CN111137897B - Preparation method of silicon dioxide nanorod array - Google Patents
Preparation method of silicon dioxide nanorod array Download PDFInfo
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- CN111137897B CN111137897B CN202010036342.4A CN202010036342A CN111137897B CN 111137897 B CN111137897 B CN 111137897B CN 202010036342 A CN202010036342 A CN 202010036342A CN 111137897 B CN111137897 B CN 111137897B
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
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Abstract
The invention provides a preparation method of a silicon dioxide nano rod array, which comprises the following steps: mixing a surfactant organic solution with a sodium citrate aqueous solution, then placing the mixture into a hydrophilic substrate, then adding an alkaline catalyst, performing ultrasonic treatment, then adding a silicon source, standing, and taking out the substrate to obtain the silicon dioxide nanorod array. Compared with the prior art, the method has the advantages that the solubility difference of water-soluble salts in the organic solvent-water mixed solution is utilized, salt liquid drops are separated out and adsorbed on a hydrophilic substrate, and the alkaline catalyst in the liquid drops is used for catalyzing and hydrolyzing a silicon source, so that the silicon dioxide nano array is prepared on the substrate, the one-step growth of no seeds through a solution liquid-phase solid-phase growth mechanism is realized, the used raw materials are cheap and pollution-free, the preparation process is simple and efficient, no pollutant is generated, the energy consumption is low, the equipment operation requirement is low, the mass production is easy to expand, and the diameter and the length of the silicon dioxide nano rod can be adjusted through the standing temperature and time.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a silicon dioxide nanorod array.
Background
The one-dimensional nanorod array has unique physical properties and geometric structures, such as short electron diffusion distance, allows integration into more complex structures, provides enough space for substance diffusion, light capturing capability and the like, and attracts more attention in the fields of photoelectrocatalysis, electrocatalytic, biochemical sensors and other energy storage and conversion.
Over the last few decades, gas-liquid-solid (VLS) mechanisms have been widely studied to provide an efficient way to produce one-dimensional nanorod arrays. For example, king et al reported that ZnO was grown on a single crystal alumina substrate based on a self-assembled template, and then used in a piezoelectric nanogenerator (Wang, z.l.; song, j.; piezoelectric Nanogenerators Based on Zinc Oxide Nanowire arrays.science2006,312 (5771), 242.); poplar et al reported that the growth site of the silicon nanowire array could be controlled in selected areas, providing the possibility for its practical integration into devices (Hochbaum, a.i.; fan, r.; he, r.; yang, p.; controlled Growth of Si Nanowire Arrays for Device integration. Nano Letters 2005,5 (3), 457-460.); ge nanowire electrodes fabricated using direct VLS growth on metal have demonstrated good performance in lithium ion batteries due to the ease of strain relaxation, short Li diffusion distances, and good electron conduction (Chan, c.k.; zhang, x.f.; cui, y.; high Capacity LiIon Battery Anodes Using Ge nanowires. Nano Letters 2008,8 (1), 307-309.). However, the nanorod array structures are all based on a VLS growth mechanism, and the growth mechanism is usually accompanied by the problems of high energy consumption, expensive reaction equipment, harsh reaction conditions and the like, and gold is also usually required to be used as a catalyst to be expensive.
Moreover, most other methods of preparing nanorod array structures involve multiple steps, which are generally complicated in step-by-step operation, and difficult to expand production and practical application. Therefore, urgent demands on nanorod array materials in the market and shortages of the current methods are caused to prompt development of a one-pot synthesis method which is simple and efficient in operation, easy to expand production and free from environmental pollution.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a simple, efficient preparation method for obtaining a silica nanorod array by a one-step method.
The invention provides a preparation method of a silicon dioxide nano rod array, which comprises the following steps:
mixing a surfactant organic solution with a sodium citrate aqueous solution, then placing the mixture into a hydrophilic substrate, then adding an alkaline catalyst, performing ultrasonic treatment, then adding a silicon source, standing, and taking out the substrate to obtain the silicon dioxide nanorod array.
Preferably, the organic solvent in the surfactant organic solution is selected from one or more of amyl alcohol, N-propanol, isopropanol, butanol and N, N-dimethylformamide; the surfactant in the surfactant organic solution is selected from polyvinylpyrrolidone, cetyltrimethylammonium bromide, sodium dodecyl sulfate and polyacrylic acid; the basic catalyst is selected from ammonia water and/or ethylenediamine; the silicon source is selected from tetraethyl silicate and/or tetramethyl silicate.
Preferably, the mass volume ratio of the surfactant to the organic solvent in the surfactant organic solution is (0.05-0.15) g:1ml; the concentration of sodium citrate in the sodium citrate aqueous solution is 0.01-0.1 mol/L; the volume ratio of the organic solvent of the surfactant organic solution to the sodium citrate aqueous solution is 1: (0.01-0.1).
Preferably, an alcohol solvent is also added when the basic catalyst is added; the volume ratio of the alcohol solvent to the organic solvent in the surfactant organic solution is 1: (8-12); the addition of both the alcohol solvent and the basic catalyst is not sequential.
Preferably, the volume ratio of the alkaline catalyst to the silicon source is (1-3): 1.
preferably, the volume ratio of the organic solvent to the silicon source in the surfactant organic solution is (50-150): 1.
preferably, the standing temperature is 10-70 ℃; the standing time is 1-8 h.
Preferably, the hydrophilic substrate is selected from one or more of a glass sheet, a metal sheet, an ITO glass, an FTO glass, a polymer film and a silicon wafer subjected to hydrophilic modification treatment.
Preferably, after the hydrophilic substrate is cleaned, the hydrophilic substrate is put into a mixed solution of a surfactant organic solution and a sodium citrate aqueous solution; the cleaning treatment is sequentially carried out by adopting acetone, deionized water and absolute ethyl alcohol.
Preferably, the diameter of the silica nanorods in the silica nanorod array is 0.2-0.5 μm; the length of the silica nano rod is 0.2-10 mu m.
The invention provides a preparation method of a silicon dioxide nano rod array, which comprises the following steps: mixing a surfactant organic solution with a sodium citrate aqueous solution, then placing the mixture into a hydrophilic substrate, then adding an alkaline catalyst, performing ultrasonic treatment, then adding a silicon source, standing, and taking out the substrate to obtain the silicon dioxide nanorod array. Compared with the prior art, the method has the advantages that the solubility difference of water-soluble salts in the organic solvent-water mixed solution is utilized, salt liquid drops are separated out and adsorbed on a hydrophilic substrate, and the alkaline catalyst in the liquid drops is used for catalyzing and hydrolyzing a silicon source, so that the silicon dioxide nano array is prepared on the substrate, the one-step growth of no seeds through a solution liquid-phase solid-phase growth mechanism is realized, the used raw materials are cheap and pollution-free, the preparation process is simple and efficient, no pollutant is generated, the energy consumption is low, the equipment operation requirement is low, the mass production is easy to expand, and the diameter and the length of the silicon dioxide nano rod can be adjusted through the standing temperature and time.
Furthermore, ammonia water is used as an alkaline catalyst, and the catalyst can be removed only by deionized washing after preparation.
Drawings
FIG. 1 is a schematic diagram of a preparation flow of a silica nanorod array provided by the invention;
FIG. 2 is a scanning electron microscope image of a silica nanorod array prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of a silica nanorod array prepared in example 2 of the present invention, and a change chart of the length of the nanorod array with the reaction time;
FIG. 4 is a scanning electron microscope image of a silica nanorod array prepared in example 3 of the present invention and a graph showing the change of the length of the nanorod array with the reaction time.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a preparation method of a silicon dioxide nano rod array, which comprises the following steps: mixing a surfactant organic solution with a sodium citrate aqueous solution, then placing the mixture into a hydrophilic substrate, then adding an alkaline catalyst, performing ultrasonic treatment, then adding a silicon source, standing, and taking out the substrate to obtain the silicon dioxide nanorod array.
Referring to fig. 1, fig. 1 is a schematic diagram of a preparation flow of a silica nanorod array provided by the invention.
The source of all the raw materials is not particularly limited, and the raw materials are commercially available.
Mixing a surfactant organic solution with a sodium citrate aqueous solution; the surfactant in the surfactant organic solution is preferably one or more of polyvinylpyrrolidone (PVP), cetyltrimethylammonium bromide (CTAB), sodium Dodecyl Sulfate (SDS) and polyacrylic acid (PAA), more preferably polyvinylpyrrolidone; the weight average molecular weight of the polyvinylpyrrolidone is preferably 10000 to 360000, more preferably 50000 to 60000, still more preferably 55000; the organic solvent in the surfactant organic solution is selected from one or more of amyl alcohol, N-propanol, isopropanol, butanol and N, N-dimethylformamide; the mass volume ratio of the surfactant to the organic solvent in the surfactant organic solution is preferably (0.05-0.15) g:1ml, more preferably (0.08 to 0.12) g:1ml, still more preferably 0.1g:1ml; the surfactant organic solution is preferably obtained by dissolving a surfactant in an organic solvent through ultrasonic treatment; the concentration of sodium citrate in the sodium citrate aqueous solution is preferably 0.01-0.1 mol/L, more preferably 0.03-0.08 mol/L, still more preferably 0.04-0.06 mol/L, still more preferably 0.05-0.055 mol/L, and most preferably 0.53mol/L; the volume ratio of the organic solvent to the sodium citrate aqueous solution in the surfactant organic solution is 1: (0.01 to 0.1), more preferably 1: (0.02 to 0.08), and more preferably 1: (0.02 to 0.06), and more preferably 1: (0.03 to 0.04), most preferably 1:0.038.
then placing the hydrophilic substrate; the hydrophilic substrate is preferably put in after being cleaned; the hydrophilic substrate is preferably one or more of a glass sheet, a metal sheet, ITO glass, FTO glass, a polymer film and a silicon wafer subjected to hydrophilic modification treatment; the cleaning treatment is preferably carried out by adopting acetone, deionized water and absolute ethyl alcohol in sequence; the cleaning treatment is preferably ultrasonic cleaning; after the cleaning treatment, the mixture is preferably dried by nitrogen and then put into a mixed solution of a surfactant organic solution and a sodium citrate aqueous solution.
Adding an alkaline catalyst, and preferably adding an alcohol solvent when adding the alkaline catalyst in the invention; the addition of both the alcohol solvent and the basic catalyst is not sequential; the alkaline catalyst is preferably ammonia water and/or ethylenediamine; the alcohol solvent is preferably one or more of methanol, ethanol, n-propanol and isopropanol, more preferably ethanol; the volume ratio of the alcohol solvent to the organic solvent in the surfactant organic solution is preferably 1: (8-12), more preferably 1: (9 to 11), and more preferably 1:10. the method does not need to additionally prepare nano particles as a catalyst, and can directly use the alkaline catalyst, so that the nano particles are easy to remove after the preparation is finished.
Performing ultrasonic treatment; the power of the ultrasonic wave is preferably 60% -99% of that of a 100W ultrasonic machine; in some embodiments provided by the present invention, the power of the sonication is preferably 80% of that of a 100W sonicator; in other embodiments provided by the present invention, the power of the sonication is preferably 99% of a 100W sonicator; the time of the ultrasonic wave is preferably 10 seconds to 20 seconds; the water temperature in the ultrasonic machine is preferably 20-40 ℃; intense agitation is provided by sonication to form a stable emulsion system.
After ultrasonic treatment, adding a silicon source; the silicon source is preferably tetraethyl silicate and/or tetramethyl silicate; the volume ratio of the silicon source to the alkaline catalyst is preferably 1: (1 to 3), more preferably 1: (1.5 to 2.5), and more preferably 1:2; the volume ratio of the silicon source to the organic solvent in the surfactant organic solution is preferably 1: (50 to 150), more preferably 1: (80 to 120), and more preferably 1: (90 to 110), most preferably 1:100.
adding a silicon source, preferably performing ultrasonic treatment, and standing; the power of the ultrasonic treatment is preferably 60% -99% of that of a 100W ultrasonic machine; in some embodiments provided by the present invention, the power of the sonication is preferably 60% of a 100W sonicator; in some embodiments provided by the present invention, the power of the sonication is preferably 80% of that of a 100W sonicator; in other embodiments provided by the present invention, the power of the sonication is preferably 99% of a 100W sonicator; the time of the ultrasonic wave is preferably 10 seconds to 20 seconds; the water temperature in the ultrasonic machine is preferably 20-40 ℃; the temperature of the standing is preferably 10-70 ℃, more preferably 20-60 ℃; in some embodiments provided herein, the resting temperature is preferably 20 ℃; in some embodiments provided herein, the resting temperature is preferably 40 ℃; in other embodiments provided herein, the resting temperature is preferably 60 ℃; the time for the standing is preferably 1 to 8 hours, more preferably 1 to 6 hours, still more preferably 1 to 4 hours; in some embodiments provided herein, the time of resting is preferably 1h; in some embodiments provided herein, the time of resting is preferably 2 hours; in some embodiments provided herein, the time of resting is preferably 4 hours. The preparation process of the invention is standing, heating and stirring are not needed, and post-treatment such as calcination is also not needed, thus the energy consumption is low.
After standing, taking out the substrate, preferably washing with water and ethanol, and drying to obtain a silica nanorod array; the diameter of the silica nanorods in the silica nanorod array is preferably 0.2-0.5 μm, more preferably 0.28-0.35 μm; the length of the silica nanorods is preferably 0.2 to 10. Mu.m, more preferably 0.2 to 6. Mu.m, still more preferably 0.29 to 4.54. Mu.m.
In the present invention, a composite nanorod array can also be obtained on the resulting silica nanorod array using various methods such as solution growth, physical sputtering, etc.
According to the invention, by utilizing the solubility difference of water-soluble salts in the organic solvent-water mixed solution, salt liquid drops are separated out and adsorbed on a hydrophilic substrate, and a silicon source is catalyzed and hydrolyzed by an alkaline catalyst in the liquid drops, so that the silicon dioxide nano array is prepared on the substrate, the growth of a seed-free one-step method through a solution liquid-phase solid-phase growth mechanism is realized, the used raw materials are cheap and pollution-free, the preparation process is simple and efficient, no pollutant is generated, the energy consumption is low, the equipment operation requirement is low, the mass production is easy to expand, and the diameter and the length of the silicon dioxide nano rod can be adjusted by standing temperature and time.
Furthermore, ammonia water is used as an alkaline catalyst, and the catalyst can be removed only by deionized washing after preparation.
In order to further illustrate the present invention, the following describes in detail a method for preparing a silica nanorod array according to the present invention with reference to examples.
The reagents used in the examples below are all commercially available; in the examples, a 100W ultrasonic machine was used for ultrasonic treatment.
Example 1
1.1 substrate cleaning: firstly, ultrasonic cleaning is carried out on the ITO glass substrate by using acetone, deionized water and absolute ethyl alcohol, and the substrate is dried by using nitrogen for standby.
1.2 Synthesis of silica nanorod arrays: 1g PVP (MW 55000) was dissolved in 10mL 1-pentanol by sonication, and 380. Mu.L aqueous sodium citrate (0.053M) was added. The cleaned ITO substrate is then immersed in the above solution. 200. Mu.L of ammonium hydroxide solution (25% -28% strength) and 1mL of ethanol were added to the reaction. Vigorous stirring was provided by sonication (power 60%, time 10 seconds, water temperature 20 ℃) to form a stable emulsion system. The growth of the silica nanorods began with the addition of 100. Mu.L of tetraethyl silicate (after the addition of tetraethyl silicate, a 60% ultrasonic power treatment was required for 10s followed by resting). The mixed solution was allowed to stand at 60℃for 4 hours. And finally, taking out the substrate from the solution, washing the substrate with water and ethanol for a plurality of times, and drying the substrate to obtain the silica nanorod array.
The silica nanorod array obtained in example 1 was detected by using a scanning electron microscope, and a scanning electron microscope diagram of the silica nanorod array is shown in fig. 2. As can be seen from fig. 2, the silica nanorods in the silica nanorod array obtained in example 1 had a diameter of 0.28 μm and a length of 4.54 μm.
Example 2
2.1 substrate cleaning: firstly, ultrasonic cleaning is carried out on the ITO glass substrate by using acetone, deionized water and absolute ethyl alcohol, and the substrate is dried by using nitrogen for standby.
2.2 Synthesis of silica nanorod arrays: in a typical experiment, 1g PVP (MW 55000) was dissolved in 10mL 1-pentanol by sonication, and 380. Mu.L sodium citrate in water (0.053M) was added. The cleaned substrate is then immersed in the solution. 200. Mu.L of ammonium hydroxide solution (25% strength) and 1mL of ethanol were added to the reaction. Intense agitation was provided by sonication (power 99%, time 20 seconds, water temperature 30 ℃) to form a stable emulsion system. Growth of the silica nanorods began with the addition of 100 μl of tetraethyl silicate (sonicated first and then allowed to stand, sonicated at 99% power for 20 seconds and then allowed to stand). The mixed solutions were allowed to stand at 60℃for 1 hour, 2 hours and 4 hours, respectively. And finally, taking out the substrate from the solution, washing the substrate with water and ethanol for a plurality of times, and drying the substrate to obtain the silica nanorod array.
The silica nanorod array obtained in example 2 was detected by using a scanning electron microscope to obtain a scanning electron microscope image and a graph of the change of the length of the nanorod array with the reaction time, as shown in fig. 3, wherein the reaction time a is 1h, the reaction time b is 2h, the reaction time c is 4h, and the length of the nanorod array with the reaction time d is the graph of the change of the length of the nanorod array with the reaction time. As can be seen from FIG. 3, the nanorod lengths were 0.68 μm,2.01 μm and 4.54 μm, respectively, with little change in diameter, when the reaction times were 1 hour, 2 hours and 4 hours, respectively. It can be seen that the length of the nanorods gradually increases with increasing reaction time, while the diameter remains unchanged, consistent with the solution liquid-solid phase growth mechanism.
Example 3
3.1 substrate cleaning: firstly, carrying out ultrasonic cleaning on ITO glass, FTO glass and a glass substrate by using acetone, deionized water and absolute ethyl alcohol, and drying the substrate by using nitrogen for standby.
3.2 Synthesis of silica nanorod arrays: in a typical experiment, 1g PVP (MW 55000) was dissolved in 10mL 1-pentanol by sonication, and 380. Mu.L sodium citrate in water (0.053M) was added. The cleaned substrate is then immersed in the solution. 200. Mu.L of ammonium hydroxide solution (25% strength) and 1mL of ethanol were added to the reaction. Vigorous stirring was provided by sonication (power 80%, time 15 seconds, water temperature 35 ℃) to form a stable emulsion system. Growth of the silica nanorods began with the addition of 100 μl of tetraethyl silicate (sonicated first and then allowed to stand, sonicated at 80% power for 15 seconds and then allowed to stand). The mixed solution was allowed to stand at 20℃and 40℃and 60℃for 4 hours, respectively. And finally, taking out the substrate from the solution, washing the substrate with water and ethanol for a plurality of times, and drying the substrate to obtain the silica nanorod array.
The silica nanorod array obtained in example 3 was detected by using a scanning electron microscope, so as to obtain a scanning electron microscope image and a graph of the change of the length of the nanorod array with the reaction temperature, as shown in fig. 4, wherein the reaction temperature a is 20 ℃, the reaction temperature b is 40 ℃, the reaction temperature c is 60 ℃, and d is the graph of the change of the length of the nanorod array with the reaction temperature. As can be seen from FIG. 4, the nanorods had lengths of 0.29 μm,1.89 μm and 4.54 μm, respectively, and diameters decreased from 0.35 μm,0.31 μm to 0.28 μm at reaction temperatures of 20 ℃, 40 ℃ and 60 ℃. It can be seen that as the reaction temperature increases, the length of the nanorods gradually increases, while the diameter gradually decreases. This suggests that the growth temperature may affect the growth rate of the silica nanorods and the amount of water in the catalyst droplets. This provides an opportunity to manipulate the shape of the silica nanorod array without changing the reaction solution.
Claims (7)
1. A method for preparing a silica nanorod array, comprising:
mixing a surfactant organic solution with a sodium citrate aqueous solution, then placing the mixture into a hydrophilic substrate, adding an alkaline catalyst, performing ultrasonic treatment, adding a silicon source, standing, and taking out the substrate to obtain a silicon dioxide nanorod array;
the organic solvent in the surfactant organic solution is selected from one or more of amyl alcohol, N-propanol, isopropanol, butanol and N, N-dimethylformamide; the surfactant in the surfactant organic solution is selected from polyvinylpyrrolidone, cetyltrimethylammonium bromide, sodium dodecyl sulfate and polyacrylic acid; the basic catalyst is selected from ammonia water and/or ethylenediamine; the silicon source is selected from tetraethyl silicate and/or tetramethyl silicate;
the mass volume ratio of the surfactant to the organic solvent in the surfactant organic solution is (0.05-0.15) g:1ml; the concentration of sodium citrate in the sodium citrate aqueous solution is 0.01-0.1 mol/L; the volume ratio of the organic solvent of the surfactant organic solution to the sodium citrate aqueous solution is 1: (0.01-0.1);
when the alkaline catalyst is added, an alcohol solvent is also added; the volume ratio of the alcohol solvent to the organic solvent in the surfactant organic solution is 1: (8-12); the addition of both the alcohol solvent and the basic catalyst is not sequential.
2. The method according to claim 1, wherein the volume ratio of the basic catalyst to the silicon source is (1 to 3): 1.
3. the method of claim 1, wherein the volume ratio of organic solvent to silicon source in the surfactant organic solution is (50-150): 1.
4. the method according to claim 1, wherein the temperature of the standing is 10 ℃ to 70 ℃; the standing time is 1-8 h.
5. The method of claim 1, wherein the hydrophilic substrate is selected from one or more of a glass sheet, a metal sheet, an ITO glass, an FTO glass, a polymer film, and a hydrophilically modified silicon wafer.
6. The method according to claim 1, wherein the hydrophilic substrate is washed and then put into a mixed solution of a surfactant organic solution and a sodium citrate aqueous solution; the cleaning treatment is sequentially carried out by adopting acetone, deionized water and absolute ethyl alcohol.
7. The method of claim 1, wherein the diameter of the silica nanorods in the silica nanorod array is 0.2-0.5 μm; the length of the silica nano rod is 0.2-10 mu m.
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| CN107195521A (en) * | 2017-04-24 | 2017-09-22 | 西北师范大学 | Silica nanometer chamber array electrode as ion channel application |
| CN108483451A (en) * | 2018-05-25 | 2018-09-04 | 苏州大学 | The preparation method of hollow-core construction micro/nano material |
| CN110540372A (en) * | 2019-09-02 | 2019-12-06 | 中国科学院合肥物质科学研究院 | Non-close-packed silicon dioxide ring nano array and preparation method thereof |
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