Point catalyst laying method based on liquid bridging
The catalyst particles are precisely transferred to the tip of the target substrate through liquid bridging technology, which solves the problems of high equipment cost and large-area batch processing, realizes high-precision and simple catalyst layout, is applicable to a variety of materials, reduces energy consumption and improves equipment life.
Patent Information
- Application Number
- CN202510665751.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-22
- Publication Date
- 2025-10-17
AI Technical Summary
Existing catalyst placement technology and equipment are expensive and difficult to implement for large-scale batch processing. Traditional methods make it difficult to achieve high-precision distribution of catalysts on cutting-edge structures.
Liquid bridge technology is used to precisely transfer catalyst particles to the tip of the target substrate using a liquid bridge through oxygen plasma surface treatment, spin formation of catalyst and assisted transfer of liquid film.
It achieves high-precision catalyst placement, reduces production costs and operating difficulty, improves production efficiency, is applicable to a variety of catalysts and substrate materials, has wide applicability and repeatability, reduces energy consumption and extends equipment life.
Smart Images
Figure CN120790460A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of catalyst layout, and particularly relates to a tip catalyst layout method based on liquid bridging. BACKGROUND
[0002] In recent years, two-dimensional materials have shown broad application prospects in the fields of electronic devices, optoelectronic devices, energy storage and conversion, etc. due to their unique physical and chemical properties. Chemical vapor deposition (CVD) method is one of the main methods for preparing high-quality two-dimensional materials, and the precise layout of catalyst is one of the key steps for preparing two-dimensional materials by the CVD method. The catalyst layout on the tip structure can significantly improve the nucleation efficiency and growth quality of two-dimensional materials by utilizing the tip effect (such as local electric field enhancement, high surface energy, etc.), so as to obtain uniform and high-performance two-dimensional materials. The traditional catalyst layout techniques mainly include spin coating method, drop coating method, electron beam deposition method and AFM (atomic force microscope) cantilever assisted dipping method, etc. Among them, the spin coating method and the drop coating method are difficult to control the local distribution of catalyst particles in the tip region of the needle, and are prone to cause large-area coverage of materials in non-target areas; the electron beam deposition and the AFM cantilever assisted dipping method have high precision, but the equipment cost is high and it is difficult to realize large-area batch processing. In view of the above problems, it is urgent to develop a method which can realize high-precision catalyst layout on the tip structure with low cost and high efficiency. SUMMARY
[0003] The application provides a tip catalyst layout method based on liquid bridging, which solves the problem of high equipment cost and difficulty in realizing large-area batch processing in the prior art.
[0004] The application provides a tip catalyst layout method based on liquid bridging, which includes the following steps:
[0005] S1, performing oxygen plasma surface treatment on an auxiliary substrate and a target substrate in advance;
[0006] S2, dropping a catalyst solution on the surface of the auxiliary substrate to form a catalyst solution film by rotation;
[0007] S3, dropping an auxiliary transfer liquid on the target substrate and the tip surface located on the target substrate to form an auxiliary transfer liquid film by rotation;
[0008] S4, contacting the catalyst solution film downward with the auxiliary transfer liquid film and keeping, forming a liquid bridge between the surface of the auxiliary substrate and the target substrate and the tip, and after the substrates are separated, the catalyst particles in the catalyst solution are transferred to the tip to complete the tip catalyst layout of the target substrate.
[0009] Further, the auxiliary substrate in the step S1 is a substrate with a flat surface, and the material is silicon or silicon oxide.
[0010] Further, the surface of the target substrate in step S1 has several tips and the rest is a flat substrate.
[0011] Further, the oxygen plasma surface treatment in step S1 uses a plasma activation machine with a power of 50-100 watts.
[0012] Further, the oxygen plasma surface treatment in step S1 has the following process parameters: oxygen plasma treatment time is 1-5 minutes, gas pressure is 0.1-1 Pascal, and oxygen flow is 10-30 standard cubic centimeters per minute.
[0013] Further, the material of the tip in step S3 is silicon, diamond, or other metal materials.
[0014] Further, the shape of the tip in step S3 is spherical, pyramidal, conical, or other conical, and the characteristic size of the tip is 3 nanometers-1 micrometer.
[0015] Further, the auxiliary transfer liquid in step S3 is deionized water, acetone, ethanol, or isopropyl alcohol.
[0016] Further, the rotation in steps S2 and S3 uses a spin coater or a spin coater.
[0017] Advantages
[0018] (1) High precision layout: The present application precisely transfers catalyst particles to the tips of the target substrate by liquid bridge method, which can realize high precision catalyst layout, avoid the problems of uneven distribution or misplacement of catalyst in traditional methods, and significantly improve the accuracy and reliability of catalyst layout.
[0019] (2) Simple operation: The present application uses liquid bridge technology, which is simple and easy to operate, without the need for complex equipment and cumbersome steps, reducing production cost and operation difficulty, improving production efficiency, and suitable for large-scale industrial application.
[0020] (3) High catalyst utilization rate: By precisely controlling the coating process of catalyst solution, the waste of catalyst can be minimized, the utilization rate of catalyst can be improved, the material cost can be reduced, and the environmental protection can be facilitated.
[0021] (4) Wide application range: The present application is suitable for various types of catalysts and substrate materials, such as ferritin solution as catalyst solution, and silicon wafer with thermal oxidation layer as auxiliary substrate, etc., with wide applicability, which can meet the needs of different application scenarios.
[0022] (5) Strong repeatability: By optimizing parameters such as oxygen plasma treatment time, gas pressure and oxygen flow, the present application can ensure the stability and repeatability of the catalyst layout process, guarantee the consistency of quality and effect of each layout, and be conducive to the standardization and quality control of industrial production.
[0023] (6) Reduce energy consumption: The present application can complete catalyst layout at room temperature or lower temperature without harsh conditions such as high temperature and high pressure, which can significantly reduce energy consumption compared with traditional high temperature sintering or chemical vapor deposition method, and meet the environmental protection requirements of energy saving and emission reduction.
[0024] (7) Improve equipment life: Due to the mild operating conditions, the wear of the equipment is small, which can prolong the service life of the equipment, reduce the equipment maintenance cost, and further improve the production benefit. BRIEF DESCRIPTION OF DRAWINGS
[0025] Figure 1 is a schematic diagram of dropping catalyst solution at the center of the auxiliary substrate.
[0026] Figure 2 is a schematic diagram of forming a catalyst solution film on the surface of the auxiliary substrate by rotation.
[0027] Figure 3 is a schematic diagram of forming an auxiliary transfer liquid film on the surface of the target substrate by rotation, wherein (a) is a schematic diagram of a conical tip, and (b) is a schematic diagram of a spherical tip.
[0028] Figure 4 is a schematic diagram of contacting the tip surface of the target substrate with the catalyst surface of the auxiliary substrate, wherein (a) is a schematic diagram of a conical tip, and (b) is a schematic diagram of a spherical tip.
[0029] Figure 5 is a schematic diagram of forming a liquid bridge between the surface of the auxiliary substrate and the tip of the target substrate to realize catalyst particle transfer, wherein (a) is a schematic diagram of a conical tip, and (b) is a schematic diagram of a spherical tip.
[0030] Figure 6 is a schematic diagram of successfully transferring catalyst particles to the tip of the target substrate after substrate separation, wherein (a) is a schematic diagram of a conical tip, and (b) is a schematic diagram of a spherical tip.
[0031] Figure 7 is a scanning electron microscope image of successfully transferring ferritin particles to the tip of a silicon substrate by the method of the present application. DETAILED DESCRIPTION
[0032] The application will be further described in connection with the specific embodiments. It should be understood that these embodiments are only used to illustrate the application and not used to limit the scope of the application. Furthermore, it should be understood that after reading the content of the application, those skilled in the art can make various modifications or changes to the application, and these equivalent forms also fall within the scope of the appended claims.
[0033] As a specific embodiment, a liquid bridge-based tip catalyst layout method is provided, comprising the following steps:
[0034] S1, pre-treating the auxiliary substrate 1 and the target substrate 3 with oxygen plasma surface treatment;
[0035] S2, as shown in the figure, dropping the catalyst solution 2 on the surface of the auxiliary substrate 1, and forming a catalyst solution 2 film by rotation; Figures 1-2
[0036] S3, as shown in the figure, dropping the auxiliary transfer liquid 5 on the surface of the target substrate 3 and the tip 4 located on the target substrate 3, and forming an auxiliary transfer liquid 5 film by rotation; Figure 3
[0037] S4, as shown in the figure, contacting the catalyst solution 2 film downward with the auxiliary transfer liquid 5 film and keeping, forming a liquid bridge between the surface of the auxiliary substrate 1 and the target substrate 3 and the tip 4, and after the substrate is separated, the catalyst particles 6 in the catalyst solution 2 are transferred to the tip 4, completing the tip catalyst layout of the target substrate 3. Figures 4-6
[0038] As a further technical solution, the auxiliary substrate 1 in step S1 is a silicon wafer with a thermal oxidation layer with a thickness of 500 nanometers on the surface.
[0039] As a further technical solution, the target substrate 3 in step S1 is a square silicon wafer with about 20,000 tips 4 with a height of 5-10 microns and a side length of 1.5 centimeters on the surface.
[0040] As a further technical solution, the instrument for oxygen plasma treatment in step S1 is a plasma activation machine with a power of 50-100 watts. The oxygen plasma surface treatment process parameters are: oxygen plasma treatment time is 1-5 minutes, gas pressure is 0.1-1 pascal, and oxygen flow is 10-30 standard cubic centimeters per minute.
[0041] As a further technical solution, the catalyst solution 2 in step S2 is an iron protein solution with a mass concentration of 300 milligrams per liter.
[0042] As a further technical solution, in step S2, a spin coater is used to rotate at a speed of 500 revolutions per minute for 20-30 seconds to form a uniform catalyst solution 2 film.
[0043] As a further technical solution, the shape of the tip 4 in step S3 is conical or spherical, and the characteristic size of the tip 4 is about 50-100 nanometers.
[0044] As a further technical solution, in step S3, a spin coater is used to rotate at a speed of 500 revolutions per minute for 10-20 seconds to form a uniform auxiliary transfer liquid 5 film.
[0045] As a further technical solution, the auxiliary transfer liquid 5 in step S3 is deionized water.
[0046] Example 1
[0047] 1. Fabricate target substrate 3
[0048] 1.1 Preparation of target substrate 3:
[0049] A square silicon wafer with a side length of 1.5 cm is selected as the material for the target substrate 3.
[0050] A tip 4 structure with a height of 6 microns is prepared on the surface of the silicon wafer through nanofabrication technology, with about 20,000 tips 4, designed as octagonal pyramids, with a characteristic size controlled at 50-100 nanometers.
[0051] 1.2 Selection of substrate:
[0052] According to the characterization results, silicon wafers with uniform tip height, uniform distribution, no obvious surface defects, and good tip 4 shape are selected as the target substrate 3 to ensure the quality and effect of subsequent catalyst layout.
[0053] 2. Oxygen plasma surface treatment
[0054] 2.1 Equipment preparation:
[0055] An oxygen plasma surface treatment is performed using a plasma activator with a power of 80 watts.
[0056] The target substrate 3 and the auxiliary substrate 1 (a silicon wafer with a 500-nanometer thermal oxide layer on the surface) are placed on the treatment platform of the plasma activator, respectively.
[0057] 2.2 Treatment process:
[0058] The oxygen plasma treatment time is set to 1.5 minutes, the gas pressure is 0.5 Pascal, and the oxygen flow rate is 20 standard cubic centimeters per minute.
[0059] Start the plasma activation machine and perform uniform oxygen plasma treatment on the surfaces of the target substrate 3 and the auxiliary substrate 1 to remove organic contaminants, oxide layers, and other impurities on the surfaces, while increasing the hydrophilicity and active sites of the surfaces, providing good surface conditions for the subsequent formation of the catalyst solution 2 and auxiliary transfer liquid 5 films.
[0060] 3. Preparation of catalyst solution film
[0061] 3.1 Solution preparation:
[0062] Prepare a ferritin solution with a concentration of 300 milligrams per liter as the catalyst solution 2.
[0063] 3.2 Film formation:
[0064] Place the oxygen plasma-treated auxiliary substrate 1 on the rotating platform of the spin coater, ensuring that the substrate surface is flat and perpendicular to the rotation axis.
[0065] Drop the ferritin solution onto the center of the auxiliary substrate 1, ensuring uniform distribution of the solution and no air bubbles.
[0066] Set the spin speed of the spin coater to 500 revolutions per minute and the rotation time to 25 seconds.
[0067] Start the spin coater to uniformly coat the surface of the auxiliary substrate 1 with a layer of ferritin solution film. By controlling the spin speed and rotation time, ensure that the film thickness is uniform and moderate, avoiding the film being too thick or too thin affecting the subsequent transfer effect.
[0068] 4. Preparation of auxiliary transfer liquid film
[0069] 4.2 Auxiliary transfer liquid preparation:
[0070] Use high-purity deionized water with a resistivity greater than 18 megohm-centimeters as the auxiliary transfer liquid 5.
[0071] 4.2 Film formation:
[0072] Place the oxygen plasma-treated target substrate 3 on the rotating platform of the spin coater, also ensuring that the substrate surface is flat and perpendicular to the rotation axis.
[0073] Drop the deionized water onto the center of the target substrate 3, ensuring the purity and uniformity of the deionized water.
[0074] Set the spin speed of the spin coater to 500 revolutions per minute and the rotation time to 15 seconds.
[0075] Start the spin coater to uniformly coat the surface of the target substrate 3 with a layer of deionized water film. By controlling the spin speed and rotation time, ensure that the deionized water film has a moderate thickness that can form a good liquid bridge with the catalyst solution 2 film.
[0076] 5. Catalyst particles transfer
[0077] 5.1 Contacting and liquid bridge formation:
[0078] Place the catalyst side of the auxiliary substrate 1 coated with a thin film of catalyst solution 2 face down and slowly and steadily contact the tip of the target substrate coated with a thin film of deionized water.
[0079] Maintain the contact between the auxiliary substrate 1 and the target substrate 3 for 25 seconds to ensure the formation of a stable liquid bridge between the surface of the auxiliary substrate 1 and the tip 4 of the target substrate 3.
[0080] Under the action of the liquid bridge, the catalyst particles 6 gradually transfer from the thin film of catalyst solution 2 on the auxiliary substrate 1 to the tip 4 of the target substrate 3 by capillary action and surface tension.
[0081] 6. Separation and transfer completion:
[0082] Slowly separate the auxiliary substrate 1 from the target substrate 3 and observe the distribution of catalyst particles 6 on the tip 4 of the target substrate 3.
[0083] By controlling the slow and vertical upward lifting of the auxiliary substrate 1 during the separation process, the catalyst particles 6 are prevented from falling off or unevenly distributed during the separation process, ensuring that the catalyst particles 6 are successfully and completely transferred to the tip 4 of the target substrate 3, as shown in Figure 7 .
[0084] Through the specific operation of the above embodiments, high-precision layout of catalyst particles on the tip of the target substrate can be achieved, providing high-quality catalyst carriers for subsequent catalytic reactions or other applications. The operation is simple, environmentally adaptable, has high catalyst utilization rate, wide application range, strong repeatability, and can reduce energy consumption and improve equipment life.
[0085] The above is only a preferred embodiment of the present application and is not intended to limit the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application shall be included within the scope of protection of the present application.
Claims
1. A method for deploying a tip catalyst based on liquid bridging, comprising the following steps: S1, pre-processing the auxiliary substrate (1) and the target substrate (3) with oxygen plasma; S2, adding a catalyst solution (2) dropwise onto the surface of the auxiliary substrate (1), and forming a catalyst solution (2) film by rotating; S3, dropping an auxiliary transfer liquid (5) on the surface of the target substrate (3) and the tip (4) located on the target substrate (3), and forming a thin film of the auxiliary transfer liquid (5) by rotating; S4. The catalyst solution (2) film is placed face down in contact with the auxiliary transfer liquid (5) film and maintained to form a liquid bridge between the surface of the auxiliary substrate (1) and the target substrate (3) and the tip (4). After the substrates are separated, the catalyst particles (6) in the catalyst solution (2) are transferred to the tip (4), completing the catalyst arrangement at the tip of the target substrate (3).
2. The tip catalyst deployment method based on liquid bridging according to claim 1, characterized in that: The auxiliary substrate (1) in step S1 is a substrate with a flat surface, and its material is silicon or silicon oxide.
3. The tip catalyst deployment method based on liquid bridging according to claim 1, characterized in that: The surface of the target substrate (3) in step S1 has several tips (4), and the rest is a flat substrate.
4. The tip catalyst deployment method based on liquid bridging according to claim 1, characterized in that: The oxygen plasma surface treatment in step S1 uses a plasma activation machine with a power of 50-100 watts.
5. The tip catalyst deployment method based on liquid bridging according to claim 1, characterized in that: The process parameters of the oxygen plasma surface treatment in step S1 are: oxygen plasma treatment time is 1-5 minutes, gas pressure is 0.1-1 Pascal, and oxygen flow rate is 10-30 standard cubic centimeters / minute.
6. The tip catalyst deployment method based on liquid bridging according to claim 1, characterized in that: The material of the tip (4) in step S3 is silicon, diamond or other metal materials.
7. The tip catalyst deployment method based on liquid bridging according to claim 1, characterized in that: The shape of the tip (4) in step S3 is spherical, pyramidal, conical or other conical shapes, and the characteristic size of the tip (4) is between 3 nanometers and 1 micrometer.
8. The tip catalyst deployment method based on liquid bridging according to claim 1, characterized in that: The auxiliary transfer liquid (5) in step S3 is deionized water, acetone, ethanol or isopropanol.
9. The tip catalyst deployment method based on liquid bridging according to claim 1, characterized in that: The rotation in steps S2 and S3 is performed using a spin coater or a spin coater.