Manufacturing Process of a Metal Matrix Ceramic Flow Reactor with Diffusion Welding Performance

Abstract

The present invention discloses a manufacturing process of a metal-based ceramic flow channel reactor with diffusion welding performance, which relates to the technical field of metal-based ceramic flow channel reactors and includes pretreatment. Through pretreatment, organic solvents are used to clean the surfaces of metals and ceramics, and acidic solutions are used to remove the oxides on the metal surfaces. Mechanical equipment is used to polish the metal surfaces to obtain flat and clean surfaces. In the present invention, a clean cloth is dipped in an appropriate amount of acetone solvent and gently wiped on the surfaces of stainless steel and zirconia. The oxides on the surface of 316L stainless steel are removed by an acidic solution, and a grinding machine is used to level and clean the surface of 316L stainless steel, so that the pretreatment can improve the welding quality and the reliability of bonding.

Description

Technical Field

[0001] The present invention relates to the technical field of manufacturing metal-based ceramic flow reactors, and specifically to a manufacturing process for metal-based ceramic flow reactors with diffusion welding performance. Background Art

[0002] A metal-based ceramic flow reactor is a special device used in the fields of chemical engineering and chemical reactions. A metal-based ceramic flow reactor is an important device for performing high-temperature and corrosive reactions in a harsh chemical environment. It has high-temperature tolerance, corrosion resistance, and abrasion resistance, and is mainly applied to petrochemical plants, chemical reaction facilities, high-temperature smelting processes, and other industrial applications that require high-temperature and corrosion-resistant properties. The manufacturing process for metal-based ceramic flow reactors with diffusion welding performance provided by the present invention can better pre-treat metal-based materials and ceramic materials, thereby improving the welding quality and joint reliability. By optimizing the coating, the quality of the ceramic coating can be improved. By preheating and soaking, the stability of diffusion welding can be improved. By curing and cooling, the problem of improving the strength of the welding can be solved.

[0003] The defects of existing metal-based ceramic flow reactors are as follows:

[0004] 1. In patent document US20210143120A1, preform diffusion welding is disclosed, which mainly considers that the solder preform can be melted and completely react with the metal regions of the semiconductor die and the substrate, without considering the problem of how to improve the welding quality and joint reliability;

[0005] 2. In patent document JP2020518456A, a solder preform for diffusion welding, its manufacturing method, and its assembly method are disclosed, which mainly consider forming at low cost and with improved processing capabilities, without considering the problem of how to improve the quality of the ceramic coating;

[0006] 3. In patent document CN111153386B, a methanol reforming hydrogen production reactor with a honeycomb structure silicon carbide ceramic is disclosed, which mainly considers the problems of improving the catalyst loading capacity, reducing pressure loss, and increasing the reaction area, without considering the problem of how to improve the stability of diffusion welding;

[0007] 4. In patent document CN110801785B, a hydrogen production reactor with a honeycomb SiC ceramic as a catalyst carrier is disclosed, which mainly considers improving the directivity and flow uniformity of fluid flow, having characteristics such as high thermal conductivity, good thermal stability, stable chemical properties, and large specific surface area, improving the mass transfer and heat transfer performance in the reactor, reducing the pressure loss in the reactor, and enhancing the catalyst loading capacity, without considering the problem of how to improve the strength of the welding. Summary of the Invention

[0008] The object of the present invention is to provide a manufacturing process for a metal-based ceramic flow channel reactor with diffusion welding performance, so as to solve the problems raised in the above-mentioned background technology.

[0009] To achieve the above object, the present invention provides the following technical solution: a manufacturing process for a metal-based ceramic flow channel reactor with diffusion welding performance, the manufacturing process of the metal-based ceramic flow channel reactor includes the following steps:

[0010] Step S1, material selection: select 316L stainless steel and zirconia ceramics;

[0011] Step S2, pretreatment: cut, process and clean the 316L stainless steel;

[0012] Step S3, spray the ceramic layer;

[0013] Step S4, diffusion welding: use a resistance furnace to control parameters for the diffusion welding machine to work;

[0014] Step S5, cooling and solidification: cool the welding area and perform the solidification step;

[0015] Step S6, inspection and quality control: perform non-destructive inspection on the welded connection and conduct quality control tests;

[0016] Step S7, post-treatment: perform surface coating or treatment on the manufactured flow channel reactor and conduct final assembly;

[0017] Step S8, testing and verification: perform performance testing and verification before actual use;

[0018] Clean the metal and ceramic surfaces using organic solvents, remove the oxides on the metal surface by using an acidic solution, and polish the metal surface using mechanical equipment to obtain a flat and clean surface for improving the quality of bonding. Spray a special coating on the metal surface in advance to improve the diffusion welding performance.

[0019] Preferably, the manufacturing process of the metal-based ceramic flow channel reactor further includes the following steps:

[0020] Step S11, clarify the usage environment and performance requirements of the reactor, select 316L stainless steel as the metal-based material, select zirconia ceramics as the ceramic spraying material, and conduct laboratory tests and sample preparation on the 316L stainless steel and zirconia ceramics;

[0021] Among them, 316L stainless steel has excellent corrosion resistance, suitable mechanical properties and good welding performance, and its basic parameters are:

[0022] Coefficient of thermal expansion: The coefficient of thermal expansion of 316L stainless steel is 16.5×10^-6 / °C (at 60°C);

[0023] Temperature range: The operating temperature range of 316L stainless steel is between -196°C and 800°C;

[0024] Among them, zirconia ceramics have high strength and wear resistance. The hardness of zirconia ceramics is very high, above HRA85, and can even reach above HRA 90, thus having excellent wear resistance. In addition, zirconia ceramics are also excellent insulating materials, with good corrosion resistance and transparency to acidic and alkaline environments;

[0025] Tensile strength: The tensile strength of zirconia ceramics is between 200 MPa and 1000 MPa;

[0026] Coefficient of thermal expansion: The coefficient of thermal expansion of zirconia ceramics is 10.5×10^-6 / °C (at 60°C);

[0027] Laboratory tests include:

[0028] (1) Diffusion welding test;

[0029] (2) Measurement of coefficient of thermal expansion.

[0030] Preferably, the manufacturing process of the metal matrix ceramic flow reactor further includes the following steps:

[0031] Step S21: During the pretreatment process, it is necessary to design and manufacture the metal matrix, and the shape and structure of the metal matrix need to meet the design requirements of the reactor.

[0032] Preferably, the manufacturing process of the metal matrix ceramic flow reactor further includes the following steps:

[0033] Step S31: Use thermal spraying technology to spray zirconia ceramics on the inner surface of the 316L stainless steel reaction flow channel, optimize the wettability between the coating and the substrate, and strictly control the temperature and environmental conditions during the coating and curing process, and perform appropriate curing and annealing processes;

[0034] Coating wetting:

[0035] (1) Temperature control: The working temperature needs to be between 2700°C and 2900°C;

[0036] (2) Adding an interface treatment agent: Add a surfactant to improve the interaction and wetting performance between the coating and the substrate;

[0037] (3) Optimizing the coating thickness: Control the thickness of the coating;

[0038] Among them, the curing and annealing process:

[0039] Put the 316L stainless steel reaction flow channel together with the zirconia ceramic coating into a high-temperature furnace. Set the temperature of the high-temperature furnace between 2700 °C and 2750 °C, with a curing time of 2 hours. Use the heat treatment process to heat the coating and the substrate together and then cool them to improve the performance of the coating. During the curing process, control different atmospheres to affect the performance of the ceramic coating. Then, lower the temperature of the high-temperature furnace to 500 °C for annealing. After curing and annealing are completed, the coating needs to be cooled to room temperature, and then inspection work is carried out on the coating.

[0040] Preferably, the manufacturing process of the metal-based ceramic flow channel reactor further includes the following steps:

[0041] Step S41, preheating and soaking: Preheat before welding to reduce the thermal stress of the material and ensure uniform preheating to prevent material deformation;

[0042] Set the preheating temperature of the high-temperature furnace between 150 °C and 300 °C, and use a thermometer to ensure the accuracy of the preheating temperature. When the preheating temperature reaches 300 °C, control the temperature of the high-temperature furnace to maintain the same temperature for soaking treatment;

[0043] Control the welding environment: Ensure the stability of the welding environment and avoid oxygen, moisture or other contaminants from entering the welding area;

[0044] It is necessary to ensure that the argon in the atmosphere is of high purity, ensure that the oxygen content in the welding environment is extremely low, and use an atmosphere analyzer and temperature control equipment to continuously monitor and record the parameters of the welding environment;

[0045] Step S42, after spraying the ceramic layer, diffusion welding is required. Assemble the stainless steel workpieces to be welded into the required shape and position. Coat molybdenum powder on the surface to be welded. Put the stainless steel workpieces and the parts coated with metal powder into a high-temperature furnace. Set the temperature of the high-temperature furnace between 1000 °C and 1100 °C. The pressure application equipment in the high-temperature furnace applies pressure to the stainless steel. During the heating process, the molybdenum powder begins to melt and diffuse into the stainless steel substrate to form a strong welded joint. After the process of molybdenum powder diffusion is completed, cool the workpiece to room temperature, and then perform post-treatment steps to achieve the required shape and surface quality through cutting and polishing.

[0046] Preferably, the manufacturing process of the metal-based ceramic flow channel reactor further includes the following steps:

[0047] Step S51, after diffusion welding is completed, determine the appropriate curing temperature and time. At the same time, ensure that the welding area is in an appropriate atmosphere, control the progressive cooling rate to avoid rapid cooling and the phenomenon of alternating hot and cold. Detection is required after curing, and record the curing parameters and results;

[0048] Curing detection:

[0049] (1) Hardness test: Test the welded position through Brinell hardness test;

[0050] Among them, the calculation formula of Brinell hardness value is:

[0051] HB = F / (D*d), where F is the test force, D is the diameter of the steel ball, and d is the diameter of the indentation;

[0052] (2) Microstructure analysis;

[0053] Analysis of the metal part: Use an optical microscope to observe the microstructure of the metal part, and determine the size and orientation of stainless steel grains through X-ray diffraction analysis;

[0054] Analysis of the ceramic part: Use X-ray diffraction analysis or electron diffraction to determine the ceramic crystal structure, use a microscope and image analysis to measure the porosity in the ceramic, and analyze the composition and structure of the ceramic through Raman spectroscopy;

[0055] Interface analysis: Use a high-resolution scanning electron microscope and energy spectrum analysis to analyze the chemical composition and structure of the interface;

[0056] (3) Visual inspection.

[0057] Preferably, the manufacturing process of the metal matrix ceramic flow channel reactor further includes the following steps:

[0058] Step S61: In the manufacturing process of the microchannel reactor by thermal spraying ceramic materials on the surface of 316L stainless steel, a series of process detections and quality controls are required to ensure its diffusion welding performance;

[0059] Raw material inspection: Check 316L stainless steel through chemical analysis and mechanical property tests. At the same time, conduct composition analysis and structure analysis on the ceramic material;

[0060] Welding process control: Monitor and record the temperature, time, and pressure during welding;

[0061] Non-destructive testing: Detect pores in the weld by using ultrasonic equipment, detect cracks and slag inclusions in the weld by using X-ray and Y-ray detection equipment, and detect cracks and fatigue on the weld and surface by using eddy current detection equipment.

[0062] Preferably, the manufacturing process of the metal matrix ceramic flow channel reactor further includes the following steps:

[0063] Step S71. The subsequent treatment is to ensure excellent diffusion welding performance and meet the requirements of specific applications. Regularly conduct weld inspections on the diffusion welded joints, eliminate residual stress and improve the material properties through heat treatment. During the subsequent treatment process, strict quality control is required, and performance tests are carried out. Assemble and seal the metal matrix ceramic reactor;

[0064] Among them, the performance tests include:

[0065] (1) Pressure test;

[0066] (2) Temperature cycle test;

[0067] (3) Chemical stability test.

[0068] Preferably, the manufacturing process of the metal matrix ceramic flow reactor further includes the following steps:

[0069] Step S81. Among them, the test and verification methods, in addition to welding quality test, material property test and ceramic coating test, also include the following test methods:

[0070] (1) Verification of heat treatment effect;

[0071] (2) Diffusion performance test;

[0072] (3) Sealing performance test;

[0073] (4) Chemical stability test;

[0074] (5) Performance simulation test;

[0075] (6) Standard compliance test;

[0076] (7) Durability test;

[0077] These test and verification steps help to ensure the manufacturing quality of the metal matrix ceramic flow reactor and ensure its excellent diffusion welding performance in practical applications.

[0078] Compared with the prior art, the beneficial effects of the present invention are:

[0079] 1. The present invention uses a cleaning cloth to dip an appropriate amount of acetone solvent, gently wipe the surfaces of stainless steel and zirconia, use a brush to handle the details, wipe the surface with a clean dry cloth to ensure the removal of residual organic solvents, use gas purging to ensure the surface is completely dry, check whether the surface is completely clean and there is no residual grease or dirt, and it is necessary to ensure that there is no residue on the cleaned surface that affects its performance and application. Remove the oxide on the surface of 316L stainless steel through an acidic solution, perform leveling and cleaning work on the surface of 316L stainless steel by using a grinding machine, use molybdenum powder to improve the performance of diffusion welding, adjust the temperature of the diffusion welding machine to 2900 °C, the pressure to 60 MPa, and the time to 2 hours, so that the pretreatment can improve the welding quality and the reliability of the joint.

[0080] 2. The present invention sprays zirconia ceramics on the inner surface of the 316L stainless steel reaction flow channel by using thermal spraying technology, optimizes the wettability between the coating and the substrate. During the coating and curing process, strictly control the temperature and environmental conditions. Put the 316L stainless steel reaction flow channel and the zirconia ceramic coating into a high-temperature furnace together, set the temperature of the high-temperature furnace between 2700 °C and 2750 °C, and the curing time is 2 hours. Use the heat treatment process to heat the coating and the substrate together and then cool to improve the performance of the coating. During the curing process, control different atmospheres to affect the performance of the ceramic coating, and then reduce the temperature of the high-temperature furnace to 500 °C for annealing work. After the curing and annealing are completed, the coating needs to be cooled to room temperature, and then inspection work is carried out on the coating, so as to improve the quality of the ceramic coating.

[0081] 3. The present invention preheats before welding. Preheating is the process of heating the workpiece to a certain temperature before the start of the welding process, which is used to reduce the thermal stress of the material, ensure uniform preheating to prevent material deformation. Set the preheating temperature of the high-temperature furnace between 150 °C and 300 °C, and use a thermometer to ensure the accuracy of the preheating temperature, so as to reduce the impact of welding heat on the workpiece, avoid deformation and cracks caused by thermal stress, and at the same time promote the diffusion process. When the preheating temperature reaches 300 °C, control the temperature of the high-temperature furnace to maintain at the same temperature for homogenization heat treatment. Control the welding environment: ensure the stability of the welding environment, avoid oxygen, moisture or other pollutants from entering the welding area, and it is necessary to ensure that the argon in the atmosphere is of high purity, ensure that the oxygen content in the welding environment is extremely low, and use an atmosphere analyzer and temperature control equipment to continuously monitor and record the parameters of the welding environment, so as to improve the stability of diffusion welding.

[0082] 4. The present invention determines appropriate curing temperature and time, with the temperature being 300 °C and the time being 2 hours. A protective atmosphere is used to prevent oxidation. In addition, the curing area is ensured to be dry to prevent moisture introduction. The internal stress of the material is reduced by a gradual cooling rate. The curing parameters and results are recorded through hardness testing, microstructure analysis, and visual inspection of the cermet joint for tracking and quality control, which is conducive to subsequent quality assurance and problem troubleshooting. It is necessary to ensure that the furnace or equipment used for curing is in good condition to ensure the accuracy of temperature and time, thereby improving the welding strength. BRIEF DESCRIPTION OF THE DRAWINGS

[0083] Figure 1 is a flow chart of the present invention;

[0084] Figure 2 is a detailed flow chart of the detection and quality control of the present invention;

[0085] Figure 3 is a detailed flow chart of the testing and verification of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0086] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0087] Embodiment 1:

[0088] Please refer to Figure 1 , a manufacturing process for a metal-based ceramic flow reactor with diffusion welding performance, including step S1, material selection: 316L stainless steel and zirconia ceramics are selected;

[0089] Step S11, clarify the usage environment and performance requirements of the reactor, select 316L stainless steel as the metal-based material and zirconia ceramics as the ceramic spraying material, and conduct laboratory tests and sample preparations on 316L stainless steel and zirconia ceramics;

[0090] Among them, 316L stainless steel has excellent corrosion resistance, appropriate mechanical properties, and good welding performance. Its basic parameters are:

[0091] Coefficient of thermal expansion: The coefficient of thermal expansion of 316L stainless steel is 16.5×10^-6 / °C (at 60 °C);

[0092] Temperature range: The working temperature range of 316L stainless steel is between -196 °C and 800 °C;

[0093] Among them, zirconia ceramics have high strength and wear resistance. The hardness of zirconia ceramics is very high, above HRA 85, and can even reach above HRA 90, thus having excellent wear resistance. In addition, zirconia ceramics are also excellent insulating materials, with good corrosion resistance and transparency to acidic and alkaline environments;

[0094] Tensile strength: The tensile strength of zirconia ceramics is between 200 MPa and 1000 MPa;

[0095] Coefficient of thermal expansion: The coefficient of thermal expansion of zirconia ceramics is 10.5×10^-6 / °C (at 60°C);

[0096] Laboratory tests include:

[0097] (1) Diffusion welding test;

[0098] (2) Measurement of coefficient of thermal expansion;

[0099] Select materials according to the service environment and performance requirements of the reactor. Its mechanical strength, corrosion resistance, thermal conductivity, and coefficient of thermal expansion need to be considered. When selecting a ceramic coating, the chemical stability, thermal stability, and wear resistance of the ceramic material need to be considered, so as to protect the metal matrix from corrosion, high temperature, and wear. Therefore, 316L stainless steel and zirconia ceramics are selected. When coating the ceramic onto the metal matrix, adhesion and curing materials are required.

[0100] Example two:

[0101] Please refer to Figure 1 , a manufacturing process for a metal matrix ceramic flow channel reactor with diffusion welding performance, including step S2, pretreatment: cutting, processing, and cleaning 316L stainless steel;

[0102] Clean the surfaces of the metal and ceramic using organic solvents, remove the oxides on the metal surface by using an acidic solution, and polish the metal surface using mechanical equipment to obtain a flat and clean surface for improving the bonding quality. Spray a special coating on the metal surface in advance to improve the diffusion welding performance;

[0103] Step S21, during the pretreatment process, it is necessary to design and manufacture the metal matrix. The shape and structure of the manufactured metal matrix need to meet the design requirements of the reactor;

[0104] By using a cleaning cloth dipped in an appropriate amount of acetone solvent, gently wipe the surfaces of stainless steel and zirconia. Use a brush to handle the details, and then wipe the surface with a clean dry cloth to ensure the removal of residual organic solvents. Use gas purging to ensure the surface is completely dry. Check whether the surface is completely clean and free of residual grease or dirt. It is necessary to ensure that there are no residues on the cleaned surface that may affect its performance and application. Remove the oxides on the surface of 316L stainless steel through an acidic solution. Carry out leveling and cleaning work on the surface of 316L stainless steel by using a grinding machine. Use molybdenum powder to improve the performance of diffusion welding. Adjust the temperature of the diffusion welding machine to 2900 °C, the pressure to 60 MPa, and the time to 2 hours, so that the pretreatment can improve the welding quality and the reliability of the joint.

[0105] Example 3:

[0106] Please refer to Figure 1 , a manufacturing process for a metal-based ceramic flow reactor with diffusion welding performance, including step S3, spraying a ceramic layer;

[0107] Step S31: Use thermal spraying technology to spray zirconia ceramics on the inner surface of the 316L stainless steel reaction flow channel, optimize the wettability between the coating and the substrate. During the coating and curing process, strictly control the temperature and environmental conditions, and carry out appropriate curing and annealing processes;

[0108] Coating wetting:

[0109] (1) Temperature control: The working temperature should be between 2700 °C and 2900 °C;

[0110] (2) Add an interface treatment agent: Add a surfactant to improve the interaction and wetting performance between the coating and the substrate;

[0111] (3) Optimize the coating thickness: Control the thickness of the coating;

[0112] Among them, the curing and annealing process:

[0113] Put the 316L stainless steel reaction flow channel and the zirconia ceramic coating into a high-temperature furnace together. Set the temperature of the high-temperature furnace between 2700 °C and 2750 °C, and the curing time is 2 hours. Use a heat treatment process to heat the coating and the substrate together, and then cool to improve the performance of the coating. During the curing process, control different atmospheres to affect the performance of the ceramic coating. Then reduce the temperature of the high-temperature furnace to 500 °C for annealing work. After the curing and annealing are completed, the coating needs to be cooled to room temperature, and then inspection work is carried out on the coating;

[0114] By using thermal spraying technology, zirconia ceramics are sprayed on the inner surface of the 316L stainless steel reaction flow channel to optimize the wettability between the coating and the substrate. During the coating and curing process, the temperature and environmental conditions are strictly controlled. The 316L stainless steel reaction flow channel and the zirconia ceramic coating are placed in a high-temperature furnace together. The temperature of the high-temperature furnace is set between 2700 °C and 2750 °C, and the curing time is 2 hours. Using the heat treatment process, the coating and the substrate are heated together and then cooled to improve the performance of the coating. During the curing process, different atmospheres are controlled to affect the performance of the ceramic coating. Then, the temperature of the high-temperature furnace is reduced to 500 °C for annealing. After curing and annealing are completed, the coating needs to be cooled to room temperature, and then the coating is inspected, so as to improve the quality of the ceramic coating.

[0115] Example 4:

[0116] Please refer to Figure 1 , a manufacturing process for a metal matrix ceramic flow reactor with diffusion welding performance, including step S4, diffusion welding: using a resistance furnace to control parameters for diffusion welding work;

[0117] Step S41, preheating and soaking: Preheating is carried out before welding to reduce the thermal stress of the material and ensure uniform preheating to prevent material deformation;

[0118] The preheating temperature of the high-temperature furnace is set between 150 °C and 300 °C, and a thermometer is used to ensure the accuracy of the preheating temperature. When the preheating temperature reaches 300 °C, the temperature of the high-temperature furnace is controlled to be maintained at the same temperature for soaking treatment;

[0119] Control the welding environment: Ensure the stability of the welding environment and avoid oxygen, moisture or other contaminants from entering the welding area;

[0120] It is necessary to ensure that the argon in the atmosphere is of high purity, ensure that the oxygen content in the welding environment is extremely low, and use an atmosphere analyzer and temperature control equipment to continuously monitor and record the parameters of the welding environment;

[0121] After spraying the ceramic layer in step S42, diffusion welding is required. The stainless steel workpieces to be welded are assembled into the required shape and position, molybdenum powder is coated on the surface to be welded, and the stainless steel workpieces and the parts coated with metal powder are placed in a high-temperature furnace. The temperature of the high-temperature furnace is set between 1000 °C and 1100 °C. The pressure application equipment in the high-temperature furnace applies pressure to the stainless steel. During the heating process, the molybdenum powder begins to melt and diffuse into the stainless steel substrate to form a strong welded joint. After the diffusion process of the molybdenum powder is completed, the workpiece is cooled to room temperature, and then post-treatment steps are carried out to achieve the required shape and surface quality through cutting and polishing;

[0122] By preheating before welding, where preheating is the process of heating the workpiece to a certain temperature before the start of the welding process, used to reduce the thermal stress of the material, ensure uniform preheating to prevent material deformation, set the preheating temperature of the high-temperature furnace between 150°C and 300°C, and use a thermometer to ensure the accuracy of the preheating temperature, thus being able to reduce the impact of welding heat on the workpiece, avoid deformation and cracks caused by thermal stress, and at the same time promote the diffusion process. When the preheating temperature reaches 300°C, control the high-temperature furnace to maintain the same temperature for homogenization heat treatment, control the welding environment: ensure the stability of the welding environment, avoid oxygen, moisture or other contaminants from entering the welding area, ensure that the argon in the atmosphere is of high purity, ensure that the oxygen content in the welding environment is extremely low, and use an atmosphere analyzer and temperature control equipment to continuously monitor and record the parameters of the welding environment, thereby being able to improve the stability of diffusion welding.

[0123] Example Five:

[0124] Please refer to Figure 1 、 Figure 2 and Figure 3 , a manufacturing process for a metal-based ceramic flow reactor with diffusion welding performance, including step S5, cooling and curing: cool the welding area and perform the curing step;

[0125] Step S51: After the diffusion welding is completed, determine the appropriate curing temperature and time. At the same time, ensure that the welding area is in an appropriate atmosphere, control the gradual cooling rate to avoid rapid cooling and the phenomenon of alternating hot and cold. Detection is required after curing, and record the curing parameters and results;

[0126] Curing detection:

[0127] (1) Hardness test: Test the welded position through Brinell hardness test;

[0128] Among them, the calculation formula for the Brinell hardness value is:

[0129] HB = F / (D*d), where F is the test force, D is the diameter of the steel ball, and d is the diameter of the indentation;

[0130] (2) Microstructure analysis;

[0131] Analysis of the metal part: Use an optical microscope to observe the microstructure of the metal part, and determine the size and orientation of stainless steel grains through X-ray diffraction analysis;

[0132] Analysis of the ceramic part: Use X-ray diffraction analysis or electron diffraction to determine the ceramic crystal structure, use a microscope and image analysis to measure the porosity in the ceramic, and analyze the composition and structure of the ceramic through Raman spectroscopy;

[0133] Interface analysis: Use high-resolution scanning electron microscopy and energy-dispersive spectroscopy to analyze the chemical composition and structure of the interface;

[0134] (3) Visual inspection;

[0135] By determining the appropriate curing temperature and time, with the temperature being 300 °C and the time being 2 hours, using a protective atmosphere to prevent oxidation, and in addition, ensuring that the curing area is dry to prevent the introduction of moisture, reducing the internal stress of the material through a gradual cooling rate, recording the curing parameters and results through hardness testing, microstructure analysis, and visual inspection of the cermet joint for tracking and quality control, which is conducive to subsequent quality assurance and problem troubleshooting. It is necessary to ensure that the furnace or equipment used for curing is in good condition to ensure the accuracy of temperature and time, thereby improving the reliability and quality of welding.

[0136] Example VI:

[0137] Please refer to Figure 1 and Figure 2 , a manufacturing process for a metal-based ceramic flow channel reactor with diffusion welding performance, including step S6, inspection and quality control: performing non-destructive inspection on the welded connection and conducting quality control tests;

[0138] In the manufacturing process of a microchannel reactor by thermally spraying ceramic materials on the surface of 316L stainless steel, a series of process inspections and quality controls are required to ensure its diffusion welding performance;

[0139] Raw material inspection: Inspect 316L stainless steel through chemical analysis and mechanical property tests. At the same time, conduct composition analysis and structure analysis on the ceramic material;

[0140] Welding process control: Monitor and record the temperature, time, and pressure during welding;

[0141] Non-destructive inspection: Detect pores in the weld using ultrasonic equipment, detect cracks and slag in the weld using X-ray and Y-ray detection equipment, and detect cracks and fatigue in the weld and on the surface using eddy current detection equipment;

[0142] To ensure that the metal matrix material meets the specified chemical composition and mechanical property requirements through chemical analysis, it is also necessary to ensure that the ceramic material meets the manufacturing requirements, detect and record the welding temperature, welding time, and pressure to ensure consistency during the diffusion welding process, use microscopes, scanning electron microscopes (SEM), and transmission electron microscopes (TEM) to analyze the microstructure of the metal and ceramic joints to ensure reasonable diffusion welding, ensure good mutual diffusion between the metal and ceramic to form a uniform interface, conduct hardness tests on the welded area to ensure that the hardness distribution meets the requirements of the design and specifications, and record all data of the manufacturing process to establish a quality traceability system.

[0143] Step S7. Post-treatment: Apply a surface coating or treatment to the manufactured flow channel reactor and perform final assembly;

[0144] Step S71. The post-treatment is to ensure excellent diffusion welding performance and meet the requirements of specific applications. Regularly conduct weld inspections on the diffusion welded joints, eliminate residual stresses and improve the material properties through heat treatment. Strict quality control is required during the post-treatment process, and performance tests are also carried out. Assemble and seal the metal matrix ceramic reactor.

[0145] Among them, the performance tests include:

[0146] (1) Pressure test;

[0147] (2) Temperature cycle test;

[0148] (3) Chemical stability test;

[0149] Use ultrasonic testing to detect the diffusion welded joints to ensure that the welding quality meets the requirements. Eliminate residual stresses and improve the material properties through heat treatment to improve the toughness and strength of the material. Ensure that the dimensions and surface quality of the metal matrix ceramic flow channel reactor meet the requirements through drilling, grinding, and turning. Perform surface treatment on the metal matrix ceramic flow channel reactor to improve the surface finish and cleanliness of the metal. Strict quality control is required during the post-treatment process to ensure that the manufactured metal matrix ceramic flow channel reactor meets the design specifications and quality standards. Assemble and seal the metal matrix ceramic reactor to ensure that it can operate under specific environmental conditions and prevent external substances from entering the reactor.

[0150] Step S8. Testing and verification: Conduct performance testing and verification before actual use;

[0151] Step S81. Among them, the testing and verification methods, in addition to welding quality testing, material property testing, and ceramic coating testing, also include the following testing methods:

[0152] (1) Heat treatment effect verification: To ensure that heat treatment can relieve residual stress and improve material properties;

[0153] (2) Diffusion performance test: To ensure that there is no leakage in the reactor during the diffusion process;

[0154] (3) Sealing performance test: Ensure that it can resist leakage under high pressure, high temperature and corrosive environments;

[0155] (4) Chemical stability test: To ensure that it can withstand the erosion of specific chemicals;

[0156] (5) Performance simulation test: To verify the reliability of the reactor in practical applications;

[0157] (6) Standard compliance test: Ensure that the reactor manufacturing complies with relevant standards and specifications;

[0158] (7) Durability test: To simulate the performance and reliability of the reactor during long-term use;

[0159] These test and verification steps help to ensure the manufacturing quality of the metal matrix ceramic flow channel reactor and ensure its excellent diffusion welding performance in practical applications;

[0160] These test and verification steps help to ensure the manufacturing quality of the metal matrix ceramic flow channel reactor and ensure its excellent diffusion welding performance in practical applications.

[0161] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and without departing from the spirit or basic characteristics of the present invention, the present invention can be implemented in other specific forms. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present invention. Any reference signs in the claims should not be regarded as limiting the claims involved.

Claims

1. A manufacturing process for a metal-based ceramic flow channel reactor with diffusion welding performance, characterized in that: The manufacturing process of the metal-based ceramic flow channel reactor includes the following steps: Step S1, Material selection: Select 316L stainless steel and zirconia ceramics; Step S2, Pretreatment: Cut, process, and clean the 316L stainless steel; Step S3, Spray the ceramic layer; Step S4, Diffusion welding: Use a resistance furnace to control parameters for the diffusion welding machine to work; Step S5, Cooling and curing: Cool the welding area and perform the curing step; Step S6, Inspection and quality control: Conduct non-destructive inspection on the welded connection and perform quality control tests; Step S7, Post-treatment: Apply a surface coating or treatment to the manufactured flow channel reactor and perform final assembly; Step S8, Testing and verification: Conduct performance testing and verification before actual use; Clean the metal and ceramic surfaces using organic solvents, remove the oxides on the metal surface by using an acidic solution, and polish the metal surface using mechanical equipment to obtain a flat and clean surface for improving the bonding quality. Spray a special coating on the metal surface in advance to improve the performance of diffusion welding; The manufacturing process of the metal-based ceramic flow channel reactor further includes the following steps: Step S31, Spray zirconia ceramics on the inner surface of the 316L stainless steel reaction flow channel using thermal spraying technology, optimize the wettability between the coating and the substrate. During the coating and curing process, strictly control the temperature and environmental conditions, and perform appropriate curing and annealing processes; Coating wetting: (1) Temperature control: The working temperature needs to be between 2700°C and 2900°C; (2) Add an interface treatment agent: Improve the interaction and wetting performance between the coating and the substrate by adding a surfactant; (3) Optimize the coating thickness: Control the thickness of the coating; Among them, the curing and annealing process: Put the 316L stainless steel reaction flow channel and the zirconia ceramic coating into a high-temperature furnace together. Set the temperature of the high-temperature furnace between 2700°C and 2750°C, the curing time is 2 hours. Use the heat treatment process to heat the coating and the substrate together, and then cool to improve the performance of the coating. During the curing process, control different atmospheres to affect the performance of the ceramic coating. Then reduce the temperature of the high-temperature furnace to 500°C for annealing. After curing and annealing are completed, the coating needs to be cooled to room temperature, and then the coating is inspected.

2. The manufacturing process for a metal-based ceramic flow channel reactor with diffusion welding performance according to claim 1, characterized in that: The manufacturing process of the metal-based ceramic flow channel reactor further includes the following steps: Step S11, Define the usage environment and performance requirements of the reactor, select 316L stainless steel as the metal-based material, select zirconia ceramics as the ceramic spraying material, and conduct laboratory tests and sample preparation on the 316L stainless steel and zirconia ceramics; Laboratory tests include: (1) Diffusion welding test; (2) Measurement of the coefficient of thermal expansion.

3. The manufacturing process for a metal-based ceramic flow channel reactor with diffusion welding performance according to claim 1, characterized in that: The manufacturing process of the metal-based ceramic flow channel reactor further includes the following steps: Step S21, During the pretreatment process, it is necessary to design and manufacture the metal matrix. The shape and structure of the manufactured metal matrix need to meet the design requirements of the reactor.

4. The manufacturing process for a metal-based ceramic flow channel reactor with diffusion welding performance according to claim 1, characterized in that: The manufacturing process of the metal-based ceramic flow channel reactor further includes the following steps: Step S41, Preheating and soaking: Preheat before welding to reduce the thermal stress of the material and ensure uniform preheating to prevent material deformation; Set the preheating temperature of the high-temperature furnace between 150°C and 300°C, and use a thermometer to ensure the accuracy of the preheating temperature. When the preheating temperature reaches 300°C, control the high-temperature furnace to maintain the same temperature for soaking treatment; Control the welding environment: Ensure the stability of the welding environment and prevent oxygen, moisture, or other contaminants from entering the welding area; Use an atmosphere analyzer and temperature control equipment to continuously monitor and record the parameters of the welding environment; Step S42, After spraying the ceramic layer, diffusion welding is required. Assemble the stainless steel workpieces to be welded into the required shape and position. Coat molybdenum powder on the surface to be welded. Place the stainless steel workpieces and the part coated with metal powder into the high-temperature furnace. Set the temperature of the high-temperature furnace between 1000°C and 1100°C. The pressure application equipment in the high-temperature furnace applies pressure to the stainless steel. During the heating process, the molybdenum powder begins to melt and diffuse into the stainless steel substrate to form a strong welded joint. After the diffusion process of the molybdenum powder is completed, cool the workpiece to room temperature, and then perform post-treatment steps to achieve the required shape and surface quality through cutting and polishing.

5. A manufacturing process for a metal matrix ceramic flow reactor with diffusion welding performance according to claim 4, characterized in that: The manufacturing process of the metal-based ceramic flow channel reactor further includes the following steps: Step S51, After the diffusion welding is completed, determine the appropriate curing temperature and time. At the same time, ensure that the welding area is in an appropriate atmosphere, and control the gradual cooling rate to avoid rapid cooling and the phenomenon of alternating hot and cold. Detection is required after curing, and record the curing parameters and results; Curing detection: (1) Hardness test: Test the welded position through Brinell hardness test; (2) Microstructure analysis; Metal part analysis: Use an optical microscope to observe the microstructure of the metal part, and determine the size and orientation of stainless steel grains through X-ray diffraction analysis; Ceramic part analysis: Use X-ray diffraction analysis or electron diffraction to determine the ceramic crystal structure, use a microscope and image analysis to measure the porosity in the ceramic, and analyze the composition and structure of the ceramic through Raman spectroscopy; Interface analysis: Use a high-resolution scanning electron microscope and energy spectrum analysis to analyze the chemical composition and structure of the interface; (3) Visual inspection.

6. A manufacturing process for a metal matrix ceramic flow reactor with diffusion welding performance according to claim 1, characterized in that: The manufacturing process of the metal-based ceramic flow channel reactor further includes the following steps: Step S61, In the manufacturing process of the microchannel reactor by thermal spraying ceramic materials on the surface of 316L stainless steel, a series of process inspections and quality controls are required to ensure its diffusion welding performance; Raw material inspection: Check 316L stainless steel through chemical analysis and mechanical property tests. At the same time, perform composition analysis and structure analysis on the ceramic material; Welding process control: Monitor and record the temperature, time, and pressure during welding; Non-destructive testing: Use ultrasonic equipment to detect pores in the weld, use testing equipment to detect cracks and slag inclusions in the weld through X-rays and Y-rays, and use eddy current testing equipment to detect cracks and fatigue in the weld and on the surface.

7. A manufacturing process for a metal matrix ceramic flow reactor with diffusion welding performance according to claim 1, characterized in that: The manufacturing process of the metal-based ceramic flow channel reactor further includes the following steps: Step S71. The subsequent treatment is to ensure excellent diffusion welding performance and meet the requirements of specific applications. Regularly conduct weld inspections on the diffusion welded joints, eliminate residual stresses and improve the material properties through heat treatment. During the subsequent treatment process, strict quality control is required, and performance tests are carried out. Assemble and seal the metal matrix ceramic reactor; Among them, the performance tests include: (1) Pressure test; (2) Temperature cycle test; (3) Chemical stability test.

8. A manufacturing process for a metal matrix ceramic flow reactor with diffusion welding performance according to claim 7, characterized in that: The manufacturing process of the metal matrix ceramic flow reactor further includes the following steps: Step S81. Among them, The test and verification methods, in addition to welding quality tests, material property tests, and ceramic coating tests, also include the following test methods: (1) Verification of heat treatment effect; (2) Diffusion performance test; (3) Sealing performance test; (4) Chemical stability test; (5) Performance simulation test; (6) Standard compliance test; (7) Durability test.

Images