Preparation device of core-shell bifunctional material
By using a core-shell bifunctional material preparation device, a uniform coating layer is formed on the material surface through a vibration module and a magnetron sputtering spraying equipment, which solves the problem of poor catalytic and adsorption effects in existing bifunctional materials and achieves significant catalytic reaction capabilities.
Patent Information
- Application Number
- CN202422948766.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-29
- Publication Date
- 2025-11-04
- Estimated Expiration
- 2034-11-29
AI Technical Summary
In existing bifunctional materials for CO2 capture and in-situ conversion to prepare high-value chemical products, the effects of adsorption sites and catalytic sites are not good, making it difficult to achieve good catalytic and adsorption effects at the same time.
A core-shell bifunctional material preparation device is used, in which the sputtered material particles are violently tumbled in the loading stage by a vibration module, and a uniform coating layer is formed on the surface by magnetron sputtering equipment to form a core-shell bifunctional material.
It improves catalytic reaction capability, adapts to existing tandem catalytic reaction systems, and significantly enhances the catalytic reaction performance of the material.
Smart Images
Figure CN223509947U_ABST
Abstract
Description
Technical Field
[0001] This application belongs to the field of chemical industry technology, and specifically relates to an apparatus for preparing core-shell bifunctional materials. Background Technology
[0002] Catalysts can alter the rate of chemical reactions of other substances, thereby increasing the rate of chemical reactions, but their own mass and chemical properties remain unchanged before and after the chemical reaction.
[0003] Catalysts play a crucial role in the development of the chemical industry and society. According to incomplete statistics, approximately 30,000 raw materials and chemical intermediates worldwide are synthesized directly or indirectly using catalysts. These materials are not only directly related to people's basic needs like food, clothing, housing, and transportation, but also involved in many modern high-tech fields, such as information transmission, network technology, aerospace, and bioengineering.
[0004] Heterogeneous solid catalysts are currently the most widely used catalysts in industry, typically comprising an active catalyst component, a co-catalyst, and a support. The preparation and pretreatment processes of catalysts play a crucial role in their properties; appropriate conditions and parameter coordination are essential for successful catalyst preparation. Commonly used catalyst preparation methods include precipitation, impregnation, ion exchange, mechanical mixing, melting, organometallic complex methods, and freeze-drying. Furthermore, many materials science preparation methods, such as sol-gel methods, co-precipitation methods, and high-temperature sol-gel decomposition methods, can be modified to prepare catalysts for wet oxidation. Co-precipitation and impregnation are the two most commonly used methods for preparing wet oxidation catalysts.
[0005] Bifunctional materials are a general term for catalysts or adsorbents that possess multiple functions. For example, a bifunctional material for CO2 capture and in-situ conversion to produce high-value chemical products consists of adsorption sites for CO2 capture and catalytic sites for CO2 hydrogenation to syngas. Existing bifunctional materials for CO2 capture and in-situ conversion to produce high-value chemical products are typically synthesized using methods such as sol-gel methods, co-precipitation methods, and high-temperature sol-gel decomposition methods. In bifunctional materials prepared in this way, the adsorption sites and catalytic sites often have different effects on each other; some result in better catalytic effects, some in worse catalytic effects, some in better adsorption effects, and many more in worse adsorption effects. Utility Model Content
[0006] This application proposes a device for preparing core-shell bifunctional materials, aiming to enable the bifunctional materials to have better catalytic reaction capabilities.
[0007] The embodiments of this application propose an apparatus for preparing core-shell bifunctional materials, comprising:
[0008] The vibration module includes a power unit, a return spring, and a vibration block. The power unit is connected to the vibration block to drive the vibration block to rotate.
[0009] A sample loading stage is provided, positioned above the vibrating block. The return spring is configured to keep the sample loading stage and the vibrating block in contact and pressed against each other.
[0010] A magnetron sputtering deposition apparatus is used to excite and eject atoms on the surface of a sputtering target by imparting incident particle energy. The sputtering target is located above a sample loading stage, and the sputtering target can sputter the material to be deposited in the sample loading stage to form a core-shell bifunctional material.
[0011] The vibrating block has protrusions on its circumference, so that when the vibrating block rotates, the protrusions can pat or knock the sample loading platform, and the sample loading platform can vibrate in the vertical direction, so that the material in the sample loading platform can bounce and roll.
[0012] In at least one possible implementation, the preparation apparatus further includes a substrate stage, the reset spring is a tension spring, one end of the tension spring is connected to the sample loading stage, and the other end of the tension spring is connected to the substrate stage. The tension provided by the tension spring keeps the sample loading stage and the vibrating block in contact and in a state of mutual compression.
[0013] In at least one possible implementation, the cross-section of the vibrating block is polygonal.
[0014] In at least one possible implementation, the vibrating block is gear-shaped.
[0015] In at least one possible implementation, the cross-section of the vibrating block is square.
[0016] In at least one possible implementation, the side length of the square is 3 to 8 centimeters.
[0017] In at least one possible implementation, the sample loading stage vibrates at an amplitude of 0.6 cm to 1.7 cm in the vertical direction.
[0018] In at least one possible implementation, the sample loading stage includes a sample pan with an opening formed in an outwardly flared shape.
[0019] In at least one possible implementation, the magnetron sputtering equipment has a sputtering power of 250 to 300 watts.
[0020] By employing the above technical solution, the particles of the sputtered material are violently tumbled in the loading stage using a vibration module. When the sputtering target is ionized and sprayed down, the particles of the sputtered material can be uniformly coated with a layer of the sputtering target, thus forming a core-shell bifunctional material. In chemical applications, the core-shell bifunctional material exhibits a more significant catalytic reaction capability due to its spatial confinement. Attached Figure Description
[0021] Figure 1 A schematic diagram of the structure of the vibrating block of the preparation apparatus for core-shell bifunctional materials according to an embodiment of this application is shown in the first position.
[0022] Figure 2 A schematic diagram of the structure of the vibrating block in the second position of the preparation apparatus for core-shell bifunctional materials according to an embodiment of this application is shown.
[0023] Explanation of reference numerals in the attached figures
[0024] 1 substrate stage
[0025] 2 Sample loading stage 21 Stabilizer 22 Sample pot
[0026] 3 Vibration Module 31 Reset Spring 32 Vibration Block 33 Rotary Shaft 34 Bearing
[0027] 100 sputtered materials
[0028] 200 Sputtering target 201 First sputtering target 202 Second sputtering target Detailed Implementation
[0029] To more clearly illustrate the above-mentioned objectives, features, and advantages of this application, specific embodiments of this application are described in detail in conjunction with the accompanying drawings in this section. Besides the embodiments described in this section, this application can also be implemented in other different ways. Those skilled in the art can make corresponding improvements, modifications, and substitutions without departing from the spirit of this application; therefore, this application is not limited to the specific embodiments disclosed in this section. The scope of protection of this application should be determined by the claims.
[0030] Magnetron sputtering is an effective method for preparing film materials in industrial applications. It is a type of physical vapor deposition (PVD). Magnetron sputtering uses high-energy particles with energies of tens of electron volts or higher to bombard a solid cathode target. This causes atoms on the target surface to gain the energy of the incident particles and be excited and ejected from the solid surface, depositing onto the substrate to form a thin film. The particles bombarding the target surface in magnetron sputtering are ions, and the process of bombarding the target surface and producing corresponding products is also called ion sputtering. Magnetron sputtering achieves the sputtering of the target material and the deposition of the thin film through ion sputtering. Compared to chemical vapor deposition (CVD), magnetron sputtering has advantages such as high sputtering rate, good film thickness uniformity, excellent film quality, ability to deposit over large areas, and applicability to a variety of materials. Compared to other physical vapor deposition techniques, such as arc plasma deposition and vacuum evaporation, it features strong adhesion, stable coating, and high deposition rate.
[0031] like Figure 1 and Figure 2 As shown, the embodiments of this application propose a preparation apparatus for core-shell bifunctional materials, which includes a vacuum chamber, a substrate stage 1, a sample loading stage 2, a vibration module 3, and a magnetron sputtering equipment.
[0032] The vacuum chamber creates a vacuum environment, and the substrate stage 1, sample loading stage 2, vibration module 3, and magnetron sputtering equipment are all located inside the vacuum chamber. The sample loading stage 2 can be connected to the substrate stage 1 via the vibration module 3, and the sample loading stage 2 can be positioned above the vibration module 3.
[0033] It is understandable that the magnetron sputtering equipment is set up in a vacuum chamber, including some of the magnetron sputtering equipment. It is possible, but not necessary, for the entire magnetron sputtering equipment to be set up in a vacuum chamber, as long as the magnetron sputtering equipment can work normally.
[0034] The vacuum chamber can be connected to a vacuum pumping system, which may include pumping equipment (such as mechanical pumps, Roots pumps, molecular pumps), detection equipment (such as resistance gauges, ionization gauges, and diaphragm gauges), and safety valves.
[0035] Magnetron sputtering equipment is located in a vacuum environment and has the following advantages.
[0036] (1) Removal of impurities: A vacuum environment can effectively remove impurities in the air, such as oxygen, nitrogen, and water vapor. These impurities will react with the target material 200 and the sputtered material 100, affecting the quality and performance of the sputtering. By drawing a vacuum, a high-purity environment can be formed, resulting in better purity and stability of the coating.
[0037] (2) Improved sputtering efficiency: In a vacuum environment, ions move more freely and are not affected by air resistance, enabling them to impact the target material 200 with higher speed and energy. This not only improves sputtering efficiency but also reduces ion scattering and collisions, thereby increasing ion utilization.
[0038] (3) Controlling coating parameters: A vacuum environment is beneficial for precisely controlling parameters such as air pressure, temperature, and power during the coating process. By adjusting these parameters, precise control over the coating thickness, composition, and structure can be achieved, thereby improving the quality and performance of the coating.
[0039] The sample loading stage 2 may include a stabilizing block 21 and a sample pot 22. The sample pot 22 may be connected above the stabilizing block 21, and the opening of the sample pot 22 may be formed in an outwardly flared funnel shape. The sample pot 22 is used to hold particulate sputtered material 100. For ease of understanding, Figure 1 and Figure 2 An example is shown where a portion of the sputtered material 100 is significantly higher than the sample pan 22.
[0040] A sputtering target 200 can be placed above the sample loading stage 2. The magnetron sputtering equipment is used to enable the atoms on the surface of the sputtering target 200 to obtain incident particle energy and be excited and ejected.
[0041] Multiple sputtering targets 200 can be provided, and the spraying directions of the multiple sputtering targets 200 can be different. The sputtering targets 200 can include a first sputtering target 201 and a second sputtering target 202. The first sputtering target 201 and the second sputtering target 202 can face different directions, so that the sputtering targets 200 can be sprayed onto the sputtered material 100 from different angles.
[0042] The vibration module 3 may include a power unit, a return spring 31, a vibration block 32, a rotating shaft 33, and a bearing 34.
[0043] The rotating shaft 33 can be connected to a power unit, which can be a motor. The vibrating block 32 can be fixedly connected to the rotating shaft 33, and the vibrating block 32 can be rotated with the rotating shaft 33 by being driven by the power unit. The substrate stage 1 can be provided with a bracket, and the rotating shaft 33 and / or the vibrating block 32 can be rotatably connected to the bracket of the substrate stage 1 through a bearing 34, so that the vibrating block 32 and the rotating shaft 33 can rotate relative to the substrate stage 1.
[0044] The return spring 31 can be configured to keep the stabilizing block 21 and the vibrating block 32 in contact and pressed against each other. Specifically, the stabilizing block 21 of the sample loading stage 2 can be connected to the substrate stage 1 by multiple (e.g., four) return springs 31. The return springs 31 can be tension springs, with one end connected to the stabilizing block 21 and the other end connected to the substrate stage 1. The tension provided by the return springs 31 can keep the stabilizing block 21 and the vibrating block 32 in contact and pressed against each other.
[0045] The vibrating block 32 can be cylindrical, with its circumferential surface designed to contact the stabilizing block 21. The circumferential surface of the vibrating block 32 may have protrusions, allowing it to tap or strike the stabilizing block 21 as the vibrating block 32 rotates. Rotating the vibrating block 32 to different positions allows the sample loading stage 2 to reach different heights. When the vibrating block 32 rotates, its protrusions push the sample loading stage 2 upwards, and the return spring 31 limits the upward displacement of the sample loading stage 2. Then, when the protrusions of the vibrating block 32 leave the stabilizing block 21, the sample loading stage 2 can move downwards to reset under the action of the return spring 31. The continuous tapping of the vibrating block 32 on the sample loading stage 2 applies an impact force to the particles inside the sample container 22, causing the particles to bounce and tumble continuously.
[0046] Optionally, the vibrating block 32 can be gear-shaped.
[0047] Optionally, the cross-section of the vibrating block 32 can be polygonal, and further, the number of sides of the polygonal cross-section of the vibrating block 32 can be 3 to 10.
[0048] Furthermore, the cross-section of the vibrating block 32 can be square, with a side length of 3 to 8 centimeters, and the vibrating block 32 can be a cube. The rotation shaft 33 can be connected to the center of the side of the vibrating block 32. It can be understood that the vibration amplitude of the sample loading stage 2 is half the difference between the side length and the diagonal of the vibrating block 32. For example, the vibration amplitude of the sample loading stage 2 in the vertical direction can be 0.6 centimeters to 1.7 centimeters.
[0049] The vibration module 3 causes the particles of the sputtered material 100 to tumble violently in the loading stage. When the sputtering target 200 is ionized and sprayed down, the particles of the sputtered material 100 can be uniformly coated with a layer of sputtering target 200, thus forming a core-shell bifunctional material. In chemical applications, the core-shell bifunctional material exhibits a more significant catalytic reaction capability due to its spatial confinement.
[0050] The embodiments of this application propose a method for preparing a core-shell bifunctional material.
[0051] S1: The particulate sputtered material 100 is loaded in the sample loading stage 2 and repeatedly impacts the bottom of the sample loading stage 2, so that the sample loading stage 2 can vibrate in the up and down direction, causing the sputtered material 100 in the sample loading stage 2 to bounce and roll continuously.
[0052] S2: The vacuum chamber is evacuated, and the sputtering target 200 is bombarded with high-energy particles. This causes the atoms on the surface of the sputtering target 200 to gain the energy of the incident particles and be excited and ejected from the surface of the sputtering target 200, and deposited on the surface of the sputtered material 100. A coating layer of the sputtering target 200 is uniformly deposited on the surface of the particulate sputtered material 100.
[0053] The resulting core-shell bifunctional material exhibits a significant coating structure and spatial confinement effect, enabling it to adapt to existing tandem catalytic reaction systems.
[0054] Optionally, the particle size (diameter) of the sputtered material 100 can be between 250 and 450 micrometers. Such a particle size allows the core-shell bifunctional material manufactured in this application to be directly used in chemical catalysis.
[0055] Optionally, the rotational speed of the rotating shaft 33 can be 20 to 50 revolutions per minute (RPM).
[0056] Optionally, the frequency at which the vibrating block 32 taps or strikes the sample loading stage 2 can be 80 to 200 times per minute. This allows the sputtered material 100 to tumble violently without being shaken out of the sample loading stage 2.
[0057] The device that uses high-energy particles to bombard the sputtering target is a magnetron sputtering spraying equipment with a spraying power of 250 to 300 watts and a spraying time of 30 to 120 minutes. This enables successful ignition and release of the ionized sputtering target 200, and allows the sputtering target 200 to be uniformly deposited on the surface of the sputtered material 100 to form a coating structure.
[0058] Optionally, the sputtered material 100 can be a mixture of calcium and aluminum, and the sputtering target 200 can be a metal, such as iron.
[0059] The plating opening can be referred to as the valve opening. The pressure in the vacuum chamber and the deposition pressure can be controlled by the size of the valve opening and the argon flow rate.
[0060] The deposition rate plays a crucial role in the growth of catalyst metals on the surface of core-shell materials. Specifically, the deposition rate determines the energy of the particles, which in turn determines the crystal phase, chemical composition, and so on of the atoms deposited on the material surface. Ultimately, it also affects the distribution morphology of the metal, the formation of defect sites, and the crystal structure.
[0061] In this application, the deposition rate can be 2 to 3.2 angstroms per second, and the argon flow rate can be 10 to 60 standard cubic centimeters per minute (sccm).
[0062] Table 1 lists three sets of optional preparation parameters for preparing Ca-Fe (a mixture of calcium and aluminum cores with iron surface) core-shell bifunctional materials.
[0063] Table 1
[0064]
[0065]
[0066] It should be understood that at least some aspects or features of the above-described implementation methods, embodiments, or examples can be appropriately combined.
[0067] It is understood that, in this application, when the number of parts or components is not specifically limited, the number can be one or more, where multiple refers to two or more. For cases where the number of parts or components shown in the drawings and / or described in the specification is, for example, two, three, four, etc., this specific number is generally exemplary and not restrictive, and can be understood as multiple, i.e., two or more; however, this does not mean that this application excludes the case of one.
[0068] In this application, unless otherwise expressly stated or limited, terms such as "installation," "assembly," "connection," "linking," "joining," "linking," "abutment," "communication," "connection," "conduction," "fixing," and "fastening" should be interpreted broadly, for example, they can be direct or indirect. For instance, regarding connection, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium; it can be the internal communication of two components or the interaction between two components, unless otherwise expressly stated or limited. For instance, regarding communication / conduction, it can be direct communication / conduction or indirect communication / conduction through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.
[0069] In this application, unless otherwise expressly stated or limited, a component being disposed / installed / located / enclosed / placed within, inside, or incorporated in another component can be either of the following two situations: a portion or a majority of the one component is located within the other component; or the one component is completely enclosed within the other component.
[0070] Although the present application has been described in detail using the above embodiments, it will be apparent to those skilled in the art that the present application is not limited to the embodiments described herein. The present application can be modified and implemented as alternative embodiments without departing from the spirit and scope of the present application as defined by the claims. Therefore, the description in this specification is for illustrative purposes only and does not have any limiting meaning for the present application.
Claims
1. An apparatus for preparing core-shell bifunctional materials, characterized in that, include: The vibration module includes a power unit, a return spring, and a vibration block. The power unit is connected to the vibration block to drive the vibration block to rotate. A sample loading stage is provided, positioned above the vibrating block. The return spring is configured to keep the sample loading stage and the vibrating block in contact and pressed against each other. A magnetron sputtering deposition apparatus is used to excite and eject atoms on the surface of a sputtering target by imparting incident particle energy. The sputtering target is located above a sample loading stage, and the sputtering target can sputter the material to be deposited in the sample loading stage to form a core-shell bifunctional material. The vibrating block has protrusions on its circumference, so that when the vibrating block rotates, the protrusions can pat or knock the sample loading platform, and the sample loading platform can vibrate in the vertical direction, so that the material in the sample loading platform can bounce and roll.
2. The apparatus for preparing core-shell bifunctional materials according to claim 1, characterized in that, The preparation apparatus also includes a substrate stage, and the reset spring is a tension spring. One end of the tension spring is connected to the sample loading stage, and the other end of the tension spring is connected to the substrate stage. The tension provided by the tension spring keeps the sample loading stage and the vibrating block in contact and in a state of mutual compression.
3. The apparatus for preparing core-shell bifunctional materials according to claim 1, characterized in that, The cross-section of the vibrating block is polygonal.
4. The apparatus for preparing core-shell bifunctional materials according to claim 1, characterized in that, The vibrating block is gear-shaped.
5. The apparatus for preparing core-shell bifunctional materials according to claim 1, characterized in that, The cross-section of the vibrating block is square.
6. The apparatus for preparing core-shell bifunctional materials according to claim 5, characterized in that, The side length of the square is 3 to 8 centimeters.
7. The apparatus for preparing core-shell bifunctional materials according to claim 1, characterized in that, The vertical vibration amplitude of the sample loading stage is 0.6 cm to 1.7 cm.
8. The apparatus for preparing core-shell bifunctional materials according to claim 1, characterized in that, The sample loading stage includes a sample pot, the opening of which is formed in an outwardly flared funnel shape.
9. The apparatus for preparing core-shell bifunctional materials according to claim 1, characterized in that, The magnetron sputtering equipment has a sputtering power of 250 to 300 watts.