 30-35 min.
Preferably, the thickness of the silicon nitride in step S1 is 200 to 250 nm.
Preferably, the noble metal in step S2 is gold, silver or platinum; the thickness of the noble metal film is 12-16 nm.
Preferably, the etching solution in step S3 is HF, HNO3And CH3A mixture of COOH.
More preferably, the HF, HNO3And CH3The volume ratio of COOH is (2-4): (20-25): (10-12); the concentration of the HF is 48-50 wt%, and the HNO is3The concentration of (A) is 55-60 wt%: the concentration of CH3COOH is 95-98 wt%.
Preferably, the stirring speed in the step S3 is 300-350 rpm, and the etching time is 3-5 min.
A T-shaped cantilever beam microstructure is prepared by the method.
The T-shaped cantilever beam microstructure is applied to the fields of aquatic equipment, water and oil proofing, microfluidics technology or biomedical treatment.
The T-shaped cantilever beam microstructure of the invention is that a silicon nitride layer grows on the surface of a cleaned silicon wafer by using a low pressure chemical vapor deposition method (LPCVD); then, spin-coating photoresist on the surface of the silicon nitride layer, covering the photoresist with a mask plate with a required pattern, and developing and exposing the photoresist on the surface of the silicon nitride layer through ultraviolet light; exposing a developed region of the silicon nitride layer to CHF3/O2Performing dry etching in the atmosphere to remove part of the silicon nitride layer which is not covered by the photoresist; evaporating a noble metal film as a catalyst, performing isotropic etching by using etching liquid to obtain a microstructure with a wide top and a narrow bottom, and etching a silicon waferAnd taking out, removing the unreacted photoresist and the noble metal film, and cleaning and drying to obtain the T-shaped cantilever beam microstructure.
The principle of the invention for realizing the super-hydrophobic and super-oleophobic function is as follows: when liquid contacts the rough surface of the micro-nano structure with the wide upper part and the narrow lower part, the liquid wets the top surface of the rough structure and flows downwards along the side wall of the vertical cantilever, but stagnates at the bottom of the vertical cantilever, and the super-hydrophobic and super-oleophobic property of the T-shaped cantilever structure is caused because the direction of the liquid surface tension is turned upwards.
Compared with the prior art, the invention has the following beneficial effects:
1. there are generally two methods of preparing lyophobic surfaces: firstly, constructing a micro-nano coarse structure on the surface of a lyophobic material with low surface energy; and secondly, modifying the micro-nano coarse structure by using a low surface energy substance. By manufacturing the T-shaped cantilever beam microstructure, the super-hydrophobic and super-oleophobic properties can be obtained without further reducing the surface energy.
2. The invention processes the micro cantilever beam structure with wide top and narrow bottom by a simple chemical etching method, and the structure has good super-hydrophobic and super-oleophobic properties.
3. The super-hydrophobic and super-oleophobic material has potential application in an oil/water/solid three-phase system, and can be applied in the fields of self-cleaning, ship corrosion prevention, water and oil prevention, microfluidics technology and the like.
Drawings
FIG. 1 is a process flow diagram of the processing method of the T-shaped cantilever microstructure of the present invention.
FIG. 2 is a schematic view of the process flow structure of the T-shaped cantilever microstructure of the present invention.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
FIG. 1 is a process flow diagram of a processing method of a T-shaped cantilever beam microstructure of the present invention, and FIG. 2 is a schematic flow structure diagram of the processing method of the T-shaped cantilever beam microstructure of the present invention. Wherein 11 is a silicon substrate layer; 12 is a silicon nitride layer; 13 is a photoresist layer; 21 is an ultraviolet light device; 23 is a mask plate; 24 is a plasma device; 25 is electron beam evaporation equipment; 14 is a noble metal film coating; 15 is etching liquid; 26 is a tetrafluoro beaker for containing etching liquid; 16 is a silicon etching structure; 27 is a stirrer; and 17 is a partially enlarged T-shaped cantilever beam microstructure. As shown in fig. 1 and 2, a method for processing a T-shaped cantilever microstructure includes the following steps:
1. with piranha solution (H)2SO4(96wt％)：H2O2(30 wt%) 1:1,) cleaning the silicon substrate layer 11 at 110 deg.c for 10min, and then blow-drying with nitrogen gas, as shown in fig. 2 (a).
2. Treating the silicon substrate layer 11 in Low Pressure Chemical Vapor Deposition (LPCVD) at 800 deg.C for 30min to grow a silicon nitride layer (SiN) with a thickness of 200nm on the silicon surface4)12 as shown in fig. 2 (b).
3. Spin-coating a photoresist layer 13 (positive photoresist) on the surface of the silicon nitride layer 12 by using a spin coater, and then covering the photoresist layer 13 with a mask plate 23 having a desired pattern, as shown in fig. 2 (c); the exposure is performed under ultraviolet light of an ultraviolet light device 21, and finally, a pattern is developed, as shown in fig. 2 (d).
4. Exposing the developed silicon nitride to CHF3/O2The plasma device 24 under the conditions performs dry etching to etch away the silicon nitride layer developed in step 3, as shown in fig. 2 (e).
5. The noble metal film plating layer (gold film) 14 having a thickness of 12nm was evaporated on the silicon substrate surface treated in step S4 by the electron beam evaporation apparatus 25 as shown in fig. 2 (f).
6. Then, the silicon substrate layer was immersed in an etching solution 15 (50 wt% HF: 60 wt% HNO in a volume ratio of 4: 25: 12) with stirring at 350rpm at room temperature using a stirrer 273：98wt％CH3Mixed liquid of COOH) to isotropic etchingIt should be 5min, as shown in (g) of FIG. 2.
7. And taking out the silicon substrate layer in the etching solution 15, washing the surface of the silicon substrate layer with deionized water for 5min to stop the etching reaction, and then blowing the surface to dry with nitrogen. Cleaning the surface with acetone, cleaning with absolute ethyl alcohol for 5min, cleaning with deionized water for 5min, cleaning the unreacted photoresist and gold film, and drying the surface with nitrogen to obtain the silicon etched structure 16, which is a cantilever beam microstructure with a wide top and a narrow bottom, namely a partially enlarged T-shaped cantilever beam micro-junction 17, as shown in (h) of FIG. 2.
Example 2
The difference from example 1 is that: step 2, the time of the 850 ℃ low-pressure vapor deposition is 35min, and the silicon nitride SiN4The thickness was 250 nm. And 5, the thickness of the evaporated gold film is 16 nm. Stirring at 300rpm at room temperature, and immersing the silicon substrate into etching solution (48 wt% HF: 55 wt% HNO with the volume ratio of 1:10: 5)3：95wt％CH3COOH mixed solution) for 3 min.
When liquid contacts the cantilever beam microstructure surface with wide top and narrow bottom, the T-shaped cantilever beam microstructure 17 of the invention wets the top of the surface, then flows downwards along the vertical side wall until the liquid flows to the bottom of the vertical cantilever, and at this time, the direction of the liquid surface tension turns upwards, so that the microstructure surface is not soaked any more, thereby achieving the properties of super-hydrophobicity and super-oleophobicity.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A processing method of a T-shaped cantilever beam microstructure is characterized by comprising the following specific steps:
s1, growing silicon nitride on the cleaned silicon substrate surface by adopting a low-pressure chemical vapor deposition method at 800-850 ℃, then spin-coating photoresist, and using a mask plate with a required patternCovering on the photoresist, and irradiating with ultraviolet light to obtain SiN4Exposing and developing the photoresist on the surface of the layer to obtain a pattern; the silicon nitride substrate is patterned by photolithography to form developed regions of the substrate, which are then exposed to CHF3/O2Under the condition, the developing area is anisotropically etched by a plasma dry method;
s2, evaporating a noble metal film on the silicon nitride surface treated in the step S1 by using an electron beam to obtain a noble metal plated silicon nitride substrate;
and S3, immersing the precious metal plated silicon nitride substrate into etching liquid, stirring, performing isotropic etching to obtain a microstructure with a wide upper part and a narrow lower part, and cleaning the surface of the microstructure to obtain the T-shaped cantilever beam microstructure.
2. The method of claim 1, wherein the step of cleaning in step S1 is as follows: firstly, using a mixture of 1:1 of 91 to 96 wt% of H2SO4And 25 to 30 wt% of H2O2And treating the piranha solution at 100-110 ℃ for 10-15 min, then treating the piranha solution for 2-3 min by using 2-5 wt% of HF solution, and finally drying the piranha solution by using nitrogen.
3. The method as claimed in claim 1, wherein the time of vapor deposition in step S1 is 30-35 min.
4. The method as claimed in claim 1, wherein the thickness of the silicon nitride in step S1 is 200-250 nm.
5. The method as claimed in claim 1, wherein the noble metal in step S2 is gold, silver or platinum; the thickness of the noble metal film is 12-16 nm.
6. The method of claim 1, wherein the etching solution in step S3 is HF、HNO3And CH3A mixture of COOH.
7. The method of claim 6, wherein the HF and HNO are selected from the group consisting of HF, HNO, and a mixture thereof3And CH3The volume ratio of COOH is (2-4): (20-25): (10-12); the concentration of the HF is 48-50 wt%, and the HNO is3The concentration of (A) is 55-60 wt%: CH (CH)3The concentration of COOH is 95-98 wt%.
8. The processing method of the T-shaped cantilever beam microstructure according to claim 1, wherein the stirring speed in step S3 is 300-350 rpm, and the etching time is 3-5 min.
9. A T-type cantilever microstructure, wherein the T-type cantilever microstructure is prepared by the method of any one of claims 1-8.
10. The use of the T-shaped cantilever microstructure of claim 9 in aquatic devices, water and oil repellency, microfluidic technology, or biomedical applications.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112618946A (en) * | 2020-12-16 | 2021-04-09 | 同济大学 | Pyramid-shaped flexible microneedle array and preparation method thereof |
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| CN102556949A (en) * | 2012-01-13 | 2012-07-11 | 合肥工业大学 | Preparation method of silicon micro/nanometer line array with controllable dimension |
| CN105789042A (en) * | 2016-03-29 | 2016-07-20 | 苏州大学 | Preparation technology of silicon micro wire array |
| CN111115548A (en) * | 2019-11-25 | 2020-05-08 | 广东工业大学 | Mushroom-shaped super-hydrophobic-super-oleophobic PDMS micro-nano composite array and preparation method and application thereof |
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| CN1884039A (en) * | 2005-06-23 | 2006-12-27 | 中国科学院微电子研究所 | Method for making single-layer bimaterial micro-cantilever beam heat-shield focal plane array |
| CN102427083A (en) * | 2011-11-10 | 2012-04-25 | 中山大学 | Water and oil repellency surface microstructure and manufacturing method thereof |
| CN102556949A (en) * | 2012-01-13 | 2012-07-11 | 合肥工业大学 | Preparation method of silicon micro/nanometer line array with controllable dimension |
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| CN112618946A (en) * | 2020-12-16 | 2021-04-09 | 同济大学 | Pyramid-shaped flexible microneedle array and preparation method thereof |
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