CN109987580B - Preparation method of nano forest structure and regulation and control method of nano forest structure - Google Patents
Preparation method of nano forest structure and regulation and control method of nano forest structure Download PDFInfo
- Publication number
- CN109987580B CN109987580B CN201910304292.0A CN201910304292A CN109987580B CN 109987580 B CN109987580 B CN 109987580B CN 201910304292 A CN201910304292 A CN 201910304292A CN 109987580 B CN109987580 B CN 109987580B
- Authority
- CN
- China
- Prior art keywords
- nano
- forest structure
- coupling agent
- mixture
- nano forest
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0061—Methods for manipulating nanostructures
-
- 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 provides a preparation method of a nano forest structure and a regulation and control method of the nano forest structure. The preparation method of the nano forest structure comprises the following steps: s1, forming a thin film layer on the substrate by adopting a mixture comprising a coupling agent and a polymer; and S2, carrying out plasma bombardment on the thin film layer to form a nano forest structure. The method is characterized in that a coupling agent is added on the basis of the polymer, in the plasma bombardment process, groups of the polymer and the coupling agent in a thin film layer are activated, organic groups and inorganic groups of the coupling agent are respectively connected with organic groups and inorganic groups of the polymer, and meanwhile, cross-linking occurs between the organic groups of the coupling agent, so that active groups generated by plasma bombardment are polymerized again, the original mixture layer disappears, and a nano forest structure is formed.
Description
Technical Field
The invention relates to the field of nanotechnology, in particular to a preparation method of a nano forest structure and a regulation and control method of the nano forest structure.
Background
The nano forest structure has special surface effects such as large surface-to-volume ratio and multiple pores, so that the nano forest structure is widely applied to devices such as biological detection and photoelectric detection, and the working performance, the preparation cost and the application range of the devices are directly influenced. The nano forest structure with simple preparation process and controllable characteristics and appearance can effectively improve the performance of integrated devices, reduce the preparation cost and widen the application range.
At present, various methods for preparing nano forest structures are reported, including electron beam exposure, nano bead etching and vls (vapor Liquid solid) chemical synthesis growth techniques, but these techniques still have great defects. The electron beam exposure technical method needs to depend on expensive equipment and belongs to serial processing, so that the preparation of a large-area nano forest structure becomes costly and time-consuming, and large-area popularization is difficult to realize; the nano-ball etching technology is combined with anisotropic etching to prepare nano forest structures in parallel, but the imaging of the nano-balls in single-layer arrangement needs strict control conditions, and large-area single-layer arrangement of the balls is difficult to realize, so that the process difficulty is increased, and the application of the technology in devices is limited. The VLS chemical synthesis technology belongs to a parallel preparation technology, has simple process steps, and can prepare a nano forest structure in a large area, but the direction and the size parameters of the nano forest structure prepared by the technology are difficult to control well, so that the characteristics of the nano forest structure are influenced, and in addition, the technology is difficult to be compatible with the conventional MEMS technology, so the application of the technology in devices is further limited.
Therefore, in view of comprehensive consideration of the aspects of nano forest structure characteristic regulation, processing cost, device integration application and the like, a process method for preparing a nano forest structure with controllable morphology and characteristics is urgently needed to be developed.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a nano forest structure and a regulation and control method of the nano forest structure, so as to provide a process method for preparing the nano forest structure with controllable appearance and characteristics.
In order to achieve the above object, according to an aspect of the present invention, there is provided a method for preparing a nano forest structure, comprising the steps of: s1, forming a thin film layer on the substrate by adopting a mixture comprising a coupling agent and a polymer; and S2, carrying out plasma bombardment on the thin film layer to form a nano forest structure.
Further, the above coupling agent is a silane coupling agent, and preferably the silane coupling agent includes any one or more of vinylsilane, aminosilane, epoxysilane, mercaptosilane, and methacryloxysilane.
Further, the above polymer includes any one or more of polyimide, polyethylene, polymethyl methacrylate, and polydimethylsiloxane.
Further, the mixture also comprises metal nanoparticles, the particle size of the metal nanoparticles is preferably 1-50 nm, and the metal nanoparticles comprise noble metal and/or copper.
Further, the mixture also comprises a photosensitive substance, and preferably, the photosensitive substance is ultraviolet photoresist or electron beam photoresist.
Further, step S1 further includes a step of diluting the mixture with a diluent, preferably the diluent includes any one or more of N-methylpyrrolidone, butyrolactone, and ethyl lactate, before the step of forming the thin film layer.
Further, in step S2, the plasma etching includes oxygen plasma bombardment, argon plasma bombardment, and alternating bombardment of oxygen plasma bombardment and argon plasma bombardment.
Further, after step S2, the preparation method further includes the steps of: and carrying out heat treatment, film coating treatment or acid-base modification treatment on the nano forest structure to modify the nano forest structure.
Further, the nano forest structure is selected from any one of a nano fiber forest structure, a nano cluster forest structure and a nano wrinkle structure.
According to another aspect of the invention, a method for regulating and controlling a nano forest structure is provided, which comprises the following steps: the preparation method of the nano forest structure is adopted, wherein the content of each component of the mixture in the step S1 of the preparation method is adjusted to obtain nano forest structures with different appearances; or the nano forest structure with different characteristics is obtained by adopting the preparation method of the nano forest structure.
The technical scheme of the invention provides a preparation method of a nano forest structure, which takes a coupling agent as an inducer, and adopts a plasma degumming process to prepare the nano forest structure after mixing polymers. The method comprises the following steps of bombarding a polymer layer by adopting plasma, enabling partial products generated by the polymer to be polymerized again to form a forest nano structure, adding a coupling agent on the basis of the polymer, activating groups of the polymer and the coupling agent in a thin film layer in the process of plasma bombardment, respectively connecting an organic group and an inorganic group of the coupling agent with an organic group and an inorganic group of the polymer, and simultaneously performing crosslinking action between the organic groups of the coupling agent, so that an active group generated by plasma bombardment is polymerized again, an original mixture layer disappears, and the nano forest structure is also formed; in addition, the preparation method can also adjust the content of the coupling agent, the polymer and other components in the mixture, so as to realize the regulation of the nano forest structure and the diversified regulation of the nano forest structure appearance; in addition, the preparation method disclosed by the invention is simple in process, can be used for parallel preparation, is strong in controllability, and is suitable for large-scale commercial production.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 is a schematic diagram illustrating a cross-sectional structure of a base after a substrate is provided in a method for preparing a nano forest structure provided by an embodiment of the present application;
FIG. 2 is a schematic cross-sectional view of a substrate after forming a thin film layer on the substrate shown in FIG. 1;
FIG. 3 is a schematic cross-sectional view of the substrate after plasma bombardment of the thin film layer shown in FIG. 2 to form the nanowire forest structure;
FIG. 4 is a schematic cross-sectional view of a nanofiber forest structure formed by plasma bombardment of a thin film layer in the method for preparing a nanofiber forest structure provided in example 1 of the present application;
FIG. 5 is a schematic cross-sectional view of another nanofiber forest structure formed by plasma bombardment of a thin film layer in the method for preparing a nano forest structure provided in example 1 of the present application;
FIG. 6 is a schematic cross-sectional view of a nanofiber forest structure formed by plasma bombardment of a thin film layer in the method for preparing a nanofiber forest structure provided in example 1 of the present application;
FIG. 7 is a schematic diagram showing a cross-sectional structure of a substrate coated with a silica film in a forest structure of nanofibers according to the method for preparing a forest structure of nanofibers provided in example 1 of the present application;
FIG. 8 is a schematic cross-sectional view of the substrate after the silica thin film of FIG. 11 has been externally modified with a bioactive layer
FIG. 9 is a schematic cross-sectional view of a nano forest structure formed by plasma bombardment on a thin film layer in the method for preparing a nano forest structure provided in example 1 of the present application;
FIG. 10 is a schematic cross-sectional view of a nano-forest structure formed by plasma bombardment on a thin film layer in the method for preparing a nano-forest structure provided in example 1 of the present application;
fig. 11 is a schematic diagram illustrating a cross-sectional structure of a substrate after a modified thin film layer containing nano-metal particles is formed on a substrate in a method for preparing a nano-forest structure according to an embodiment of the present disclosure;
FIG. 12 is a schematic cross-sectional view of the substrate after plasma bombardment of the thin film layer shown in FIG. 11 to form the nano-forest structure.
Wherein the figures include the following reference numerals:
101. a substrate; 102. a thin film layer; 103. a nanowire forest structure; 104. a nanofiber forest structure; 105. a silicon dioxide film; 106. a biologically active layer; 107. a nano-cluster forest structure; 108. nano-fold forest structures; 202. modifying the thin film layer; 203. and (5) modifying the nano forest structure.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the technical solutions of the present invention better understood, 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.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged under appropriate circumstances in order to facilitate the description of the embodiments of the invention herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
As introduced in the background art, in view of comprehensive consideration of the aspects of nano forest structure characteristic control, processing cost, device integration application and the like, a process method for preparing a nano forest structure with controllable morphology and characteristics is urgently needed to be developed. The inventor of the invention researches the problems and provides a preparation method of a nano forest structure, which comprises the following steps: s1, forming a thin film layer on the substrate by adopting a mixture comprising a coupling agent and a polymer; and S2, carrying out plasma bombardment on the thin film layer to form the nano forest structure.
The preparation method takes the coupling agent as the inducer, and adopts the plasma degumming process to prepare the nano forest structure after mixing the polymers. The method is characterized in that a coupling agent is added on the basis of the polymer, in the plasma bombardment process, groups of the polymer and the coupling agent in a thin film layer are activated, organic groups and inorganic groups of the coupling agent are respectively connected with organic groups and inorganic groups of the polymer, and meanwhile, cross-linking occurs between the organic groups of the coupling agent, so that active groups generated by plasma bombardment are polymerized again, the original mixture layer disappears, and a nano forest structure is formed.
In addition, the preparation method can also adjust the content of the coupling agent, the polymer and other components in the mixture, so as to realize the regulation of the nano forest structure morphology and realize the diversified regulation of the nano forest structure morphology; in addition, the preparation method disclosed by the invention is simple in process, can be used for parallel preparation, is strong in controllability, and is suitable for large-scale commercial production.
An exemplary embodiment of the method for producing a nano-forest structure according to the invention will be described in more detail below. These exemplary embodiments may, however, be embodied in many different forms and should not be construed as limited to only the embodiments set forth herein. It should be understood that these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of these exemplary embodiments to those skilled in the art.
First, step S1 is executed: a thin film layer is formed on a substrate using a mixture including a coupling agent and a polymer. The mixture may be provided on the surface of the substrate by a spin coating process and then subjected to a baking process to form the thin film layer, and the base sheet on which the mixture layer is formed may be placed on a hot plate and baked, or the mixture may be provided on the substrate by spraying, pasting, imprint-curing, or the like.
In step S1, the substrate may be a single crystal silicon wafer, such as a 4 inch, 6 inch, 8 inch, 12 inch wafer, or other substrate pieces of various shapes and sizes suitable for use in microfabrication processes. It should be noted that, besides monocrystalline silicon, the substrate may be a substrate commonly used in micromachining processes including polycrystalline silicon, amorphous silicon, glass, quartz, ceramics, and polymers.
In the above step S1, preferably, the coupling agent is a silane coupling agent, more preferably, the silane coupling agent includes any one or more of vinyl silane, amino silane, epoxy silane, mercapto silane, and methacryloxy silane; also, preferably, the compound includes polyimide, polyethylene, polymethyl methacrylate, and polydimethylsiloxane.
In a preferred embodiment, the mixture further comprises metal nanoparticles. By adding the metal nano particles, the regulated nano forest structure has the characteristics of the nano forest structure and the nano silver particles, and the respective small-size effect and the surface effect of the nano forest structure and the nano silver particles can influence each other, so that some special effects can be generated, and the nano forest structure can be used for improving the performance of a device and further expanding the application field of the device. More preferably, the particle size of the metal nanoparticles is 1 to 50 nm; more preferably, the metal nanoparticles include a noble metal and/or copper, and the noble metal may be gold and/or silver.
In a preferred embodiment, the mixture further comprises a photosensitive substance. Because the photosensitive material on the substrate can form a specific pattern after being processed by the patterning process, the patterned nano forest structure can be further prepared on the basis of the specific pattern. The photosensitive material may include uv photoresist, electron beam photoresist, and other special process photoresist, and those skilled in the art can reasonably select the kind of the photosensitive material according to the prior art.
In a preferred embodiment, the step S1 further includes a step of diluting the mixture with a diluent before the step of forming the thin film layer. The solid content and viscosity of the mixture are reduced by diluting the mixture, and the thin film layer prepared by the spin coating process at the same rotating speed is thinner due to the fact that the solid content and viscosity of the diluted mixture are lower, so that a nanofiber forest structure with lower height can be formed on the substrate after subsequent plasma bombardment.
In the preferred embodiment, the ratio of the diluent to the mixture is optionally 1:1 to 1:10, and more preferably, the diluent includes one or more of N-methylpyrrolidone, butyrolactone and ethyl lactate. But the above preferred species are not limited thereto, and those skilled in the art can select the above diluent species appropriately according to the prior art.
After step S1 is completed, step S2 is performed: and carrying out plasma bombardment on the thin film layer to form the nano forest structure.
The nano forest structure is formed by bombarding the mixture film layer by plasma, for example, forming a nano-wire forest structure under the bombardment of oxygen plasma, and further, bombarding the nano-wire forest structure by argon plasma to change the nano-wire forest structure into a stronger nano-fiber forest structure. In addition, the nano fiber forest structure, the nano cluster forest structure and the nano wrinkle forest structure with various morphologies can be obtained by changing the types of the coupling agent and the polymer in the mixture and the content of the coupling agent and the polymer.
The plasma bombardment process can be carried out by adopting plasma cleaning equipment in a semiconductor process, the type of the plasma can be any other plasma and mixed gas thereof capable of bombarding a mixture layer besides oxygen plasma and argon plasma, in the plasma bombardment process, a single gas source can be adopted for plasma bombardment, multiple gas sources can be adopted for alternative bombardment, the flow of the plasma source can be 20-400 sccm, the cavity pressure can be 2-40 Pa, the radio frequency power can be 50-400W, and the treatment time can be 2-120 min.
In the process of plasma bombardment, groups of a polymer and a coupling agent in the mixture layer are activated, then, an organic group and an inorganic group of a silane coupling agent are respectively connected with an organic group and an inorganic group of the polymer, and meanwhile, a crosslinking effect is generated between the organic groups of the coupling agent, so that an active group generated by plasma bombardment is polymerized again, the original mixture layer disappears, and a nano forest structure is formed. The diameter of each single nanofiber in the nanofiber forest structure is 20-200 nm, the height of each single nanofiber is about 1-6 mu m, and the distance between every two single nanofibers is about 50-300 nm.
In a preferred embodiment, after the above step S2, the preparation method further comprises the steps of: and carrying out heat treatment, film coating treatment or acid-base modification treatment on the nano forest structure to modify the nano forest structure. After the steps of heat treatment, film coating treatment or acid-base modification treatment and the like are carried out on the nano forest structure, the nano forest structure has stronger toughness and higher biocompatibility, and is expected to be widely applied to the field of biomedicine.
According to another aspect of the present invention, there is also provided a method for controlling a nano forest structure, comprising the steps of: the preparation method of the nano forest structure is adopted, wherein the content of each component of the mixture in the step S1 of the preparation method is adjusted to obtain the nano forest structures with different appearances; or carrying out heat treatment, film coating treatment or acid-base modification treatment on the nano forest structure to obtain nano forest structures with different characteristics.
The preparation of the nano forest structure according to the invention will be further illustrated with reference to the following examples.
Example 1
The preparation method of the nano forest structure provided by the embodiment is shown in fig. 1 to 3, and comprises the following steps:
providing a substrate 101, wherein the substrate 101 is a monocrystalline silicon wafer;
providing a mixture of a coupling agent and a polymer, wherein the coupling agent in the mixture adopts a coupling agent containing an epoxy group, the polymer adopts a polyimide photoresist, the ratio of the coupling agent to the polymer is 1:10, the mixing is carried out in a yellow light environment selected at normal temperature and normal pressure, the coupling agent and the photoresist are mixed and stirred for 10min by using a stirring rod, and the mixture is kept stand for 30 min;
spin-coating the mixture on a substrate 101 by a spin-coating method, wherein a low rotation speed of 750rpm is adopted in the process for 8s, a high rotation speed of 4000rpm is adopted for 25s to form a thin film layer with the thickness of 8 μm, and then the substrate 101 with the mixture spin-coated is placed on a hot plate to be baked at the baking temperature of 120 ℃ for 20min to form the thin film layer 102;
and bombarding the thin film layer 102 by adopting oxygen plasma, wherein the flow of oxygen in the oxygen plasma gas bombardment process is 50sccm, the cavity pressure is 5Pa, the time is 40min, the cavity power is kept at 200W in the whole bombardment process, after the mixture layer is completely removed, the nanowire forest structure 103 is formed on the area of the original mixture layer, the bottom of the formed nanowire forest structure 103 is relatively dispersed, and the structure height is about 5 microns.
Example 2
The difference between the preparation method of the nano forest structure provided in this example and example 1 is that:
the plasma gas source is argon, the flow of the argon in the bombardment process is 20sccm, the pressure of the cavity is 2Pa, the time is 60min, and the power of the cavity is kept at 200W in the whole bombardment process. After the bombardment process is finished, the bottom of the nano forest structure shrinks and gathers, and a relatively thick nano fiber forest structure 104 with a height of about 4 μm is formed, as shown in fig. 4.
Example 3
The difference between the preparation method of the nano forest structure provided in this example and example 1 is that:
after a mixture of a coupling agent and a polymer is provided, diluting the mixture by adopting N-methyl pyrrolidone, wherein the ratio of the N-methyl pyrrolidone to the mixture is 1:2 to obtain a mixture with lower solid content, and standing at normal temperature after dilution to regulate and control the height of a forest structure of the nanofiber;
the diluted mixture is adopted to form a thin film layer 102 on the substrate 101, and the thin film layer 102 prepared by the spin coating process at the same rotating speed is thinner and has the thickness of about 1 mu m because the solid content and the viscosity of the diluted mixture are reduced;
the thin film layer 102 is bombarded with oxygen plasma and argon plasma in sequence to form a forest of nanofibres 104 on the substrate 101, having a height of about 500 nm.
Example 4
The difference between the preparation method of the nano forest structure provided in this example and example 1 is that:
regulating and controlling the proportion of the coupling agent in the mixture to obtain a mixture with the volume percentage of the coupling agent being 1%;
oxygen plasma and argon plasma bombardment were sequentially used to form a forest structure 104 of nanofibers on the substrate 101 having a density different from that in example 2, as shown in fig. 5.
Example 5
The difference between the preparation method of the nano forest structure provided in this example and example 1 is that:
regulating and controlling the proportion of the coupling agent in the mixture to obtain a mixture with the coupling agent volume percentage of 20%;
oxygen plasma and argon plasma bombardment were sequentially used to form a forest structure 104 of nanofibers on the substrate 101 having a density different from that in examples 2 and 4, as shown in fig. 6.
It can be seen from examples 2 and 4-5 that the density of the nano forest structure is gradually increased with the increase of the proportion of the coupling agent, because the proportion of the coupling agent in the mixture is different, the central point of the mixture layer where the repolymerization can occur is increased with the increase of the proportion of the coupling agent, and therefore, the density of the nano forest structure formed by the mixture layer with the high content of the coupling agent is larger by the plasma bombardment.
Example 6
The difference between the preparation method of the nano forest structure provided in this example and example 1 is that:
in this example, the volume percentage of the coupling agent in the fixed mixture is 20%, and the coupling agent containing vinyl is mixed with the photoresist to obtain a mixture containing different types of coupling agents.
Example 7
The difference between the preparation method of the nano forest structure provided in this example and example 1 is that:
the volume percentage of the coupling agent in the mixture is 20%, and the coupling agent containing methacryloxy groups is mixed with the photoresist to obtain a mixture containing different types of coupling agents.
In the above examples 6 and 7, since the kinds of the coupling agents are different in the mixture, there are differences in the organic groups to be re-polymerized, and thus there are differences in the strength and form of the re-polymerization, so that there are differences in the diameter and height of the forest structure of nanofibers.
Example 8
The difference between the preparation method of the nano forest structure provided in this example and example 1 is that:
after the nanowire forest structure 103 is formed, the substrate 101 with the nano forest structure is placed on a hot plate with the temperature of 350 ℃ to be heated for 60min, polyamide resin in the nano forest structure is heated and converted into polyimide, the toughness of the nano forest structure can be effectively improved, an oven in a nitrogen environment can be selected for heating in the high-temperature heating process, the temperature is 350 ℃, and the time is 120 min;
forming a silicon dioxide film 105 with a thickness of 50nm on the nano forest structure by adopting a PECVD method, as shown in figure 7;
by means of H
2O
2：H
2SO
4Soaking the nano forest structure for 1 hour by using a solution with the ratio of 1:2, then placing the nano forest structure in deionized water for 5min by ultrasonic treatment, and hydroxylating the nano forest structure to form a bioactive layer 106 on the surface of the silicon dioxide film 105, as shown in fig. 8, so that the nano forest structure has higher biocompatibility.
Example 9
The difference between the preparation method of the nano forest structure provided in this example and example 1 is that:
in the embodiment, the volume percentage of the coupling agent in the fixed mixture is 20%, and a polyimide photoresist (type: AZ9920) is mixed with the coupling agent to obtain a mixture containing different polymers from the mixture of the embodiment 1;
bombardment with oxygen plasma and argon plasma in sequence is used to form nanocluster forest structures 107, as shown in fig. 9.
Example 10
The difference between the preparation method of the nano forest structure provided in this example and example 1 is that:
in the embodiment, the volume percentage of the coupling agent in the fixed mixture is 20%, a polyimide photoresist and the coupling agent are mixed, the solid content and the viscosity of the photoresist are greater than those of the photoresist in the embodiment 9, and a mixture containing different polymers from those in the embodiment 1 is obtained;
bombarding with oxygen plasma and argon plasma in sequence to form the nano-corrugated forest structure 108, as shown in fig. 10.
From examples 9-10 it can be seen that due to the different types of polymers in the mixture, there are differences in the organic groups which are re-polymerized with the coupling agent, and thus in the form and formation of re-polymerization, resulting in the formation of nanocluster forest structures and nano-corrugated forest structures, respectively.
Example 11
The difference between the preparation method of the nano forest structure provided in this example and example 1 is that:
in the embodiment, metal silver nanoparticles with the particle size of 20nm are added into the mixture;
forming the modified thin film layer 202 containing metallic silver nanoparticles on the substrate 101, as shown in fig. 11;
a modified nano-forest structure 203 with metallic silver nanoparticles is formed on the substrate 101 using a plasma bombardment process, as shown in fig. 12.
Because the nano forest structure contains the silver nano particles, the regulated nano forest structure has the characteristics of the nano forest structure and the nano silver particles, and the respective small-size effect and the surface effect of the nano forest structure and the nano silver particles can influence each other, so that some special effects can be generated, and the nano forest structure can be used for improving the performance of a device and further expanding the application field of the device.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
1. the technological method for preparing and regulating the nano forest structure based on the coupling agent can regulate and control the shape and the size of the nano forest structure, so that the regulation and control of the characteristics of the nano forest structure can be realized, and the performance of devices after the nano forest structure is integrated can be improved.
2. The technological method for preparing and regulating the nano forest structure based on the coupling agent can modify the nano forest structure by adding additional substances into the mixture and subsequent processes, and is favorable for regulating and controlling the characteristics of the nano forest structure to expand the application range of the nano forest structure.
3. The process method for preparing and regulating the nano forest structure based on the coupling agent has the advantages of low cost, simple and convenient process and strong controllability, and can realize commercial large-scale production.
4. The nano forest structure obtained by the process method based on the coupling agent preparation and the nano forest structure regulation and control has extremely high transmittance, has good optical characteristics when being prepared on a transparent substrate or transferred to a specific substrate, and can be widely applied to the fields of optical detection and the like.
5. The nano forest structure obtained by the process method based on the coupling agent preparation and the nano forest structure regulation has good moisture absorption property and super-hydrophilic property, and can be widely used in the fields of humidity detection, bacteria detection and the like.
6. The nano forest structure obtained by the process method based on the coupling agent preparation and the nano forest structure regulation can have super-hydrophobic characteristics after being transferred to a specific substrate, and can be widely applied to the fields of fog prevention, pollution prevention, corrosion prevention, oil stain resistance and the like.
7. The nano forest structure obtained by the process method based on the coupling agent preparation and the nano forest structure regulation can form a cone-shaped structure with the top characteristic, has the physical and chemical characteristics capable of effectively inhibiting the growth of bacteria, and can be widely applied to the fields of antibiosis and sterilization.
8. The nano forest structure obtained by the process method based on the coupling agent preparation and the nano forest structure regulation has the characteristics of large surface-to-body ratio and strong adsorption force, and can be widely used in the fields of biomolecule adsorption and the like.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (15)
1. A preparation method of a nano forest structure is characterized by comprising the following steps:
s1, forming a thin film layer on the substrate by adopting a mixture comprising a coupling agent and a polymer;
and S2, performing plasma bombardment on the thin film layer, wherein in the plasma bombardment process, the groups of the polymer and the coupling agent in the thin film layer are activated, and the active groups generated by the plasma bombardment are polymerized again to form the nano forest structure.
2. The production method according to claim 1, wherein the coupling agent is a silane coupling agent.
3. The production method according to claim 2, wherein the silane coupling agent includes any one or more of a vinyl silane, an amino silane, an epoxy silane, a mercapto silane, and a methacryloxy silane.
4. The method of claim 1, wherein the polymer comprises any one or more of polyimide, polyethylene, polymethyl methacrylate, and polydimethylsiloxane.
5. The method of any one of claims 1 to 4, wherein the mixture further comprises metal nanoparticles.
6. The method according to claim 5, wherein the metal nanoparticles have a particle size of 1 to 50 nm.
7. The production method according to claim 5, wherein the metal nanoparticles comprise a noble metal and/or copper.
8. The method according to any one of claims 1 to 3, wherein the mixture further comprises a photosensitive substance.
9. The method according to claim 8, wherein the photosensitive substance is an ultraviolet resist or an electron beam resist.
10. The production method according to any one of claims 1 to 4, wherein the step S1 further includes a step of diluting the mixture with a diluent before the step of forming the film layer.
11. The method of claim 10, wherein the diluent comprises any one or more of N-methylpyrrolidone, butyrolactone, and ethyl lactate.
12. The method according to any one of claims 1 to 4, characterized in that, in the step S2, the plasma etching includes oxygen plasma bombardment, argon plasma bombardment, and alternating bombardment of oxygen plasma bombardment and argon plasma bombardment.
13. The production method according to any one of claims 1 to 4, characterized in that, after the step S2, the production method further includes the steps of:
and carrying out heat treatment, film coating treatment or acid-base modification treatment on the nano forest structure to modify the nano forest structure.
14. The method of manufacturing as claimed in claim 1, wherein the nano forest structures are selected from any one of nano fiber forest structures, nano cluster forest structures and nano corrugated structures.
15. A method for regulating and controlling a nano forest structure is characterized by comprising the following steps:
a method of producing a nano-forest structure according to any one of claims 1 to 14, wherein the content of each component of the mixture in step S1 of the production method is adjusted to obtain different morphologies of the nano-forest structure; or using the method of manufacturing a nano forest structure according to claim 13, to obtain the nano forest structures of different characteristics.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910304292.0A CN109987580B (en) | 2019-04-16 | 2019-04-16 | Preparation method of nano forest structure and regulation and control method of nano forest structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910304292.0A CN109987580B (en) | 2019-04-16 | 2019-04-16 | Preparation method of nano forest structure and regulation and control method of nano forest structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109987580A CN109987580A (en) | 2019-07-09 |
| CN109987580B true CN109987580B (en) | 2020-02-11 |
Family
ID=67133836
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910304292.0A Active CN109987580B (en) | 2019-04-16 | 2019-04-16 | Preparation method of nano forest structure and regulation and control method of nano forest structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109987580B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110600376B (en) * | 2019-09-20 | 2022-04-08 | 上海华力微电子有限公司 | Polymer removal process |
| CN111607113B (en) * | 2020-05-29 | 2022-03-11 | 南京工业大学 | Preparation method of polymer nano forest structure film |
| CN111896121A (en) * | 2020-07-13 | 2020-11-06 | 无锡物联网创新中心有限公司 | MEMS thermopile infrared detector |
| CN112533468B (en) * | 2020-12-08 | 2021-11-30 | 江苏创芯海微科技有限公司 | Anti-reflection electromagnetic shielding structure and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1916034A (en) * | 2006-08-25 | 2007-02-21 | 南京大学 | Solidifiable composition material by ultraviolet light and application |
| CN102424356A (en) * | 2011-11-24 | 2012-04-25 | 宁波大学 | Device and method for preparing metal nanoparticle microarray chip |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10241708B4 (en) * | 2002-09-09 | 2005-09-29 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | A method of reducing the interfacial reflection of plastic substrates and such modified substrate and its use |
| US9347939B2 (en) * | 2012-05-23 | 2016-05-24 | University of Pittsburgh—of the Commonwealth System of Higher Education | Method for making polymer single nanowires and sensors utilizing the same |
| CN105084305B (en) * | 2015-06-17 | 2017-07-04 | 中国科学院微电子研究所 | A kind of nanostructured and preparation method thereof |
| CN107991768A (en) * | 2017-11-28 | 2018-05-04 | 中国科学院微电子研究所 | MEMS optics, light-absorption nano structure and preparation method thereof |
-
2019
- 2019-04-16 CN CN201910304292.0A patent/CN109987580B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1916034A (en) * | 2006-08-25 | 2007-02-21 | 南京大学 | Solidifiable composition material by ultraviolet light and application |
| CN102424356A (en) * | 2011-11-24 | 2012-04-25 | 宁波大学 | Device and method for preparing metal nanoparticle microarray chip |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109987580A (en) | 2019-07-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109987580B (en) | Preparation method of nano forest structure and regulation and control method of nano forest structure | |
| Wang et al. | A lotus-leaf-like SiO2 superhydrophobic bamboo surface based on soft lithography | |
| CN108424543B (en) | Preparation method of light transmittance adjustable force response type surface wrinkles | |
| US20080050564A1 (en) | Method of Forming a Nano-Structure and the Nano-Structure | |
| KR20100132637A (en) | A method for treating high hydrophobic surface of substrate | |
| CN108854571B (en) | Method for preparing separation membrane by ultrasonic atomization deposition method | |
| CN102795595A (en) | Preparation method of wrinkles by combining selected area ultraviolet ozonization and solvent swelling and application thereof | |
| KR20090044220A (en) | Conductive and superhydrophobic coatings, and its fabrication method | |
| Zhu et al. | A novel process to form a silica-like thin layer on polyethylene terephthalate film and its application for gas barrier | |
| CN104148266A (en) | Self-cleaning high polymer film or coating and preparation method thereof | |
| Liu et al. | Facile preparation of super-hydrophobic fabrics composed of fibres with microporous or microspherical coatings using the static breath figure method | |
| KR101291727B1 (en) | Method for manufacturing implint resin and implinting method | |
| US20080311337A1 (en) | Substrates coated with organosiloxane nanofibers, methods for their preparation, uses and reactions thereof | |
| Lee et al. | Fabrication of a Large‐Area Hierarchical Structure Array by Combining Replica Molding and Atmospheric Pressure Plasma Etching | |
| CN108179404A (en) | A kind of method that orderly metal nano hole array is constructed based on growth method | |
| CN105088538B (en) | A kind of preparation method of hydrophobin coating | |
| CN209513602U (en) | A kind of producing device of self-assembly structure | |
| KR20100092091A (en) | Method of fabricting a nano-structure | |
| JP2011192397A (en) | Substrate for forming transparent conductive film, substrate with transparent conductive film, and manufacturing method of transparent conductive film | |
| Ma et al. | Preparation of super-hydrophobic cotton fabric with crosslinkable fluoropolymer | |
| KR101207841B1 (en) | Method for fabrication of microparticles with superhydrophobic surface structures and coating them on substrates | |
| Cheng et al. | Large-scale and low-cost preparation of ordered honeycomb-patterned film by solvent evaporation-induced phase separation method | |
| CN110540372B (en) | Non-close-packed silicon dioxide ring nano array and preparation method thereof | |
| CN109012221A (en) | Utilize magnetron sputtering SiO2Nanoparticle prepares the method and products thereof of high-hydrophilic PVDF filter membrane | |
| CN108264016A (en) | A kind of diverse nano structure composite array and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |