Methods for protecting micro / nano structures and methods for preparing protective layer solutions

Abstract

This invention discloses a method for protecting micro / nanostructures. A protective layer solution is applied to the object to be protected. After the solution dries, a protective layer forms on the object. The protective layer solution is prepared by dissolving various soluble organic materials in water. The solution is not limited to, but includes, solutions made by mixing polyethylene glycol, polyacrylamide, sodium carboxymethyl cellulose, polyvinylpyrrolidone, and soluble starch in water at specific mass ratios. This invention provides protection for fragile micro / nanostructure materials, making them less susceptible to structural damage and performance degradation during transportation, storage, and installation. Furthermore, the protective layer is easily removable without affecting the performance of the micro / nanostructure material.

Description

Technical Field

[0001] This invention relates to the field of micro / nano structures and manufacturing, and in particular to a method for protecting micro / nano structures and a method for preparing a protective layer solution. Background Technology

[0002] With the development of nanotechnology, materials with micro / nano structures have exhibited many unique properties, and their applications in various fields are rapidly expanding. Micro / nano structured materials have wide applications in optical manipulation, light-absorbing materials, mechanical structures, superhydrophobicity, and other fields, occupying a leading position in these areas and at the forefront of the industry. However, due to their size, material, and structural characteristics, micro / nano structures are generally fragile and easily contaminated. Their structure is easily damaged during production, transportation, storage, and use, thus affecting the performance of micro / nano structured materials. Therefore, protection of micro / nano structures is necessary. Protection technologies for micro / nano structures are of great significance for expanding their application scenarios, increasing efficiency, and extending their service life. Currently, the protection of micro / nano structured materials is a key focus of attention in the development of micro / nano structured materials.

[0003] Superblack materials, as important light-absorbing materials, play a crucial role in light energy conversion, stray light suppression, blackbody calibration, laser stealth, and infrared shielding. However, high-performance superblack materials often possess fragile micro / nanostructures, which are easily damaged during production, transportation, storage, and use. Micro / nanostructures fabricated on the surface of core-pore membranes exhibit excellent optical properties, achieving high absorption in the ultraviolet to terahertz bands. However, these micro / nanostructures on polymer substrates also suffer from the fragility inherent in micro / nanostructures, thus requiring protection. Protective materials can safeguard various micro / nanostructures, and core-pore membrane materials with micro / nanostructures are just one example of such protection.

[0004] There are few existing protection schemes for micro / nanostructures on light-absorbing materials. Current protection methods are complex to fabricate, inefficient, and cannot be mass-produced. Furthermore, they may damage parts of the original micro / nanostructure, resulting in a loss of performance. For example, patent 202210585422.4 attempts to protect the micro / nanostructure by fabricating a grating structure higher than the height of the micro / nanostructure on the substrate. However, this scheme is costly to fabricate and cannot achieve large-area protection. This scheme reduces the proportion of the light-absorbing area of ​​the micro / nanostructure by fabricating the grating on the substrate, as the grating area occupies the original micro / nanostructure area. The grating structure also adds an extra reflective surface, reducing the material's performance.

[0005] In summary, existing solutions cannot provide non-destructive and effective protection for fragile micro / nanostructured materials, thereby damaging their unique properties during transportation and application, and are not feasible for large-scale fabrication. Summary of the Invention

[0006] This invention provides a method for protecting micro- and nanostructures, which solves the problems of existing technologies being unable to provide non-destructive and effective protection for fragile micro- and nanostructure materials and being unable to fabricate them on a large scale.

[0007] To address the aforementioned technical problems, the present invention provides a method for protecting micro / nano structures.

[0008] A pre-prepared protective layer solution is applied to the surface of the micro / nano structure to be protected.

[0009] After the protective layer solution applied to the surface of the protected micro / nano structure dries, the protective layer solution forms a protective layer on the protected micro / nano structure.

[0010] The protective layer solution is prepared from soluble organic materials.

[0011] Optionally, the protective layer solution includes, but is not limited to, at least two polyethylene glycols with different molecular weights.

[0012] Optionally, the protective layer solution comprises 10%-20% polyethylene glycol 400, 10%-20% polyethylene glycol 600, 10%-20% polyethylene glycol 1000, and 60-80% polyethylene glycol 2000.

[0013] Optionally, the protective layer solution may further include 0%-10% polyethylene glycol 3000.

[0014] Optionally, the protective layer solution may further include 0%-5% polyacrylamide.

[0015] Optionally, the protective layer solution may further include 0%-5% sodium carboxymethyl cellulose.

[0016] Optionally, the protective layer solution may further include 0%-5% polyvinylpyrrolidone.

[0017] Optionally, the protective layer solution may further include 0%-5% soluble starch.

[0018] Optionally, the protective layer solution is applied to the surface of the protected micro / nano structure by spraying.

[0019] Optionally, the step of applying the protective layer solution to the surface of the protected micro / nanostructure includes:

[0020] S1. Atomize the protective layer solution using an atomizing gun and apply the protective layer solution to the object to be protected by spraying.

[0021] S2. After the protective layer solution applied to the object has dried, apply the atomized protective layer solution to the object again;

[0022] S3. Repeat steps S1-S2 until the thickness of the formed protective layer reaches the predetermined thickness.

[0023] Optionally, in step S3, the thickness of the protective layer is greater than the vertical dimension of the micro / nano structure of the protected object.

[0024] Optionally, the micro / nanostructure is a gold nanocone surface micro / nanostructure.

[0025] Optionally, the micro / nano structure is a micro / nano structure on the surface of a nuclear pore membrane.

[0026] The present invention also provides a method for preparing a protective layer solution for micro / nano structures, wherein the protective layer solution is prepared from at least two polyethylene glycols of different molecular weights.

[0027] Optionally, the protective layer solution comprises at least 10%-20% polyethylene glycol 400, 10%-20% polyethylene glycol 600, 10%-20% polyethylene glycol 1000, and 60-80% polyethylene glycol 2000.

[0028] The beneficial effects of the present invention are as follows: The water-soluble micro-nano structure protective layer of the present invention can provide protection for fragile micro-nano structure materials. The protective layer material completely fills and covers the microstructure on the surface of the nuclear pore membrane, has a flat surface, and has a certain mechanical strength. It can protect the microstructure, making it less likely that the fragile micro-nano structure materials will have their structural characteristics damaged during transportation, storage, installation and other operations, thereby damaging their performance.

[0029] Another technical advantage of this invention is that the protective layer is easy to remove and leaves no residue, which ensures that the properties of materials with micro-nano structures are not affected by residues, thus achieving non-destructive and effective protection for micro-nano structure materials.

[0030] Another technical advantage of this invention is that it can achieve large-area protection, the implementation method is simple and easy to operate, the cost is low, the application is convenient, the production is simple, and it is easy to prepare on a large scale. Attached Figure Description

[0031] Figure 1 This is a schematic diagram of the protective layer and the protected micro / nano structure described in this invention;

[0032] Figure 2 These are photographs of the nuclear pore membrane with micro-nano structure before protection, during protection, and after the protective layer is removed, as shown in the embodiments of the present invention.

[0033] Figure 3 These are electron microscope (EM) images of the surface of a nuclear pore membrane with micro-nano structures before, during, and after the protective layer is removed in an example of the present invention. The EEM images were taken with the sample stage tilted at 30°.

[0034] Figure 4 This refers to the reflectance of the nuclear pore membrane before and after the protective layer is removed in the examples of this invention.

[0035] Figure 5 These are photographs of the unprotected nuclear pore membrane in an example of the present invention before, during, and after being touched.

[0036] Figure 6 The images shown are electron microscope (EM) images of the unprotected nuclear pore membrane of this invention before and after being touched. The EEM images were taken with the sample stage tilted at 30°.

[0037] Figure 7 The reflectance of the unprotected nuclear pore membrane in this invention example is the reflectance of the nuclear pore membrane before and after pressing.

[0038] The labels in the diagram mean: 1. Micro / nano structure; 2. Protective layer.

[0039] The accompanying drawings are for illustrative purposes only and should not be construed as limiting the scope of this patent. To better illustrate this embodiment, some components in the drawings may be omitted, enlarged, or reduced, and do not represent the actual dimensions of the product. It is understandable to those skilled in the art that some well-known structures and their descriptions may be omitted in the drawings. The same or similar reference numerals correspond to the same or similar components. The terms describing positional relationships in the drawings are for illustrative purposes only and should not be construed as limiting the scope of this patent. Detailed Implementation

[0040] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.

[0041] like Figure 1 As shown in the schematic diagram, this invention illustrates the protection of a conical micro / nanostructure material, including a micro / nanostructure 1 and a protective layer 2. This invention is universally applicable and can be used for the protection of various micro / nanostructure materials. Therefore, the schematic diagram in this application should not be considered as being limited to the protection of materials with this specific structure. The embodiments described in this specification are merely one embodiment of the invention, intended to further illustrate the content of the invention, and should not be considered as limiting the specific scope of the invention. Based on the embodiments described in this specification, other embodiments obtained by those skilled in the art without inventive effort should all fall within the scope of this invention.

[0042] Example 1:

[0043] This embodiment discloses a method for preparing a micro / nano structure protective layer solution, as detailed below:

[0044] The protective layer solution is prepared by dissolving various soluble organic materials in water, including polyethylene glycol 400 (15%), polyethylene glycol 600 (15%), polyethylene glycol 1000 (15%), polyethylene glycol 2000 (70%), polyethylene glycol 3000 (5%), polyacrylamide (2.5%), sodium carboxymethyl cellulose (2.5%), polyvinylpyrrolidone (2.5%), and soluble starch (2.5%), which are mixed and dissolved in water to form the protective solution.

[0045] Example 2:

[0046] This embodiment discloses a method for preparing a micro / nano structure protective layer, as detailed below:

[0047] The protective layer solution prepared according to the method in Example 1 was applied to the surface of the nuclear pore membrane using an atomized spraying method to cover its surface micro-nano structures. The number of spraying times was determined based on the actual size of the micro-nano structures on the nuclear pore membrane surface. After each spraying, the sample was placed horizontally and allowed to air dry or placed on a heated platform to dry. The dried protective layer has a cell-like structure, a relatively flat surface, is flexible and bendable, and has a dense structure layer in its microstructure. The protective layer material completely fills and covers the microstructure on the surface of the nuclear pore membrane, has a flat surface, and possesses a certain mechanical strength, thus effectively protecting the microstructure.

[0048] Example 3:

[0049] This embodiment discloses a method for protecting the micro / nano structures on the surface of nuclear pore membranes, as detailed below:

[0050] First, a protective layer solution was prepared. This solution was made by dissolving various soluble organic materials in water. Specifically, polyethylene glycol 400 (10%), polyethylene glycol 600 (10%), polyethylene glycol 1000 (10%), and polyethylene glycol 2000 (60%) were mixed and dissolved in water to form the protective solution. In this example, a nuclear pore membrane sample with an area of ​​4 square centimeters was used. Its micro / nano structure was a cone-shaped structure with a length of approximately 30 μm. The sample was sprayed 8 times, with each spray lasting 5 seconds and an interval of 25 minutes between sprays. After each spraying, the sample was placed horizontally on a heated platform to air dry at a temperature of 35 degrees Celsius.

[0051] The micro-nanostructures on the surface of nuclear pore membranes are relatively fragile and easily contaminated. Their structure can be easily damaged during production, transportation, storage, and use, thus affecting the performance of the micro-nanostructured materials. In practical use, compressed air is used to blow away dust and other contaminants from the surface of the nuclear pore membrane. During application, the surface is touched and pressed, which can damage the micro-nanostructures and affect its performance. Before protection, scanning electron microscopy (SEM) images and reflectance measurements are performed. After protection, the nuclear pore membrane is subjected to compressed air blowing, touching, and pressing operations. After these operations, the membrane with the protective layer applied is immersed in water for 5 minutes to completely dissolve the protective layer material. Then, the membrane is placed in another cup of clean water to wash away all the protective layer material. SEM images and hemispherical reflectance measurements are then performed on the nuclear pore membrane after the protective layer material has been washed away.

[0052] like Figure 2 As shown, photographs of the nuclear pore membrane before protection, during protection, and after the above operations and cleaning off the protective layer were taken. It can be seen that the surface of the nuclear pore membrane during protection is covered with a thick protective layer material, and there is no difference between the nuclear pore membrane before and after protection.

[0053] like Figure 3 As shown, electron micrographs of the nuclear pore membrane were taken before protection, during protection, and after the above operations were performed and the protective layer was washed off. It can be seen that the surface of the nuclear pore membrane during protection is covered with a protective layer material, and the micro-nano structure on the surface of the nuclear pore membrane after protection is not bent or damaged.

[0054] like Figure 4 As shown, the reflectance of the nuclear pore membrane before protection and after the above operation and cleaning were measured using a Lambda 1050+ UV-Vis spectrophotometer. It can be seen that there is no difference in the reflectance of the nuclear pore membrane before protection and after pressing and cleaning.

[0055] In addition, the same operation was performed on nuclear pore membranes without a protective layer, serving as a control group.

[0056] like Figure 5 As shown, after undergoing compressed air purging, touching, and pressing operations, the pressed area of ​​the control group sample turned white.

[0057] like Figure 6 As shown, the micro-nano structures on the surface of the nuclear pore membrane bend and collapse after being pressed, and the unique micro-nano structures are damaged by external forces.

[0058] like Figure 7As shown, the reflectance of the nuclear pore membrane before and after the aforementioned operations and cleaning of the protective layer were measured using a Lambda 1050+ UV-Vis spectrophotometer. The reflectance of the unprotected nuclear pore membrane significantly decreased after being subjected to compressed air purging, touching, and pressing. This indicates that the protective layer effectively protected the nuclear pore membrane, ensuring that the micro / nano structure was not damaged by external forces and that the reflectance performance was not compromised. Furthermore, the absence of protective layer material residue after cleaning does not affect the performance of the micro / nano structure material.

[0059] Example 4:

[0060] This embodiment discloses a method for protecting the micro / nanostructures on the surface of gold nanocones, as detailed below:

[0061] First, a protective layer solution was prepared. This solution was made by dissolving various soluble organic materials in water. Specifically, polyethylene glycol 400 (20%), polyethylene glycol 600 (20%), polyethylene glycol 1000 (20%), polyethylene glycol 2000 (80%), polyethylene glycol 3000 (10%), polyacrylamide (5%), sodium carboxymethyl cellulose (5%), polyvinylpyrrolidone (5%), and soluble starch (5%) were mixed and dissolved in water to form the protective solution. In this example, a circular gold nanocone array sample with a diameter of 8 mm was used. Its micro / nano structure was a cone-shaped structure with a length of approximately 30 μm. The sample was sprayed 10 times, with each spraying lasting 5 seconds and an interval of 30 minutes between sprayings. After each spraying, the sample was placed horizontally and allowed to air dry.

[0062] Gold nanocone arrays are broadband absorbers, but their surface microstructures are fragile and easily contaminated. During production, transportation, storage, and use, their structure can be easily damaged, affecting the performance of the microstructured materials. In practical applications, compressed air is used to blow away dust and other contaminants from the gold nanocone array surface. Touching and pressing on the surface during operation can also damage the microstructure, affecting its performance. Before protection, scanning electron microscopy (SEM) imaging and reflectance measurements were performed. The protected core-pore membrane was then subjected to compressed air blowing, touching, and pressing operations. After these operations, the gold nanocone array sample with the protective layer applied was immersed in water for 5 minutes to completely dissolve the protective layer material. The core-pore membrane was then rinsed in another cup of clean water to remove all the protective layer material. The absorbance of the gold nanocone array sample remained unchanged before and after protection, indicating that the protective layer effectively protected the gold nanocone array, preventing damage to the microstructure from external forces and maintaining its absorbance performance. Furthermore, no protective layer material residue remained after cleaning, ensuring no impact on the microstructure material's performance.

[0063] Numerous specific details are set forth in the specification provided herein. However, it will be understood that embodiments of the invention may be practiced without these specific details. Similarly, for the sake of brevity and to aid in understanding one or more aspects of the invention, in the description of exemplary embodiments of the invention above, various features of the embodiments are sometimes grouped together in a single embodiment, figure, or description thereof. The claims, which follow the detailed description, are hereby expressly incorporated into that detailed description, wherein each claim itself is a separate embodiment of the invention.

[0064] It should be noted that the above embodiments are illustrative of the invention and not restrictive, and those skilled in the art can devise alternative embodiments without departing from the scope of the appended claims. In the claims, any reference signs placed between parentheses should not be construed as limiting the claims. Clearly, the above embodiments of the invention are merely examples for clearly illustrating the invention and are not intended to limit the implementation of the invention. Those skilled in the art can make other variations or modifications based on the above description. It is neither necessary nor possible to exhaustively describe all embodiments here. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the invention should be included within the scope of protection of the claims of this invention.

Claims

1. A method for protecting micro / nano structures, characterized in that: A pre-prepared protective layer solution is applied to the surface of the micro / nano structure to be protected. After the protective layer solution applied to the surface of the protected micro / nano structure dries, the protective layer solution forms a protective layer on the protected micro / nano structure. The protective layer solution is prepared from soluble organic materials; The protective layer solution includes, but is not limited to, at least two types of polyethylene glycol with different molecular weights; The protective layer solution comprises 10%-20% polyethylene glycol 400, 10%-20% polyethylene glycol 600, 10%-20% polyethylene glycol 1000, and 60-70% polyethylene glycol 2000.

2. The method for protecting micro / nano structures according to claim 1, characterized in that: The protective layer solution also includes 0%-10% polyethylene glycol 3000.

3. The method for protecting micro / nano structures according to claim 1, characterized in that: The protective layer solution also includes 0%-5% polyacrylamide.

4. The method for protecting micro / nano structures according to claim 1, characterized in that: The protective layer solution also includes 0%-5% sodium carboxymethyl cellulose.

5. The method for protecting micro / nano structures according to claim 1, characterized in that: The protective layer solution also includes 0%-5% polyvinylpyrrolidone.

6. The method for protecting micro / nano structures according to claim 1, characterized in that: The protective layer solution also includes 0%-5% soluble starch.

7. The method for protecting micro / nano structures according to claim 1, characterized in that: The protective layer solution is applied to the surface of the protected micro / nano structure by spraying.

8. The method for protecting micro / nano structures according to any one of claims 1-7, characterized in that, The step of applying the protective layer solution to the surface of the protected micro / nano structure includes: S1. The protective layer solution is atomized using an atomizing gun and applied to the surface of the micro / nano structure to be protected by spraying. S2. After the protective layer solution applied to the object dries, apply the atomized protective layer solution again to the surface of the protected micro / nano structure; S3. Repeat steps S1-S2 until the thickness of the formed protective layer reaches the predetermined thickness.

9. The method for protecting micro / nano structures according to claim 8, characterized in that: In step S3, the thickness of the protective layer is greater than the vertical dimension of the micro / nano structure of the protected object.

10. The method for protecting micro / nano structures according to claim 8, characterized in that: The micro / nano structure is a gold nanocone surface micro / nano structure.

11. The method for protecting micro / nano structures according to claim 8, characterized in that: The micro / nano structure is a micro / nano structure on the surface of a nuclear pore membrane.

12. A method for preparing a protective layer solution for micro / nano structures, characterized in that: The protective layer solution is prepared from at least two polyethylene glycols with different molecular weights, and the protective layer solution includes at least 10%-20% polyethylene glycol 400, 10%-20% polyethylene glycol 600, 10%-20% polyethylene glycol 1000, and 60-70% polyethylene glycol 2000.

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