CN114477078A - Processing method and application of integrated cross-scale micro-nano column array - Google Patents
Processing method and application of integrated cross-scale micro-nano column array Download PDFInfo
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- 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
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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
- B81B3/0018—Structures acting upon the moving or flexible element for transforming energy into mechanical movement or vice versa, i.e. actuators, sensors, generators
- B81B3/0021—Transducers for transforming electrical into mechanical energy or vice versa
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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
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
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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
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
- B81C1/00492—Processes for surface micromachining not provided for in groups B81C1/0046 - B81C1/00484
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
Abstract
The invention discloses a processing method and application of an integrated cross-scale micro-nano column array, wherein the processing steps are as follows: firstly, processing a micropore array with nanometer pits on the inner wall on a polymer template with a flexible film attached to the surface by femtosecond laser; and then removing the flexible film on the polymer template, coating the liquid flexible material on the surface of the polymer template and diffusing the liquid flexible material into the micropore array, and curing and demolding to obtain the integrated cross-scale micro-nano column array. The micro-nano structure prepared by the invention has the advantages of integration, flexibility, lightness, thinness, stability, reliability, easiness in integration and the like, is applied to the flexible micro-pressure sensor, and senses large pressure and micro pressure by using the micro-column and the nano-bulge, so that the flexible micro-pressure sensor can detect extremely small pressure and has the characteristics of wide linear range and high sensitivity.
Description
Technical Field
The invention relates to the technical field of micro-nano processing, in particular to a method for preparing an integrated cross-scale micro-nano column array.
Background
The main manifestation form of the trans-scale micro-nano structure is that micro-nano structures coexist in the same object, but the trans-scale micro-nano structure is divided into a core-shell structure, a mixed micro-structure with nano particles dispersed and a hierarchical heterostructure according to different shapes of the micro-structure and the nano-structure. The core-shell structure is formed by coating a layer of nanoscale same shape on the surface of a micron-sized sphere or cube; the mixed microstructure of dispersed nano-particles is uniformly dispersed nano-particles on the surfaces of micron-sized cubes or columns; the hierarchical heterogeneous micro-nano structure is generally formed by one-dimensional nanorods epitaxially growing on the surface of the micro-structure, thereby forming a hierarchical micro-nano structure composed of different materials. Compared with single-scale components, the trans-scale micro-nano structure shows unique performance in specific applications due to its micro-and nano-combined structure, such as: in the field of sensors, the microstructure can be used for sensing large pressure, and the nanostructure can be used for sensing small pressure; in the field of surface super-hydrophobicity, the micro-nano structure can be used for realizing super-hydrophobicity, and the functions of self-cleaning, anti-fog and anti-freezing, liquid drop transportation and the like are realized; in the field of optics, the absorption rate and the reflectivity of the surface of a material to light can be changed through a micro-nano structure, and then the color of the surface of an object is changed. Therefore, the cross-scale micro-nano structure has a wide application prospect in practical application, and a plurality of processing methods of the cross-scale micro-nano structure appear in the prior art.
In the current research, many researchers mostly adopt the technical methods of deposition, epitaxial growth, micro-nano processing and the like to prepare the cross-scale micro-nano structure, and the following four methods are mainly adopted. The first is chemical vapor deposition, which epitaxially grows nano-heterostructures in a highly controlled manner, and growth can be controlled by fine-tuning the growth temperature, reaction time, concentration, flow rate of the vapor precursor, and the properties of the precursor and substrate, as described by Zhao et al ACS Applied Materials&Interfaces (12 months 2020) reports that the application of three-dimensional carbon nanotube fiber sponge synthesized by chemical vapor deposition to piezoresistive sensors[1]However, this method requires more severe experimental conditions, such as high temperature and high vacuum; in addition, chemical vapor deposition requires a substrate to support the target material for growth, so additional processing is required to transfer the synthesized material for further research and applicationThe application is as follows. The second method for preparing the micro-Nano structure is electrochemical deposition, for example, Kong et al reported that the electrochemical deposition method is used to deposit Nano-scale zinc particles on the surface of a copper electrode in ACS Nano 2021, 9 months[2](ii) a The method can realize the epitaxial growth of the nano structure in the solution phase at room temperature, but the method has complex procedure and slow reaction, mainly deposits the nano structure on the surface of the metal, and has limited application of the metal in the field of flexible electronic devices. The third method is to use a more hydrothermal method, dissolve the reaction precursor together with a surfactant in water or an organic solvent, then introduce the mixed solution into a teflon-lined steel autoclave, and then heat the autoclave to above the boiling point of the solvent to generate high pressure in the autoclave to promote crystal growth. For example, Xiao et al reported that ZnO nanowire is hydrothermally grown on polystyrene surface in Advanced Materials 2011 and 10 months[3]By the method, high yield and large-scale synthesis of the epitaxial hybrid nanostructure can be realized at relatively low temperature and low cost, but the uniform growth of the nanostructure is difficult to realize in a controllable manner, and the reaction solution is toxic and harmful and is not easy to process. The fourth method is a micro-nano processing mode, and adopts a grading processing mode to process the micro-structure and then process the nano-structure. Methods employing graded lithography are reported by Wang et al in Advanced Functional Materials 2021[4]The first photoetching utilizes a micron-scale mask to etch a micron-scale structure, and the second photoetching utilizes a nanometer-scale mask to etch a nanometer-scale structure. At present, there are researches on forming micro-nano-pillars by orthogonally scanning flexible materials with femtosecond lasers, such as the preparation of micro-pillar arrays with granular nano-structures on surfaces by femtosecond lasers reported by Bai et al in "Chemical Engineering Journal" in 2019 in 10 months[5]However, the nanostructure is obtained by re-depositing and solidifying material scraps generated when the micro-column is processed by the femtosecond laser on the micro-column, and the nanostructure and the bulk material of the micro-column are non-integrated layered structures. In the method, the schemes of deposition and growth are mostly utilized, and the prepared micro-nano structures are all non-integrated layeredThe structure has the phenomena that the nano structure is easy to fall off and the performance is unstable when the structure is applied in a complex environment; although the integrated micro-nano structure can be prepared by adopting the photoetching method, the processing cost is high and the process is complex.
The non-integrated micro-nano layered structure, namely the micro-nano structure and the nano structure have a layered interface, and under the action of an external force, the nano structure is easy to peel off or fall off from the surface of the micro structure at the layered interface. Therefore, the research and development of a preparation method with a micron-nanometer integrated structure is urgently needed, the structure can effectively improve the overall stability and reliability of the micron-nanometer structure, the service life of a device is prolonged, and the structure can be widely applied to the field of flexible electronic devices.
Reference documents:
[1]ZHAO X F, HANG C Z, WEN X H, et al. Ultrahigh-Sensitive Finlike Double-Sided E-Skin for Force Direction Detection [J]. ACS Appl Mater Interfaces, 2020, 12(12): 14136-44.
[2]KONG H, SONG Z, LI W, et al. Skin-Inspired Hair-Epidermis-Dermis Hierarchical Structures for Electronic Skin Sensors with High Sensitivity over a Wide Linear Range [J]. ACS Nano, 2021, 15(10): 16218-27.
[3]XIAO X, YUAN L, ZHONG J, et al. High-strain sensors based on ZnO nanowire/polystyrene hybridized flexible films [J]. Adv Mater, 2011, 23(45): 5440-4.
[4]WANG X, YANG J, MENG K, et al. Enabling the Unconstrained Epidermal Pulse Wave Monitoring via Finger‐Touching [J]. Advanced Functional Materials, 2021, 31(32).
[5]BAI X, YANG Q, FANG Y, et al. Superhydrophobicity-memory surfaces prepared by a femtosecond laser [J]. Chemical Engineering Journal, 2020, 383。
disclosure of Invention
Based on the problems in the prior art, a first object of the present invention is to provide a method for processing an integrated trans-scale micro/nano column array, wherein dendritic nano structures are uniformly distributed on the surface of a micro column processed by the method, and the micro column and the nano structure are integrated structures without a layered interface. The invention also provides an application of the integrated cross-scale micro-nano column array in a flexible micro-pressure sensor, wherein a two-layer integrated cross-scale micro-nano column interlocking structure is adopted, the change of resistance caused by the change of the contact area between dendritic nano structures can sense micro pressure, and the change of the contact area between micro columns can sense large pressure, so that the requirement of measuring pressures with different sizes can be met, the integrated cross-scale micro-nano column array has the characteristics of wider linear range and high sensitivity, and has wide application prospects in the fields of wearable electronic skin, mechanical arms, human-computer interaction and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a processing method of an integrated cross-scale micro-nano column array, which mainly relates to femtosecond laser etching and polymer replica mold reversing, and mainly comprises the following steps: firstly, tightly attaching a polymer template to the surface of a high-flatness hard base material without gaps, and avoiding influence of the self curvature of the polymer template on the accuracy of femtosecond laser processing; secondly, attaching the flexible film on the surface of the polymer template, and generating a nano structure when the flexible film is used for femtosecond laser processing; then processing a polymer template attached with a flexible film by femtosecond laser, and processing a micropore array with a nanometer pit on the inner wall on the polymer template; then removing the flexible film attached to the surface of the polymer, coating the liquid flexible material on the surface of the polymer template and diffusing the liquid flexible material into the micropore array; and finally, after drying and curing, stripping the flexible material from the surface of the polymer template to form the flexible micro-nano column array with the integrated micro-nano structure. Compared with the prior art, the method can prepare the integrated flexible micro-nano structure array which is stable, reliable and good in consistency, and is simple in processing method, free of pollution to the environment and low in cost.
In the processing method, the key step of generating the integrated micro-nano column is to prepare the micropore array template with the nanometer pits on the inner wall. The flexible film is attached to the polymer template, when the flexible film and the polymer template are sequentially penetrated by the femtosecond laser, nanometer-scale flexible film splash with a certain temperature can be generated, part of splash can splash to the upper surface of the flexible film, the other part of splash can enter the inner wall of the micron hole of the polymer template, and the high temperature of the splash can melt the inner wall of the micron hole to form a compact nanometer pit. When the liquid flexible material is coated on the surface of the polymer template, the liquid flexible material can fill the micropores and the nanometer pits under the action of gravity and diffusion; and after drying and curing, peeling the flexible material from the polymer template to obtain the micro-column with the integrated micro-nano structure. In addition, the thickness of the flexible film can also be used as an auxiliary method for adjusting the micropore depth of the polymer template, namely, under the condition that the femtosecond laser processing power is not changed, the thicker the flexible film is, the smaller the micropore depth of the polymer template is. As shown in fig. 2, a flexible film is attached to the surface of a polymer template, and a micro-nano column with a dendritic nano structure is formed by femtosecond laser and polymer replica reverse molding; fig. 3 shows the micro-pillars processed under the same conditions except that the flexible film is not attached to the polymer surface, and it can be seen that the structure of fig. 3 has a height higher than that of fig. 2, is easy to bend, and has a relatively smooth surface, and it is difficult to obtain a dense nano-convex structure.
The femtosecond laser etching can process a three-dimensional structure in any shape with high precision, and heat is transmitted to the surface of a material through a high-energy laser beam, so that melting and vaporization are generated in a light spot irradiation area, and a microstructure is formed. Compared with chemical vapor deposition, femtosecond laser etching does not need vapor experimental conditions, the processing conditions are relatively easy to adjust, and three-dimensional microstructures with different shapes and sizes can be obtained by changing process parameters such as power, scanning time and scanning distance; compared with electrochemical deposition, the femtosecond laser etching can prepare a flexible micro-nano structure, and the flexible structure has wider application prospect; compared with a hydrothermal growth method, the prepared micro-nano column array is of an integrated structure, and the nano structure is more stable and reliable. In the invention, the femtosecond laser is utilized to process the micropore array on the surface of the polymer, and the three-dimensional microstructure with any shape can be processed by adjusting the processing power and the scanning time.
The invention is implemented by the following technical scheme: a processing method of an integrated cross-scale micro-nano column array comprises the following steps:
the method comprises the following steps that (1) a polymer template is tightly attached to the surface of a hard base material with high flatness through an adhesive to form a flat horizontal plane;
step (2), adhering the flexible film to the surface of the polymer template through the self adhesiveness;
processing a polymer template attached with a flexible film by using femtosecond laser, and processing a micropore array with a nano pit on the inner wall of the micropore array;
step (4), removing the flexible film on the upper surface after the processing is finished, attaching the limiting frame to the periphery of the polymer template, coating the prepared liquid flexible material in the limiting frame, and uniformly diffusing the liquid flexible material on the surface of the polymer template and in the micropore array;
and (5) drying and curing the liquid flexible material, and peeling the flexible material from the polymer template to obtain the integrated cross-scale micro-nano column array.
Further, the polymer template in the step (1) is a polymer material, specifically polytetrafluoroethylene, polyvinyl chloride, fluorinated ethylene propylene copolymer, and the like, the high-flatness hard substrate is a glass sheet, and the adhesive is a room-temperature curing type, a thermosetting type, an ultraviolet curing type, a hot-melt type or a pressure-sensitive adhesive, specifically, polyurethane, polyacrylate, a double-sided adhesive, and the like.
Further, the flexible film in the step (2) is polydimethylsiloxane, polyimide, epoxy resin, polyurethane, polyethylene terephthalate, polyethylene naphthalate, polyvinyl alcohol, polyamideimide, polycarbonate, or the like.
Further, the power of the femtosecond laser processing in the step (3) is 100-500mW, the center wavelength is 700-1000 nm, the pulse width is less than 120fs, the repetition frequency is 0.1-1000 KHz, the scanning speed is 10-100 mm/s, the laser scanning interval is 50-350 μm, and the scanning time of each micropore array is 100-300 ms.
Further, the liquid flexible material in the step (4) is polydimethylsiloxane solution, Ecoflex, Dragon Skin, or the like, and the limiting frame is a polymer material hollowed in the middle, specifically polytetrafluoroethylene, polyvinyl chloride, fluorinated ethylene propylene copolymer, or the like.
Further, the drying and curing conditions in the step (5) are 65 ℃ for 5 hours.
The integrated cross-scale micro-nano column array obtained based on the processing method comprises a substrate and the micro-nano column array, wherein the micro-nano column is formed by distributing dendritic nano structures on the surface of a micro column, and the micro column and the dendritic nano structures are of an integrated structure without a layered interface. Wherein the micron column array can be arranged into shapes of rectangle, circle, ring and the like according to actual requirements, the micron column actually presents a circular truncated cone shape, the diameter of the bottom surface of the circular truncated cone is 35-60 mu m, the diameter of the top surface of the circular truncated cone is 15-30 mu m, the height of the circular truncated cone is 120-200 mu m, and the density of the circular truncated cone is 1-3.24 x 108Per m2(ii) a The diameter of the dendritic nano structure is 800-950 nm; the thickness of the substrate is 100-500 μm.
By using the processing method, two same integrated cross-scale micro-nano column array single layers (the array density can be 1-3.24 x 10)8Per m2Adjusted within a range) can be assembled to form a flexible micro-pressure sensor. The method mainly comprises the following processing steps:
firstly, respectively carrying out magnetron sputtering on two prepared same integrated trans-scale micro-nano column arrays, and sputtering a layer of conductive metal material on the surfaces of the micro-nano column arrays for electric signal transmission of the sensor. The conductive metal material may be gold, silver, copper, etc., and the thickness of the conductive metal material is in the range of 50-100 nm.
And then, performing oxygen plasma hydrophilic treatment on the two integrated trans-scale micro-nano column arrays and the elastic layer, and then bonding to form a three-layer structure of the integrated trans-scale micro-nano column array, the elastic layer and the integrated trans-scale micro-nano column array from top to bottom, wherein the two micro-nano column arrays on the upper layer and the lower layer form an interlocking structure (the micro columns of the two arrays are alternately arranged to form the interlocking structure), and the elastic layer is positioned at the periphery of the two interlocked micro-nano column arrays, so that the flexible micro-pressure sensor is obtained.
In conclusion, the invention solves the problems of layered growth, non-integrated structure of micron and nanometer structures and easy falling off under stress in the traditional preparation of the micro-nano structure, provides a new method for preparing the integrated trans-scale micro-nano structure and also provides a new idea for preparing the flexible micro-pressure sensor.
Compared with the prior art, the invention has the beneficial effects that:
(1) the micro-nano structure in the flexible micro-pressure sensor prepared by the invention is integrated, and compared with a layered micro-nano structure prepared by a traditional growth mode, the integrated structure is uniform and stable, and does not fall off after repeated action for many times, which is an important premise for improving the stability and consistency of the sensor and prolonging the service life of devices.
(2) The micro-nano structure prepared by the invention is flexible, the micro-pressure sensor is also flexible, the state of the micro-pressure sensor can be changed according to the requirement, and the micro-nano structure prepared into wearable equipment has the characteristics of comfortable wearing and convenient carrying.
(3) The method for preparing the integrated micro-nano structure has the advantages of simple processing technology, low cost and better processing consistency, and the prepared flexible micro-pressure sensor has small size and is beneficial to subsequent integration and miniaturization packaging.
(4) The flexible micro-pressure sensor prepared by the integrated micro-nano structure can detect extremely small pressure (as low as 15 Pa), and has high sensitivity (which can reach 0.63/kPa under small pressure) and a wide detection range (15 Pa-25 kPa).
Drawings
Fig. 1 is a flow chart of a method for processing an integrated trans-scale micro-nanorod array.
FIG. 2 is a scanning electron microscope picture of the integrated trans-scale micro-nano column array.
FIG. 3 is a scanning electron microscope image of a smoother micropillar prepared without attaching a flexible film to the surface of a polymer template.
FIG. 4 is a scanning electron microscope picture of the integrated trans-scale micro-nanorod array.
FIG. 5 is a scanning electron microscope picture of the integrated trans-scale micro-nanorod array at another magnification.
Fig. 6 is a scanning electron microscope picture of a dendritic nanostructure on the surface of a single integrated trans-scale micro-nano column.
Fig. 7 is a schematic structural diagram of a flexible micro-pressure sensor.
Fig. 8 is a graph of the relative change in resistance of a flexible micro-pressure sensor as a function of pressure.
The reference numbers in the figures: 1-a hard substrate, 2-a polymer template, 3-a flexible film, 4-a limiting frame, 5-an integrated trans-scale micro-nano column array and 6-an elastic layer.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof will be described in detail with reference to the following examples. The following is merely exemplary and illustrative of the inventive concept and various modifications, additions and substitutions of similar embodiments may be made to the described embodiments by those skilled in the art without departing from the inventive concept or exceeding the scope of the claims defined thereby.
Example 1
As shown in fig. 1, the integrated cross-scale micro-nano column array is processed according to the following steps:
step (1), as shown in fig. 1-1, a polymer template 2 (800 μm thick ptfe) is tightly attached to the surface of a high-flatness rigid substrate 1 (glass substrate, 75 × 50 × 0.55 mm) by a double-sided adhesive tape to form a flat horizontal plane.
Step (2), as shown in 1-2 of fig. 1, a flexible film 3 (a polydimethylsiloxane film with the thickness of 200 μm) is adhered to the surface of the polymer template 2 through the self-adhesiveness; before attaching, the surface of the polymer template is wiped by alcohol, so that the cleanness of the surface of the polymer template is ensured, and the accuracy of femtosecond laser processing is not influenced.
Step (3), as shown in 1-3 in fig. 1, placing the polymer template attached with the flexible film in the femtosecond laser processing range, and processing a micropore array with nanometer pits on the inner wall on the surface by using the femtosecond laser; the specific technological parameters of the femtosecond laser processing are as follows: the power is 300mW, the central wavelength is 800nm, the pulse width is less than 104fs, the repetition frequency is 1kHz, the scanning speed is 10mm/s, the laser scanning interval is 70 mu m, and the scanning time of each micropore array is 200 ms.
And (4) as shown in 1-4 in fig. 1, removing the flexible film on the upper surface after the femtosecond laser processing is finished, and preparing for the next reverse mold process. As shown in fig. 1-5, a limiting frame 4 (a polytetrafluoroethylene film with a thickness of 500 μm, the thickness of the substrate of the micro-nano column array is adjusted by the thickness of the limiting frame, wherein the limiting frame is formed by scratching a rectangle on the central region of the polytetrafluoroethylene film and leaving only a rectangular frame at the edge as the limiting frame for limiting the flow of the liquid flexible material) is attached to the periphery of the polymer template 2, and the prepared flexible material (liquid polydimethylsiloxane, which is prepared by mixing a prepolymer and a curing agent according to a ratio of 10: 1) is poured into the limiting frame and uniformly diffused on the surface of the polymer template and inside the micro-pore array; after the surface is leveled, the mixture is placed in a drying oven at 65 ℃ for curing for 5 hours, and the horizontal state of the position of the mixture during curing is ensured.
And (5) drying and solidifying the liquid flexible material, and peeling the flexible material from the polymer template to obtain the integrated cross-scale micro-nano column array 5 as shown in 1-6 in figure 1.
Fig. 4 and 5 are scanning electron microscope images of the integrated cross-scale micro-nano column array processed in this embodiment at different magnifications, and fig. 6 is a scanning electron microscope image of a dendritic nano structure on the surface of a single integrated cross-scale micro-nano column. According to the figure, the integrated cross-scale micro-nano column array is composed of a substrate and the micro-nano column array, dendritic nano structures are distributed on the surfaces of micro columns, and the micro columns and the dendritic nano structures are of integrated structures without layered interfaces. Wherein the micron column array is rectangular, each micron column is actually in the shape of a circular truncated cone, the diameter of the bottom surface of the circular truncated cone is 35 mu m, and the diameter of the top surface of the circular truncated cone is15 μm, a height of 125 μm, and a density of 2.04 x 108Per m2(ii) a The diameter of the dendritic nanostructure is 900 nm; the thickness of the substrate was 500. mu.m.
The integrated cross-scale micro-nano column array can be assembled into a flexible micro-pressure sensor, and the specific method comprises the following steps:
firstly, magnetron sputtering is carried out on two prepared same integrated cross-scale micro-nano column arrays, and a layer of conductive metal material is sputtered on the surfaces of the micro-nano column arrays (firstly, 5nmCr and then 50nmAu are sputtered) and is used for electric signal transmission of the sensor.
Then, performing oxygen plasma hydrophilic treatment on the two integrated trans-scale micro-nano column arrays and the elastic layer (a polydimethylsiloxane film with the thickness of 250 μm), and bonding to form a three-layer structure which is sequentially an integrated trans-scale micro-nano column array 5, an elastic layer 6 and an integrated trans-scale micro-nano column array 5 from top to bottom, as shown in fig. 7, so as to obtain the flexible micro-pressure sensor. And the two micro-nano column arrays on the upper layer and the lower layer form an interlocking structure (the micro columns of the two arrays are alternately arranged, so that the interlocking structure is formed). The elastic layer is a rectangular frame with a hollow center and is positioned on the periphery of the two interlocked micro-nano column arrays.
Silver wires are fixed on the conductive metals on the surfaces of the two micro-nano column arrays respectively through conductive silver paste, and then a meter pen of the universal meter is connected onto the silver wires, so that the resistance change condition of the flexible micro-pressure sensor after being pressed can be measured.
In the embodiment, the thickness of the elastic layer is 250 μm which is exactly equal to the height of two layers of micro-nano columns, and the top ends of the elastic layer are exactly contacted under the condition of no stress, so that the micro pressure can be measured; if the elastic layer is smaller than 250 μm, the function of measuring micro pressure can be realized, but the space range of the upper and lower micro columns when in contact with each other is smaller than that of the elastic layer of 250 μm along with the increase of pressure, so that the measuring range of the sensor is reduced; if the thickness of the elastic layer is larger than 250 micrometers, the two layers of the micro-nano columns are not in contact when the sensor is not stressed, the sensor is not conducted, and the micro pressure cannot be detected. Therefore, the thickness of the elastic layer is designed to be the sum of the heights of the two layers of micro-nano columns, and the effect is optimal.
When pressure acts on the upper surface of the flexible micro-pressure sensor, the contact area between the micro-nanorod arrays can be changed. When the pressure is lower, the nano structures on the surface of the micro-nano column are contacted, and the micro pressure can be measured; the larger the pressure, the more the contact area, resulting in a smaller resistance value of the output. Fig. 8 shows the relative change of the resistance of the flexible micro-pressure sensor along with the change of the pressure, the minimum detection pressure of the flexible micro-pressure sensor can be as low as 15Pa, the detection range is 15 Pa-25 kPa, the sensitivity under a small pressure can reach 0.630/kPa, and the flexible micro-pressure sensor has very high force detection resolution, a wide linear range and high sensitivity.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A processing method of an integrated cross-scale micro-nano column array is characterized by comprising the following steps: firstly, processing a micropore array with nanometer pits on the inner wall on a polymer template with a flexible film attached to the surface by femtosecond laser; and then removing the flexible film on the polymer template, coating the liquid flexible material on the surface of the polymer template and diffusing the liquid flexible material into the micropore array, and curing and demolding to obtain the integrated cross-scale micro-nano column array.
2. The processing method of the integrated cross-scale micro-nanorod array according to claim 1, characterized by comprising the following steps:
step (1), a polymer template is tightly attached to the surface of a hard base material through an adhesive;
step (2), attaching the flexible film to the surface of the polymer template;
processing a polymer template attached with a flexible film by using femtosecond laser, and processing a micropore array with a nano pit on the inner wall of the micropore array;
step (4), removing the flexible film on the upper surface after the processing is finished, attaching the limiting frame to the periphery of the polymer template, coating the liquid flexible material in the limiting frame, and uniformly diffusing the liquid flexible material on the surface of the polymer template and in the micropore array;
and (5) drying and curing the liquid flexible material, and peeling the flexible material from the polymer template to obtain the integrated cross-scale micro-nano column array.
3. The processing method of the integrated cross-scale micro-nano column array according to claim 1 or 2, characterized in that: the polymer template is polytetrafluoroethylene, polyvinyl chloride or fluorinated ethylene propylene copolymer.
4. The processing method of the integrated cross-scale micro-nano column array according to claim 1 or 2, characterized in that: the flexible film is polydimethylsiloxane, polyimide, epoxy resin, polyurethane, polyethylene terephthalate, polyethylene naphthalate, polyvinyl alcohol, polyamide imide or polycarbonate.
5. The processing method of the integrated cross-scale micro-nano column array according to claim 1 or 2, characterized in that: the femtosecond laser processing power is 100-500mW, the central wavelength is 700-1000 nm, the pulse width is less than 120fs, the repetition frequency is 0.1-1000 KHz, the scanning speed is 10-100 mm/s, the laser scanning interval is 50-350 μm, and the scanning time of each micropore array is 100-300 ms.
6. The processing method of the integrated cross-scale micro-nano column array according to claim 1 or 2, characterized in that: the liquid flexible material is polydimethylsiloxane solution, Ecoflex or Dragon Skin.
7. An integrated trans-scale micro-nano column array obtained by the processing method of any one of claims 1 to 6, wherein the integrated trans-scale micro-nano column array is characterized in that: the integrated cross-scale micro-nano column array is composed of a substrate and a micro-nano column array, dendritic nano structures are distributed on the surface of a micro column, and the micro column and the dendritic nano structures are of an integrated structure without a layered interface.
8. The integrated trans-scale micro-nanorod array according to claim 7, wherein: the micron column is in a round table shape, the diameter of the bottom surface of the round table is 35-60 mu m, the diameter of the top surface of the round table is 15-30 mu m, the height of the round table is 120-200 mu m, and the density of the micron column is 1-3.24 x 108Per m2(ii) a The diameter of the dendritic nano structure is 800-950 nm; the thickness of the substrate is 100-500 μm.
9. A flexible micro-pressure sensor, characterized by: the integrated trans-scale micro-nano column array is formed by oppositely superposing two integrated trans-scale micro-nano column arrays according to claim 7 or 8, the two micro-nano column arrays form an interlocking structure, elastic layers are arranged on the peripheries of the two interlocked micro-nano column arrays, and the upper surface and the lower surface of each elastic layer are respectively attached to the substrates of the two micro-nano column arrays.
10. A method for manufacturing the flexible micro-pressure sensor of claim 9, wherein:
firstly, respectively carrying out magnetron sputtering on two identical integrated cross-scale micro-nano column arrays, and sputtering a layer of conductive metal material on the surfaces of the micro-nano column arrays; and then, carrying out oxygen plasma hydrophilic treatment on the two integrated cross-scale micro-nano column arrays and the elastic layer, and then bonding to form a three-layer structure of the cross-scale micro-nano column array, the elastic layer and the integrated cross-scale micro-nano column array which are sequentially integrated from top to bottom, wherein the two micro-nano column arrays on the upper layer and the lower layer form an interlocking structure, and the elastic layer is positioned on the periphery of the two interlocked micro-nano column arrays, so that the flexible micro-pressure sensor is obtained.
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