CN116177596B - A method for preparing a randomly dispersed microsphere template on a solid substrate surface and its application - Google Patents
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Abstract
本发明提供了一种在固体基材表面制备无序分散微球模板的方法及应用，该方法包括：将尺寸不同的大尺寸微球和小尺寸微球混合均匀；通过自组装技术在固体基材表面构建得到单层微球薄膜；利用刻蚀技术去除所述小尺寸微球，从而在固体基材表面得到均匀分散且无序排列的大尺寸微球模板；模板的密度可以通过改变大、小尺寸微球的混合比例来进行调控。解决了在固体基材表面构建密度可控且无序分散的微球模板这一技术难题。且由于本发明所述方法基于自组装技术，所以能够低成本、大面积、高效地在固体基材表面制备微球模板，工艺过程简单且成本低廉，适用于批量及工业化生产。
The present invention provides a method and application for preparing a disorderly dispersed microsphere template on the surface of a solid substrate, the method comprising: uniformly mixing large-sized microspheres and small-sized microspheres of different sizes; constructing a single-layer microsphere film on the surface of a solid substrate by self-assembly technology; removing the small-sized microspheres by etching technology, thereby obtaining a uniformly dispersed and disorderly arranged large-sized microsphere template on the surface of a solid substrate; the density of the template can be regulated by changing the mixing ratio of large-sized and small-sized microspheres. The technical problem of constructing a density-controllable and disorderly dispersed microsphere template on the surface of a solid substrate is solved. And because the method of the present invention is based on self-assembly technology, it is possible to prepare a microsphere template on the surface of a solid substrate at low cost, large area, and high efficiency, the process is simple and low cost, and is suitable for batch and industrial production.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a method for preparing an unordered dispersion microsphere template on the surface of a solid substrate and application thereof.
Background
The microstructure constructed on the surface of the solid substrate can endow the material with special functional characteristics, so that the method has wide application prospects in the fields of biomedical materials, chemical sensing, surface enhanced Raman scattering, super-hydrophilic/super-hydrophobic surfaces, catalysis and the like. For example, in the biomedical material field, different micro-or nano-structures on the surface of the material can activate intracellular mechanical signal transduction pathways and initiate intracellular signaling cascades, thereby changing the phenotype and function of the cells and further endowing the medical material with certain unique biological functions. Compared with chemical methods such as grafting chemical molecules, the material surface physical morphology modification method has the characteristics of high safety, long persistence, small side effect on tissues and the like. Studies have shown that the construction of cellular titanium dioxide microporous structures on metallic titanium surfaces can regulate macrophage polarization behavior and promote the osteointegrative properties of titanium [ Zhuetal, SCIENCEADVANCES2021;7: eabf6654]. In the field of industrial photocatalysis, the honeycomb-shaped micropore structure on the surface of the solid catalytic material can greatly improve the photocatalysis performance due to larger specific surface area and reactive sites.
Although advanced processing techniques such as imprinting, lithography, focused ion beam etching, electron beam etching, etc. can be used to process microstructures on the surface of solid substrates with high precision, the wide application of these processing techniques is severely limited in terms of processing area, processing efficiency, processing cost, substrate selectivity, etc. The microsphere array is constructed on the surface of the solid substrate to be used as a template for subsequent treatment, so that the method is the simplest and most effective method for constructing microstructures with different morphologies. And if the microspheres can spontaneously form different structures in a self-assembly mode, the construction cost of the surface microstructure of the solid substrate can be further greatly reduced. Therefore, the preparation of self-assembled microsphere templates on the surface of solid substrates is a key to the construction of structures of different morphologies. Under proper assembly conditions, the microspheres are self-assembled into a layer of closely arranged monolayer microsphere film under the influence of gravity, capillary force, van der Waals force, electrostatic force and the like. At present, the method for preparing the ordered microsphere templates closely arranged on the surface of the solid substrate is mature, but the method for preparing the microsphere templates dispersed and unordered is rarely reported. Therefore, how to prepare a disordered microsphere template with controllable density and uniform dispersion on the surface of a solid substrate is a current technical problem.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for preparing an unordered dispersion microsphere template on the surface of a solid substrate and application thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the first aspect of the present invention provides a method for preparing an unordered dispersion microsphere template on a surface of a solid substrate, the method comprising uniformly mixing large-sized microspheres and small-sized microspheres having different sizes; and removing the small-size microspheres by using an etching technology, thereby obtaining the uniformly dispersed large-size microsphere templates with controllable density and disordered arrangement on the surface of the solid substrate. In the method provided by the invention, in the monolayer microsphere film constructed by the self-assembly technology, the small-size microspheres are closely arranged and the large-size microspheres are randomly separated, so that the large-size microspheres are distributed and disordered on the surface of the solid substrate.
Further, the step of constructing the single-layer microsphere film on the surface of the solid substrate by the self-assembly technology comprises the step of directly carrying out self-assembly on the large-size microsphere and the small-size microsphere on the surface of the solid substrate to obtain the single-layer microsphere film on the surface of the solid substrate.
The step of constructing the single-layer microsphere film on the surface of the solid substrate by the self-assembly technology comprises the steps of firstly carrying out self-assembly on the large-size microsphere and the small-size microsphere on the surface of a solution, and then transferring the single-layer microsphere film to the surface of the solid substrate to obtain the single-layer microsphere film on the surface of the solid substrate.
Further, the step of uniformly mixing the large-size microspheres and the small-size microspheres with different sizes comprises the step of controlling the separation distance of the large-size microspheres in the single-layer microsphere film by controlling the mixing proportion of the large-size microspheres and the small-size microspheres. I.e. the density of the large-size microspheres is controllable. For example, in the case where the amount of the large-sized microspheres added is not changed, the larger the small-sized microspheres are added, the larger the large-sized microspheres are separated by a larger distance.
Further, the self-assembly technology is one or more of a dip coating method, a spin coating method, an electric field assisted self-assembly method, an evaporation induced self-assembly method and an inclined plane induced self-assembly transfer method.
Further, the etching technique is plasma etching, electron beam etching or focused ion beam etching.
Further, the diameter of the large-size microsphere is 1-10 μm, and the diameter of the small-size microsphere is 0.1-2 μm. The diameter sizes of the large-size microspheres and the small-size microspheres can be overlapped in the value range, but the size difference between the large-size microspheres and the small-size microspheres needs to be pulled apart as much as possible in the selection process.
The second aspect of the invention provides a large-size microsphere template with uniformly dispersed, controllable density and disordered arrangement on the surface of a solid substrate, which is prepared by the method for preparing the disordered dispersed microsphere template on the surface of the solid substrate.
The third aspect of the invention provides application of the uniformly dispersed, density-controllable and disordered large-size microsphere template on the surface of a solid substrate in the field of surface modification of biomedical materials and the field of research on influence of porous microstructures with different densities on cell or bacterial behaviors and functions.
Compared with the prior art, the technical scheme provided by the invention has at least the following advantages:
1. The method solves the technical problem of constructing the microsphere template with controllable density and unordered dispersion on the surface of the solid substrate;
2. Because the method is based on the self-assembly technology, the microsphere template can be prepared on the surface of the solid substrate with low cost, large area and high efficiency;
3. the method can simply and conveniently regulate and control the density of the microsphere template;
4. the technology used in the method is a common technology which is already mature and applied, the process is simple, the cost is low, and the method is suitable for batch and industrialized production.
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One or more embodiments are illustrated by way of example and not limitation in the figures of the accompanying drawings, which are not to be construed as limiting the embodiments unless specifically indicated otherwise.
FIG. 1a is an optical microscope photograph of a microsphere thin film (Ti 100) on the surface of a titanium sheet prepared by using a microsphere mixed solution in which the proportion of 2 μm microspheres is 100% in example 2;
FIG. 1b is an optical microscope photograph of a microsphere thin film (Ti 80) on the surface of a titanium sheet prepared by using a microsphere mixed solution in which the proportion of 2 μm microspheres is 80% in example 2;
FIG. 1c is an optical microscope photograph of a microsphere thin film (Ti 50) on the surface of a titanium sheet prepared by using a microsphere mixed solution in which the proportion of 2 μm microspheres is 50% in example 2;
FIG. 1d is an optical microscope photograph of a microsphere thin film (Ti 20) on the surface of a titanium sheet prepared by using a microsphere mixed solution in which 2 μm microspheres account for 20% in example 2;
FIG. 2a is a scanning electron microscope image of a Ti20 sample of example 3 prior to plasma etching treatment;
FIG. 2b is a scanning electron microscope image of the Ti20 sample of example 3 after plasma etching treatment;
FIG. 3a is a scanning electron microscope picture of the Ti100S sample of example 5, taken at low magnification on the left and at high magnification on the right;
FIG. 3b is a scanning electron microscope picture of the Ti80S sample of example 5, taken at low magnification on the left and at high magnification on the right;
FIG. 3c is a scanning electron microscope picture of the Ti50S sample of example 5, taken at low magnification on the left and at high magnification on the right;
FIG. 3d is a scanning electron microscope picture of the Ti20S sample of example 5, taken at low magnification on the left and at high magnification on the right;
FIG. 4 is a schematic illustration of closely ordered monolayer close-packed microspheres formed by self-assembly on a solid substrate surface;
FIG. 5 is a graph showing that after decreasing the density of microspheres, the microspheres still tend to partially aggregate together rather than uniformly disperse on the surface of a solid substrate;
FIG. 6 is a flow chart of a method for preparing an unordered dispersion microsphere template on the surface of a solid substrate.
Detailed Description
The inventor finds that the key point of the preparation of the microstructure on the surface of the solid substrate is the design and construction of templates, and most of the preparation of microstructures at present takes self-assembled microspheres as templates. Therefore, parameters such as the assembly method and the order degree of the microsphere are key factors for determining the morphology and the order degree of the obtained microstructure. The technology for assembling the two-dimensional monolayer microspheres on the surface of the solid substrate comprises dip coating, spin coating, electric field assisted self-assembly, evaporation induced self-assembly, inclined plane induced self-assembly transfer and the like. By using the techniques, a close-packed microsphere template of a close-ordered monolayer can be prepared on the surface of a solid substrate, as shown in FIG. 4. However, it is difficult to obtain the desired effect when one wants to prepare a uniformly dispersed, density-controllable, disordered array of monolayer microsphere templates using these techniques. Because when the density of the microspheres is reduced in order to have the microspheres randomly dispersed on the surface of the solid substrate, the microspheres still tend to aggregate together due to the liquid surface tension and the presence of charge forces between the microspheres, as shown in fig. 5. It is therefore difficult to spontaneously form uniformly dispersed, density-controllable, disordered array monolayer microsphere templates on the surface of a solid substrate by means of self-assembly.
To solve this problem, the present invention proposes to add microspheres of smaller size to self-assembled microspheres. The microspheres with two sizes are uniformly mixed and then self-assembled, and the microspheres with small sizes are closely arranged and randomly separated from the microspheres with large sizes. The spacing distance between the large-size microspheres, namely the density of the large-size microspheres, can be regulated by regulating the adding proportion of the two different-size microspheres. And then removing the small-size microspheres by using an etching technology, so that the uniformly dispersed microsphere template with controllable density and disordered arrangement can be obtained on the surface of the solid substrate.
The invention discloses a method for preparing a uniformly dispersed, disordered and density-controllable microsphere template on the surface of a solid substrate in a large area and at low cost and application thereof. The method uses two kinds of microspheres with different sizes, uniformly mixes the microspheres according to different proportions, and constructs a single-layer microsphere film formed by mixing and arranging the two kinds of microspheres on the surface of a solid substrate in a self-assembly mode. The small-size microspheres are closely arranged in the microsphere film, and the large-size microspheres are randomly separated from each other, so that the large-size microspheres can be stably, randomly and dispersedly distributed in the film. And then removing the microspheres with smaller sizes by using an etching technology, and forming unordered and dispersed microsphere templates on the surface of the solid substrate by using the microspheres with larger residual sizes. The separation density of the large-size microspheres can be controlled by regulating the adding proportion of the large-size microspheres.
The first aspect of the present invention provides a method for preparing an unordered dispersion microsphere template on a surface of a solid substrate, the method comprising uniformly mixing large-sized microspheres and small-sized microspheres having different sizes; and removing the small-size microspheres by using an etching technology, thereby obtaining the uniformly dispersed large-size microsphere templates with controllable density and disordered arrangement on the surface of the solid substrate.
The second aspect of the invention provides a large-size microsphere template which is prepared by the method for preparing the disordered dispersed microsphere template on the surface of the solid substrate and is uniformly dispersed on the surface of the solid substrate, controllable in density and disordered in arrangement.
The third aspect of the invention provides application of the large-size microsphere template which is uniformly dispersed on the surface of a solid substrate, controllable in density and randomly arranged in the field of surface modification of biomedical materials and the research field of influence of porous microstructures with different densities on cell or bacterial behaviors and functions.
The present invention will be described in detail with reference to the following embodiments.
The large and small microspheres in the following examples are respectively polystyrene (Polystyrene, PS) microspheres with two sizes of 2 μm and 0.1 μm, the solid substrate is pure titanium sheet, the construction technology of microsphere film is transferred to the surface of the solid substrate by using dip-coating method after liquid level self-assembly, and the etching technology is plasma etching, so as to prove the feasibility of the method. In addition, the prepared microsphere templates will also be further processed in this example, thereby confirming the feasibility of constructing different microstructures on the surface of a solid substrate using the microsphere templates.
Example 1
Titanium sheets 10mm in diameter and 2mm in thickness were sanded sequentially with 800 mesh, 1200 mesh, 2000 mesh and 4000 mesh sandpaper. Then sequentially ultrasonic cleaning with acetone, alcohol and deionized water for 10 minutes. The titanium sheet thus obtained after pretreatment was used as a solid base material in this example. In addition, the plasma cleaning machine can be used for treating the titanium sheet to improve the hydrophilicity of the titanium sheet, so that the transfer of subsequent microspheres on the surface of the titanium sheet is facilitated.
Example 2
An aqueous suspension containing 10wt% of PS microspheres of 0.1 μm and 2 μm was mixed with an equal volume of ethanol, respectively. Then, the mixture was subjected to ultrasonic dispersion for 30 minutes using an ultrasonic cleaner. PS microspheres with the volume ratio of 0.1 mu m to 2 mu m after ultrasonic dispersion are mixed according to different proportions of 0:1, 1:4, 1:1 and 4:1, and after vortex oscillation, ultrasonic dispersion is carried out again for 30 minutes to ensure that the PS microspheres are uniformly mixed. The proportion of 2 μm microsphere in the microsphere mixture is 100%, 80%, 50% and 20%.
One clean glass slide is taken, one side of the glass slide is immersed into a culture dish containing distilled water, and the other side of the glass slide is supported to have an inclination angle of about 50 degrees. And then, slowly dripping PS microsphere mixed liquids with different proportions on an inclined glass slide, and uniformly self-assembling the microsphere mixed liquids on the water surface under the actions of Brownian motion, surface tension and the like to form a single-layer microsphere film after the microsphere mixed liquids contact the distilled water surface. Then immersing the bottom of the culture dish into an ultrasonic cleaner for ultrasonic treatment for 5min, so that the microspheres are dispersed more uniformly. Finally, the titanium sheet obtained in example 1 was immersed below the water surface along the side of the dish using tweezers. After the titanium sheet is transferred below the single-layer microsphere film, the titanium sheet is vertically lifted upwards, so that the microsphere film on the liquid level is transferred to the surface of the titanium sheet by the dipping-lifting method. The titanium sheet was then laid flat and dried at room temperature. The titanium sheet samples obtained are named as Ti100, ti80, ti50 and Ti20 according to the proportion of 2 mu m microspheres in the microsphere mixed solution.
The distribution of the microspheres on the surface of the titanium sheet was observed by an optical microscope (only large-sized microspheres having a diameter of 2 μm were visible by the optical microscope, and small-sized microspheres having a diameter of 0.1 μm were not visible). As shown in fig. 1a-d, as the proportion of the large-sized (2 μm) microspheres in the microsphere mixed solution decreases, the density of the large-sized microspheres on the surface of the titanium sheet gradually decreases, and the distribution state thereof gradually evolves from a highly ordered distribution (Ti 100) to a disordered dispersed distribution (Ti 80, ti50 and Ti 20).
Example 3
The small-sized microspheres in the microsphere thin film built on the surface of the titanium sheet in example 2 were removed using a plasma etching technique. And placing the sample into a sample chamber of a plasma etching machine, and vacuumizing. Then the power of the radio frequency power supply is set to be 100W, the pressure in the sample chamber is enabled to reach about 0.4mbar after oxygen is introduced, the plasma etching treatment is activated for 5-10min after the plasma etching treatment is stabilized, the PS microspheres with the diameter of 0.1 mu m are removed, and the PS microspheres with the diameter of 2 mu m are reserved. Samples Ti100, ti80, ti50 and Ti20 after plasma etching treatment were labeled as Ti100P, ti, 80, P, ti P and Ti20P, respectively. Fig. 2a shows the morphology of the microsphere film on the surface of the Ti20 sample before plasma etching, which is photographed by a scanning electron microscope. From the figure, it can be seen that the large-sized microspheres are randomly and randomly distributed on the surface, while the small-sized microspheres are closely arranged between the large-sized microspheres. Fig. 2b shows the morphology of the microsphere film on the surface of the Ti20 sample after plasma etching, which is photographed by a scanning electron microscope. It can be seen from the figure that after etching treatment, the small-sized microspheres are not substantially visible on the surface of the titanium sheet, and that after treatment the diameters of the large-sized microspheres are not substantially changed significantly. Therefore, the microsphere template with controllable density and unordered dispersion is successfully prepared on the surface of the titanium sheet through the treatment.
Example 4
The microsphere template prepared in the above example is further processed, thereby constructing disordered microstructures with different densities on the surface of the titanium sheet.
Preparing 0.5wt% titanium sulfate (Ti (SO 4)2) solution by using 0.05MH 2SO4 solution, adding 120 mu L of titanium isopropoxide (TTIP) into 10mL of absolute ethyl alcohol, blowing and mixing uniformly, vibrating for 30min, then dropwise adding 100 mu L of mixed solution of pure water and 2mL of isopropanol, continuously vibrating and mixing uniformly for 30min, regulating the pH to 3-4 by using a plurality of drops of concentrated hydrochloric acid, mixing uniformly to obtain a titanium dioxide hydrosol precursor, taking 20 mu L of prepared Ti (SO 4)2 solution or titanium dioxide hydrosol precursor, dropwise adding the Ti (SO 4)2 solution or titanium dioxide hydrosol precursor) onto microsphere templates with different densities prepared in the embodiment 3, and airing at room temperature.
Example 5
The Ti (SO 4)2 or hydrosol precursor) on the surface of the sample can be generated into a titanium dioxide film layer by high-temperature treatment, and the PS microsphere template with the thickness of 2 mu m can be removed by high-temperature treatment, then the titanium sheet is cooled to room temperature along with furnace cooling, SO that disordered TiO 2 porous structures with uniform distribution and different densities can be obtained, the porous samples obtained by the treatment are respectively marked as Ti100S, ti80S, ti S and Ti20S, and the surface morphology of the structures obtained by observation of a scanning electron microscope is shown in a figure X, as can be seen from FIGS. 3a to 3d, as the proportion of 2 μm microspheres added decreases, the density of holes in the resulting microstructure gradually decreases and the microstructure gradually evolves from a highly ordered (Ti 100S) to a random disordered state (Ti 80S, TI S and TI 20S).
The technical scheme of the invention is mainly divided into two parts, namely 1, uniformly mixing microspheres with different sizes (theoretically, the diameter difference is larger, such as 0.1 mu m and 2 mu m), and 2, constructing a single-layer microsphere film on the surface of a solid substrate in a self-assembly mode. The self-assembly can be directly carried out on the surface of the solid substrate, such as spin coating, evaporation induced self-assembly and the like, or can be carried out on the surface of the solution first, and then the monolayer microsphere film is transferred to the surface of the solid substrate. The microsphere film has small-size microspheres closely arranged and large-size microspheres randomly separated from each other, so that the large-size microspheres are dispersed and randomly arranged on the surface of the solid substrate. The separation distance of the large-size microspheres can be regulated by regulating the mixing proportion of the large-size microspheres. 3. The small-size microspheres are removed by etching technology, and a large-size microsphere template which is uniformly dispersed, controllable in density and unordered in arrangement is left. A flow chart of the method is shown in fig. 6.
In summary, the present invention provides a method for constructing a microsphere template with controllable density and unordered dispersion on the surface of a solid substrate in a large area and at low cost. The microspheres with smaller sizes are added into the conventional self-assembled microspheres, so that the microspheres with smaller sizes are randomly separated in the self-assembly process, and then the microspheres with smaller sizes are removed by an etching method, so that the uniformly dispersed, density-controllable and unordered large-size microsphere template is obtained on the surface of the solid substrate. The method can be used for surface modification of biomedical materials to improve the service effect of the materials, or can be applied to basic researches, such as the influence research of porous microstructures with different densities on the behavior and functions of cells or bacteria. The template preparation method provided by the invention can be applied to industrial manufacture as well, for example, to the manufacture of photoetching templates.
It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples of carrying out the application and that various changes in form and details may be made therein without departing from the spirit and scope of the application. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the application, and the scope of the application is therefore intended to be limited only by the appended claims.
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| PCT/CN2023/142451 WO2024159989A1 (en) | 2023-02-01 | 2023-12-27 | Method for preparing disordered and dispersed microsphere templates on surface of solid substrate, and use thereof |
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| CN101143710A (en) * | 2007-10-17 | 2008-03-19 | 中国科学院光电技术研究所 | Fabrication method of diamond-shaped metal nanoparticle array structure |
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| CN102923647A (en) * | 2012-11-22 | 2013-02-13 | 武汉大学 | Method for preparing ordered array of metal nano-particles with adjustable space and appearance |
| CN103499847B (en) * | 2013-10-11 | 2015-01-28 | 吉林大学 | Method for preparing hollow nanocone array film with optical anti-reflection function |
| CN103529081B (en) * | 2013-10-21 | 2016-02-03 | 苏州慧闻纳米科技有限公司 | A kind of preparation method of multiple layer metal oxide porous membrane gas-sensitive nano material |
| CN103933902B (en) * | 2014-05-12 | 2016-03-02 | 武汉大学 | A kind of binary ordered colloidal crystal, metal nano array and preparation method thereof |
| CN106542496A (en) * | 2015-09-18 | 2017-03-29 | 韩山师范学院 | The preparation method of ordered nano array structure |
| CN106082112A (en) * | 2016-06-24 | 2016-11-09 | 中国科学院长春光学精密机械与物理研究所 | A kind of micro structure silica-base material and preparation method thereof, semiconductor device |
| CN107758610A (en) * | 2017-10-17 | 2018-03-06 | 云南大学 | A kind of method that orderly small size silicon nanowire array is prepared based on ion beam etching |
| CN111816558A (en) * | 2019-04-12 | 2020-10-23 | 中国科学院长春光学精密机械与物理研究所 | A kind of manufacturing method of silicon-based deep hole microstructure |
| CN111272730B (en) * | 2020-02-11 | 2022-08-02 | 南京信息工程大学 | High-sensitivity optical fiber surface plasmon sensor and preparation method thereof |
| CN116177596B (en) * | 2023-02-01 | 2025-01-28 | 中国科学院深圳先进技术研究院 | A method for preparing a randomly dispersed microsphere template on a solid substrate surface and its application |
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2023
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- 2023-12-27 WO PCT/CN2023/142451 patent/WO2024159989A1/en not_active Ceased
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101143710A (en) * | 2007-10-17 | 2008-03-19 | 中国科学院光电技术研究所 | Fabrication method of diamond-shaped metal nanoparticle array structure |
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