Micro-bulge structure generation method based on controllable gas phase microreactor

Abstract

The invention relates to the technical field of preparation of surface micro-nano structures, and discloses a method for generating a micro-bulge structure based on a controllable gas phase microreactor, which comprises the following steps: preparing an organic mixed solution, mixing a driving solution methyl methacrylate into an initiator di-tert-butyl peroxide solution, then adding a solvent dimethyl sulfoxide solution, and stirring to obtain a mixed solution; meanwhile, ultrasonic oscillation is carried out for 10 minutes; according to the method for generating the micro-bulge structure based on the controllable gas-phase microreactor, the preparation of the micro-bulge structure can be realized only by directly dropwise adding a precursor organic mixed solution of a polymer on the surface of a substrate with a photothermal effect and then controlling the irradiation position and energy of continuous wave laser; compared with a photoetching method, the method has the advantages that complicated equipment operation and tedious process steps are not needed, and compared with the photoetching method, expensive photoetching machines, masks, vacuum chambers and complicated chemical reagent treatment processes are not needed, so that the operation flow is simplified.

Description

Technical Field

[0001] The invention relates to the technical field of preparation of surface micro-nano structures, and in particular to a method for generating a micro-convex structure based on a controllable gas phase microreactor. Background Art

[0002] Surface micro-nanostructures play an important role in improving catalytic performance, enhancing surface stability and durability, energy conversion and storage applications, and optimizing composite material performance.

[0003] At present, there are many methods for preparing surface micro-nano structures, such as high-energy beam direct writing, photolithography, hydrothermal synthesis, soft template method, etc. High-energy beam direct writing mainly relies on high-energy beam devices such as focused ion beam, electron beam, femtosecond / picosecond laser, etc., and uses the photochemical, thermochemical or thermophysical effects generated by them to etch or deposit materials on the surface of materials, thereby achieving high-precision micro-nano structure processing. However, the high-energy beam system generally required by this method is often expensive and has relatively high maintenance costs. At the same time, the processing speed is relatively slow. In order to ensure processing accuracy and quality, the direct writing method requires high technical level and experience of the operator. When processing certain special materials, thermal effects and possible damage will also affect the accuracy of micro-nano structures. Photolithography generally transfers the structure on the photomask template to the sample surface accurately through specific light exposure and etching. However, the production process of this method involves expensive photolithography machines, masks, vacuum chambers and complex chemical reagents, which is not only time-consuming but also cumbersome. In addition, the template removal process may generate waste, which has a certain impact on the environment. The hydrothermal synthesis method mainly places the polymer precursor solution in a closed reactor at high temperature and high pressure, and uses the high temperature and high pressure environment of the hydrothermal synthesis to promote the chemical reaction to obtain a polymer microstructure. However, this method is difficult to prepare polymer microstructures on the surface in a controllable manner, and requires special equipment to complete. The soft template synthesis method uses a substance with a nanostructure and easily controllable shape as a template, such as colloidal particles, microspheres, oil droplets, etc., and deposits it on the surface of the template by physical or chemical methods, and then removes the template to obtain a nanomaterial with the standard morphology and size of the template. However, the distribution and size of the soft template in this method are difficult to control.

[0004] In summary, both the high-energy beam direct writing method and the hydrothermal synthesis method require special equipment to complete the preparation of surface micro-nano structures. The photolithography method is simple to prepare surface micro-nano structures, but the operation process is complicated and the preparation conditions are relatively strict. The soft template method is simple to prepare surface micro-nano structures, but the controllability of the prepared micro-nano structures is poor. Therefore, it is necessary to invent a method for generating micro-protrusion structures based on a controllable gas phase microreactor to solve the above problems. Summary of the invention

[0005] The present invention provides the following technical solution: a method for generating a micro-protrusion structure based on a controllable gas phase microreactor, comprising the following steps:

[0006] S1. Prepare an organic mixed solution, mix the body solution methyl methacrylate into the initiator di-tert-butyl peroxide solution, then add the solvent dimethyl sulfoxide solution, and oscillate ultrasonically for 10 minutes.

[0007] S2. Prepare a substrate sample. Take a piece of fused quartz glass and perform a series of cleanings. Then, use magnetron sputtering to deposit a layer of precious metal nanoparticles on its surface to complete the sample preparation.

[0008] S3. Fill the glass cuvette with the organic mixed solution prepared in step S1, and place the fused quartz glass sample inside.

[0009] S4. Turn on the laser and focus the laser on the upper surface of the substrate sample. In about 40ms, a micrometer-scale plasmon bubble will quickly form at the light spot on the surface of the substrate sample, inducing a chemical reaction between gaseous molecules in the high-temperature environment inside the gas phase microreactor, and producing a micro-convex structure on the surface of the substrate sample.

[0010] S5. After the laser irradiates continuously for a period of time, turn off the laser, and the gas phase microreactor will immediately desorb the surface of the substrate sample. Then, the substrate surface is taken out of the cuvette, cleaned with a large amount of ethanol, and then blown dry with nitrogen, so that the micro-protrusion structure can be prepared on the sample surface.

[0011] Preferably, in step S1, the molar concentration of the methyl methacrylate solution is 3 mol / L, the volume fraction is 45%, the volume fraction of the di-tert-butyl peroxide solution is 12%, the mass fraction of the active ingredient di-tert-butyl peroxide is 10%, and the volume fraction of the dimethyl sulfoxide solution is 43%.

[0012] Preferably, in step S2, the noble metal nanoparticles may be gold nanoparticles and silver nanoparticles.

[0013] Preferably, in step S4, the laser power can be 75mW, 100mW, 150mW, or 200mW, and a 20X focusing objective lens is used.

[0014] Preferably, in step S5, the irradiation time is 50 seconds.

[0015] Compared with the prior art, the present invention provides a method for generating a micro-protrusion structure based on a controllable gas phase microreactor, which has the following beneficial effects:

[0016] 1. The method for generating micro-convex structures based on a controllable gas phase microreactor only requires dripping the precursor organic mixed solution of the polymer directly onto the surface of the substrate with a photothermal effect, and then controlling the irradiation position and energy of the continuous wave laser to achieve the preparation of the micro-convex structure. It does not require complex equipment operation and cumbersome process steps. Compared with photolithography, it does not require expensive photolithography machines, masks, vacuum chambers, and complex chemical reagent processing processes, thereby simplifying the operation process.

[0017] 2. The method for generating micro-convex structures based on a controllable gas-phase microreactor can rapidly generate micron-scale surface micro-convex structures. The size, generation position and generation speed of the gas-phase microreactor completely depend on the position and energy parameters of the continuous wave laser irradiation on the substrate surface. By changing the irradiation position of the laser, the generation position of the micro-convex structure can be precisely controlled, so that micro-convex structures with specific sizes and morphologies can be prepared according to actual needs, thereby achieving a high degree of controllability in the preparation of surface micro-convex structures. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 Schematic diagram of the preparation process of the surface micro-protrusion structure of the present invention;

[0019] Figure 2 A schematic diagram of a scanning sample of an atomic force microscope on a surface micro-convex structure of the present invention;

[0020] Figure 3 A schematic diagram of a scanning sample of a scanning electron microscope of a surface micro-protrusion structure of the present invention;

[0021] Figure 4 It is a schematic diagram of a sample of the regulation of the surface micro-protrusion structure according to the position of the gas phase micro-reactor of the present invention;

[0022] Figure 5 This is a schematic diagram of a sample of the present invention in which the surface micro-protrusion structure is regulated by the size of the gas phase micro-reactor. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] Embodiment 1:

[0025] See also Figure 1-5 The present invention provides a technical solution: a method for generating a micro-protrusion structure based on a controllable gas phase microreactor, comprising the following steps:

[0026] S1. Prepare an organic mixed solution, mix the molar concentration of 3 mol / L and the volume fraction of 45% methyl methacrylate as the body solution into the volume fraction of 12% and the initiator di-tert-butyl peroxide solution of 10% of the active ingredient di-tert-butyl peroxide, and then add the solvent dimethyl sulfoxide solution of 43% by volume, accompanied by ultrasonic oscillation for 10 minutes.

[0027] S2. Prepare a substrate sample. Take a piece of fused quartz glass and perform a series of cleanings. Then, use magnetron sputtering to deposit a layer of gold nanoparticles on its surface to complete the sample preparation.

[0028] S3. Fill the glass cuvette with the organic mixed solution prepared in step S1, and place the fused quartz glass sample inside.

[0029] S4. Turn on the laser, set the laser power to 75 mW, use a 20X focusing objective lens to focus the laser on the upper surface of the substrate sample, generate a gas phase microreactor at position 1 on the substrate surface, turn off the laser after 50 seconds of laser irradiation, and obtain a micro-protrusion structure.

[0030] S5. After the laser is continuously irradiated for a period of time, turn off the laser, the gas phase microreactor will immediately desorb the surface of the substrate sample, then take the substrate surface out of the cuvette, wash it with a large amount of ethanol, and then blow it dry with nitrogen to prepare a micro-protrusion structure on the sample surface. Then, move the laser to position 2 on the substrate surface, turn on the laser again to generate a gas phase microreactor, turn off the laser after continuous irradiation for 50s, and obtain a new micro-protrusion structure. Move the laser to position 3 on the substrate surface again, turn on the laser again to generate a gas phase microreactor, turn off the laser after continuous irradiation for 50s, and obtain a new micro-protrusion structure. As the laser focus spot moves on the substrate surface, the position of the micro-protrusion structure is regulated.

[0031] Embodiment 2:

[0032] A method for generating a micro-protrusion structure based on a controllable gas phase microreactor comprises the following steps:

[0033] S1. Prepare an organic mixed solution, mix the molar concentration of 3 mol / L and the volume fraction of 45% methyl methacrylate as the body solution into the volume fraction of 12% and the initiator di-tert-butyl peroxide solution of 10% of the active ingredient di-tert-butyl peroxide, and then add the solvent dimethyl sulfoxide solution of 43% by volume, accompanied by ultrasonic oscillation for 10 minutes.

[0034] S2. Prepare a substrate sample. Take a piece of fused quartz glass and perform a series of cleanings. Then, use magnetron sputtering to deposit a layer of gold nanoparticles on its surface to complete the sample preparation.

[0035] S3. Fill the glass cuvette with the organic mixed solution prepared in step S1, and place the fused quartz glass sample inside.

[0036] S4. Turn on the laser, set the laser power to 100 mW, use a 20X focusing objective lens to focus the laser on the upper surface of the substrate sample, generate a gas phase microreactor at position 1 on the substrate surface, turn off the laser after 50 seconds of laser irradiation, and obtain a micro-protrusion structure.

[0037] S5. After the laser is continuously irradiated for a period of time, turn off the laser, and the gas-phase microreactor will immediately desorb the surface of the substrate sample. Then, take the substrate surface out of the cuvette, wash it with a large amount of ethanol, and then blow it dry with nitrogen to prepare a micro-protrusion structure on the sample surface. Then, move the laser to position 2 on the substrate surface, turn on the laser again to generate a gas-phase microreactor, turn off the laser after continuous irradiation for 50 seconds, and obtain a new micro-protrusion structure. Move the laser to position 3 on the substrate surface again, turn on the laser again to generate a gas-phase microreactor, turn off the laser after continuous irradiation for 50 seconds, and obtain a new micro-protrusion structure. As the laser focus spot moves on the substrate surface, the position of the micro-protrusion structure is regulated.

[0038] Embodiment three:

[0039] A method for generating a micro-protrusion structure based on a controllable gas phase microreactor comprises the following steps:

[0040] S1. Prepare an organic mixed solution, mix the molar concentration of 3 mol / L and the volume fraction of 45% methyl methacrylate as the body solution into the volume fraction of 12% and the initiator di-tert-butyl peroxide solution of 10% of the active ingredient di-tert-butyl peroxide, and then add the solvent dimethyl sulfoxide solution of 43% by volume, accompanied by ultrasonic oscillation for 10 minutes.

[0041] S2. Prepare a substrate sample. Take a piece of fused quartz glass and perform a series of cleanings. Then, use magnetron sputtering to deposit a layer of gold nanoparticles on its surface to complete the sample preparation.

[0042] S3. Fill the glass cuvette with the organic mixed solution prepared in step S1, and place the fused quartz glass sample inside.

[0043] S4. Turn on the laser, set the laser power to 150 mW, use a 20X focusing objective lens to focus the laser on the upper surface of the substrate sample, generate a gas phase microreactor at position 1 on the substrate surface, turn off the laser after 50 seconds of laser irradiation, and obtain a micro-protrusion structure.

[0044] S5. After the laser is continuously irradiated for a period of time, turn off the laser, the gas phase microreactor will immediately desorb the surface of the substrate sample, then take the substrate surface out of the cuvette, wash it with a large amount of ethanol, and then blow it dry with nitrogen to prepare a micro-protrusion structure on the sample surface. Then, move the laser to position 2 on the substrate surface, turn on the laser again to generate a gas phase microreactor, turn off the laser after continuous irradiation for 50s, and obtain a new micro-protrusion structure. Move the laser to position 3 on the substrate surface again, turn on the laser again to generate a gas phase microreactor, turn off the laser after continuous irradiation for 50s, and obtain a new micro-protrusion structure. As the laser focus spot moves on the substrate surface, the position of the micro-protrusion structure is regulated.

[0045] Embodiment 4:

[0046] A method for generating a micro-protrusion structure based on a controllable gas phase microreactor comprises the following steps:

[0047] S1. Prepare an organic mixed solution, mix the molar concentration of 3 mol / L and the volume fraction of 45% methyl methacrylate as the body solution into the volume fraction of 12% and the initiator di-tert-butyl peroxide solution of 10% of the active ingredient di-tert-butyl peroxide, and then add the solvent dimethyl sulfoxide solution of 43% by volume, accompanied by ultrasonic oscillation for 10 minutes.

[0048] S2. Prepare a substrate sample. Take a piece of fused quartz glass and perform a series of cleanings. Then, use magnetron sputtering to deposit a layer of gold nanoparticles on its surface to complete the sample preparation.

[0049] S3. Fill the glass cuvette with the organic mixed solution prepared in step S1, and place the fused quartz glass sample inside.

[0050] S4. Turn on the laser, set the laser power to 200 mW, use a 20X focusing objective lens to focus the laser on the upper surface of the substrate sample, generate a gas phase microreactor at position 1 on the substrate surface, turn off the laser after 50 seconds of laser irradiation, and obtain a micro-protrusion structure.

[0051] S5. After the laser is continuously irradiated for a period of time, turn off the laser, and the gas-phase microreactor will immediately desorb the surface of the substrate sample. Then, take the substrate surface out of the cuvette, wash it with a large amount of ethanol, and then blow it dry with nitrogen to prepare a micro-protrusion structure on the sample surface. Then, move the laser to position 2 on the substrate surface, turn on the laser again to generate a gas-phase microreactor, turn off the laser after continuous irradiation for 50 seconds, and obtain a new micro-protrusion structure. Move the laser to position 3 on the substrate surface again, turn on the laser again to generate a gas-phase microreactor, turn off the laser after continuous irradiation for 50 seconds, and obtain a new micro-protrusion structure. As the laser focus spot moves on the substrate surface, the position of the micro-protrusion structure is regulated.

[0052] The method for generating a micro-convex structure based on a controllable gas phase microreactor can control the position and size of the micro-convex structure by regulating the focusing position of the laser on the substrate surface and the laser energy parameters. A continuous wave laser in the plasmon resonance band with the substrate surface material is used to irradiate the substrate surface immersed in an organic mixed solution to trigger a photothermal effect. A local heat source is formed at the light plate irradiated by the laser, which rapidly generates a large amount of heat to vaporize the solution and generate micron-sized plasmon bubbles. The bubbles rapidly separate the organic mixed solution from the substrate surface to form a gas phase microreactor. The gas phase microreactor has a high temperature inside and contains different gaseous molecules of the organic mixed solution. Under the condition of continuous input of laser energy, the different gaseous molecules inside the gas phase microreactor undergo a chemical reaction and are then deposited on the substrate surface at the bottom of the gas phase microreactor to form a micro-convex structure. The size, generation position and generation speed of the gas phase microreactor are completely dependent on the position and energy parameters of the continuous wave laser irradiation on the fused quartz surface, so the preparation of the surface micro-convex structure is highly controllable.

[0053] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for generating a micro-protrusion structure based on a controllable gas phase microreactor, characterized in that: The following steps are involved: S1, preparing an organic mixed solution, mixing the body solution methyl methacrylate into the initiator di-tert-butyl peroxide solution, and then adding the solvent dimethyl sulfoxide solution, accompanied by ultrasonic oscillation for 10 minutes; S2. Prepare a substrate sample, take a piece of fused quartz glass, perform a series of cleanings, and then deposit a layer of noble metal nanoparticles on its surface by magnetron sputtering to complete the sample preparation; S3, filling a glass cuvette with the organic mixed solution in step S1, and placing the fused quartz glass sample inside the glass cuvette; S4, turn on the laser and focus the laser on the upper surface of the substrate sample. In about 40ms, a micron-sized plasmon bubble will quickly form at the spot on the surface of the substrate sample, inducing a chemical reaction between gaseous molecules in the high temperature environment inside the gas phase microreactor, and generating a micro-convex structure on the surface of the substrate sample; S5. After the laser irradiates continuously for a period of time, turn off the laser, and the gas phase microreactor will immediately desorb the surface of the substrate sample. Then, the substrate surface is taken out of the cuvette, cleaned with a large amount of ethanol, and then blown dry with nitrogen, so that the micro-protrusion structure can be prepared on the sample surface.

2. The method for generating a micro-protrusion structure based on a controllable gas phase microreactor according to claim 1, characterized in that: In step S1, the molar concentration of the methyl methacrylate solution is 3 mol / L, the volume fraction is 45%, the volume fraction of the di-tert-butyl peroxide solution is 12%, the mass fraction of the effective ingredient di-tert-butyl peroxide is 10%, and the volume fraction of the dimethyl sulfoxide solution is 43%.

3. The method for generating a micro-protrusion structure based on a controllable gas phase microreactor according to claim 1, characterized in that: In step S2, the noble metal nanoparticles may be gold nanoparticles and silver nanoparticles.

4. The method for generating a micro-protrusion structure based on a controllable gas phase microreactor according to claim 1, characterized in that: In step S4, the laser power can be 75mW, 100mW, 150mW, or 200mW, and a 20X focusing objective lens is used.

5. The method for generating a micro-protrusion structure based on a controllable gas phase microreactor according to claim 1, characterized in that: In step S5, the irradiation time is 50 seconds.

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