A high-throughput method for studying interfacial reactions between superalloy melts and refractories

Abstract

The present application belongs to the high-throughput preparation technical field in the material gene engineering plan, and particularly relates to a high-throughput method for researching the interface reaction between high-temperature alloy melt and refractory material. The method steps are as follows: (1) preparing a wax mold; (2) combining the wax mold; (3) preparing a mold shell; (4) cutting high-temperature alloy samples with different chemical compositions; (5) placing the mold shell with the alloy samples with different chemical compositions into a directional solidification furnace for melting and solidification to obtain the interface reaction sample between the alloy melt and the refractory material; and (6) observing the interface reaction product and the reaction degree between the alloy melt and the refractory material by using advanced multi-scale characterization equipment, and determining the influence law of alloy elements on the interface reaction between the melt and the refractory material. The method can reduce the period and cost of the experimental research on the interface reaction between the high-temperature alloy melt and the refractory material, accelerate the research and development efficiency of high-temperature alloy castings, and promote the engineering application of new materials.

Description

Technical Field

[0001] This invention belongs to the field of high-throughput preparation technology in the Materials Genome Project, specifically relating to a high-throughput method for studying the interfacial reaction between high-temperature alloy melts and refractory materials. Background Technology

[0002] In the investment casting process of high-temperature alloy castings, the high-temperature alloy melt and the ceramic refractory are in contact for a long time at high temperature. Complex interactions usually occur at the interface. These interactions include both thermomechanical penetration and thermophysical-chemical interactions, which can easily lead to the formation of various types of casting defects on the surface of the casting. Mechanical sand adhesion and chemical sand adhesion are the main manifestations of these defects.

[0003] The interfacial reaction between high-temperature alloy melt and ceramic refractories alters the surface composition of castings, leading to a decline in surface quality and mechanical properties. However, in actual production, surface sand adhesion often occurs in a complex manner. Chemical sand adhesion caused by interfacial chemical reactions can cause gases generated during the reaction to form porosity defects on the casting surface, while the penetration of the alloy melt at high temperatures easily creates mechanical sand adhesion at the interface, thus expanding the chemical reaction zone, increasing surface roughness, reducing surface quality, and even affecting the casting's usability. Therefore, to improve the surface quality of castings, it is necessary to study the interfacial interaction mechanism and influencing factors between high-temperature alloy melt and ceramic refractories. Currently, research methods for interfacial reactions between high-temperature alloy melt and ceramic refractories mainly include the drop method, leaching method, and actual casting sampling analysis. Compared to the drop method and leaching method, actual casting sampling analysis can reflect the actual interfacial reaction products and degree of reaction during the casting process and is the most widely used in the study of melt-refractory interface reactions. However, at present, actual casting sampling analysis can only study the interfacial reaction behavior between a high-temperature alloy and ceramic refractory through a single experiment, which undoubtedly increases the experimental cycle and cost.

[0004] In recent years, to accelerate the efficiency of new material research and development, shorten the research and development cycle, reduce research and development costs, and promote the engineering application of new materials, my country has launched the "Materials Genome Engineering" project. The basic goal is to halve both research and development costs and timelines. This is achieved through the development of common key technologies and equipment such as efficient materials computing, high-throughput experiments, and big data. Among these, high-throughput materials experiments mainly include experimental techniques and methods such as high-throughput preparation, high-throughput characterization, and efficient evaluation of service performance. Through high-throughput experiments, rapid material screening and rapid accumulation of experimental data can be achieved, promoting the progress of materials research and development and engineering applications.

[0005] Therefore, there is an urgent need to develop a high-throughput method for studying the interfacial reaction between high-temperature alloy melts and refractory materials, so as to reduce the cycle and cost of experimental research on the interfacial reaction between melts and refractory materials, and accelerate the research and development of high-temperature alloy castings. Summary of the Invention

[0006] To address the problems in existing technologies, this invention provides a high-throughput method for studying the interfacial reaction between high-temperature alloy melts and refractory materials. This method allows for the acquisition of interfacial reaction samples of alloys with various chemical compositions and ceramic refractory materials in a single experiment, thereby enabling rapid characterization of the products and reaction extent of these reactions. This reduces experimental time and cost, and accelerates the development of high-temperature alloy castings.

[0007] The technical solution of this invention is:

[0008] A high-throughput method for studying the interfacial reaction between high-temperature alloy melts and refractory materials includes the following steps:

[0009] Step (1) Prepare a wax model for placing the high-temperature alloy sample by means of injection molding or 3D printing;

[0010] Step (2) Weld the wax model used to place the high-temperature alloy sample to the connecting column, the support column wax model and the base to complete the wax model assembly tree;

[0011] Step (3) Clean the surface of the assembled wax mold, repeatedly coat the outside with ceramic refractory slurry and repeatedly sprinkle sand to form a wet blank shell, and then carry out dewaxing and baking processes at high temperature to obtain a high-throughput mold shell device for studying the interface reaction between high-temperature alloy melt and refractory material.

[0012] Step (4) Based on the size of the wax mold on which the high-temperature alloy sample is placed, use wire cutting to cut out high-temperature alloy experimental samples with different chemical compositions, and place the alloy samples in a high-throughput mold shell device for studying the interface reaction between high-temperature alloy melt and refractory.

[0013] Step (5) Place the mold containing alloy samples with different chemical compositions in a directional solidification furnace for melting and solidification to obtain interface reaction samples of different alloy melts and ceramic refractory materials.

[0014] Step (6) Use advanced multi-scale characterization equipment to observe the reaction products and degree of reaction at the interface between the alloy melt and the refractory material, and clarify the influence of alloying elements on the reaction at the interface between the melt and the refractory material.

[0015] Furthermore, in the above-mentioned high-throughput method for studying the interfacial reaction between high-temperature alloy melt and refractory material, in step (1), the wax mold preparation process by injection is as follows: the paraffin wax is melted at 50~80℃, and the molten paraffin wax is injected into the metal mold through a wax injection machine. The injection pressure is 0.5~2MPa, and the pressure is maintained at room temperature for 1~10min. The size of the wax mold is determined according to the number of high-throughput experiments required.

[0016] Furthermore, in the above-mentioned high-throughput method for studying the interfacial reaction between high-temperature alloy melt and refractory material, in step (2), according to the high-throughput experimental quantity requirements, the wax model assembly tree is a single layer or a multi-layer wax model.

[0017] Furthermore, in step (3) of the above-mentioned high-throughput method for studying the interfacial reaction between high-temperature alloy melt and refractory material, the ceramic refractory slurry is prepared from basic materials such as corundum sand and silica sol, and the slurry is repeatedly applied and sand is sprinkled 5 to 10 times; high-temperature dewaxing is carried out in a dewaxing kettle at a temperature of 160 to 180°C; and shell sintering is carried out in a sintering furnace at a temperature of 900 to 1000°C for a sintering time of 1 to 3 hours.

[0018] Furthermore, in the above-mentioned high-throughput method for studying the interfacial reaction between high-temperature alloy melt and refractory material, in step (4), after cutting the high-temperature alloy sample by wire cutting, sandpaper is used to polish the oxide scale on the alloy surface to ensure the cleanliness of the alloy.

[0019] Furthermore, in the above-mentioned high-throughput method for studying the interfacial reaction between high-temperature alloy melt and refractory material, the melting and solidification process in step (5) is as follows: the vacuum degree is 0.01~10Pa, then the temperature is raised to 1400~1650℃ at 5~30℃ / min, and held for 10~60min to melt the alloy sample. Then, the shell is lowered to the water-cooled copper ring area at a pulling speed of 5~20mm / min for cooling and solidification. After the process is completed, the shell is cooled and removed with the furnace.

[0020] Furthermore, in the above-mentioned high-throughput method for studying the interfacial reaction between high-temperature alloy melt and refractory, the advanced multi-scale characterization equipment in step (6) includes scanning electron microscope, X-ray diffractometer and electron probe X-ray microanalyzer, etc.

[0021] The design concept of this invention is:

[0022] The interfacial reaction between high-temperature alloy melts and ceramic refractories alters the surface composition of castings, leading to a decline in surface quality and mechanical properties. Therefore, it is necessary to study the interfacial interaction mechanism and influencing factors between high-temperature alloy melts and ceramic refractories to provide theoretical guidance for the development of high-temperature alloy casting processes. Traditional experimental methods, such as the drop method, immersion method, and actual casting sampling analysis, can only study the interfacial reaction behavior of one type of high-temperature alloy melt with ceramic refractories in a single experiment, which undoubtedly increases the experimental cycle and cost.

[0023] High-throughput materials testing refers to experimental techniques and methods that include high-throughput preparation, high-throughput characterization, and efficient evaluation of service performance. High-throughput materials preparation allows for the simultaneous preparation or processing of batches of samples—dozens or hundreds—significantly improving the efficiency of new material development. Therefore, developing a high-throughput device and method for studying the interfacial reaction between high-temperature alloy melts and refractory materials, enabling the acquisition of interfacial reaction samples of alloys with various chemical compositions and ceramic refractory materials in a single experimental study, can significantly reduce the cycle and cost of melt-refractory interfacial reaction experimental research, accelerate the development of high-temperature alloy castings, and has significant theoretical research and application value.

[0024] Advantages and beneficial effects of the present invention:

[0025] 1. The process design of this invention is reasonable. By designing a high-throughput device and method for studying the interfacial reaction between high-temperature alloy melt and refractory, it is possible to obtain interfacial reaction samples of alloys with multiple chemical compositions and ceramic refractory in a single experiment. This enables rapid characterization of the interfacial reaction products and reaction degree of alloys with multiple chemical compositions and ceramic refractory, thereby reducing the experimental cycle and cost, avoiding the waste of manpower and resources caused by traditional experimental methods, and effectively improving the R&D efficiency of high-temperature alloy casting process.

[0026] 2. This invention is simple to operate, reasonably designed, and highly operable. It can provide methodological guidance for high-throughput research and characterization of interfacial reactions between other types of alloy melts and various ceramic refractory materials.

[0027] 3. The method of the present invention is simple and easy to implement, and is suitable for engineering application and promotion. Attached Figure Description

[0028] Figure 1 This invention provides a schematic diagram of a high-throughput device for studying the interfacial reaction between high-temperature alloy melts and refractory materials, wherein... Figure 1 (a) is the front view. Figure 1 (b) is a top view;

[0029] Figure 2 The surface morphology and Hf element distribution of the refractory material after the interfacial reaction between the high-temperature alloy melt with Hf content of 1.3 wt% and the refractory material;

[0030] Figure 3 The surface morphology and Hf element distribution of the refractory material after the interfacial reaction between the high-temperature alloy melt with Hf content of 1.4 wt% and the refractory material;

[0031] Figure 4 The surface morphology and Hf element distribution of the refractory material after the interfacial reaction between the high-temperature alloy melt with Hf content of 1.5 wt% and the refractory material;

[0032] In the figure, 1-wax model for placing high-temperature alloy samples; 2-connecting column; 3-support column; 4-base. Detailed Implementation

[0033] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. Example 1

[0034] This embodiment studies a high-throughput method for the interfacial reaction between high-temperature alloy melt and refractory material, including the following steps:

[0035] (1) A wax mold for placing high-temperature alloy samples was prepared by injection molding. The process of preparing the wax mold by injection molding was as follows: the paraffin wax was melted at 60°C, and the molten paraffin wax was injected into the metal mold by a wax injection machine. The injection pressure was 1 MPa, and the pressure was maintained at room temperature for 5 min. The diameter of the wax mold was 30 mm and the height was 30 mm.

[0036] (2) Weld the wax model 1 used to place the high-temperature alloy sample to the connecting column 2 and the supporting column 3, and the wax model and base 4 to complete the wax model assembly. According to the high-throughput experiment quantity requirements, the number of layers is set to 3 when assembling the model, and the number of wax models used to place the high-temperature alloy sample in a single layer is 6.

[0037] (3) The surface of the assembled wax mold is cleaned, and the exterior is repeatedly coated with ceramic refractory slurry and sprinkled with sand. The ceramic refractory slurry is prepared by corundum sand and silica sol base material. The slurry and sand are repeatedly applied and sprinkled 6 times to form a wet shell. High-temperature dewaxing is performed in a dewaxing kettle at a temperature of 170℃; the shell is sintered in a sintering furnace at a temperature of 980℃ for 2 hours to obtain a high-throughput mold shell device for studying the interfacial reaction between high-temperature alloy melt and refractory material. The structural schematic diagram of the high-throughput mold shell device is shown below. Figure 1 As shown.

[0038] (4) High-temperature alloy experimental samples with different Hf element contents were cut using wire cutting. The sample size was 10×10×10mm, and the mass fraction of Hf element was 1.3%, 1.4% and 1.5% respectively. The oxide scale on the alloy surface was polished with 400# sandpaper to ensure the cleanliness of the alloy. The polished high-temperature alloy experimental samples were placed in a high-throughput mold shell device used to study the interface reaction between high-temperature alloy melt and refractory.

[0039] (5) Place the mold shell containing high-temperature alloy samples with different Hf element contents into a directional solidification furnace for melting and solidification. The melting and solidification process is as follows: the vacuum degree is 0.1 Pa, and then the temperature is raised to 1550℃ at 20℃ / min and held for 20 min to melt the alloy sample. Then, the mold shell is lowered to the water-cooled copper ring area at a pulling speed of 10 mm / min for cooling and solidification. After the process is completed, the mold shell is cooled and removed with the furnace to obtain the interface reaction samples of high-temperature alloy melt with different Hf element contents and ceramic refractory.

[0040] (6) The reaction products and degree of reaction at the interface between high-temperature alloy melts with different Hf element contents and refractory materials were observed using a scanning electron microscope. The results are as follows: Figures 2-4 As shown, the method of this invention enables high-throughput preparation and observation of samples showing the interfacial reaction between melt and ceramic refractory, demonstrating the feasibility of the method.

[0041] In summary, the present invention establishes a high-throughput device and method for studying the interfacial reaction between high-temperature alloy melts and refractory materials, enabling high-throughput preparation and observation of samples of the interfacial reaction between melts and refractory materials. This reduces the cycle and cost of experimental research on the interfacial reaction between high-temperature alloy melts and refractory materials, accelerates the R&D efficiency of high-temperature alloy castings, and provides methodological guidance for accelerating the development and engineering application of new metallic materials.

[0042] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit them. Although the invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A high-throughput method for investigating the interfacial reaction of a superalloy melt with a refractory material, characterized in that, The method comprises the following steps: Step (1) preparing a wax mold for placing a high-temperature alloy sample by a compression molding method or a 3D printing method; Step (2) welding the wax mold for placing the high-temperature alloy sample with a connecting column, a supporting column wax mold and a base to complete a wax mold assembly tree; Step (3) cleaning the surface of the assembled wax mold assembly tree, repeatedly coating ceramic refractory slurry outside and repeatedly sanding to form a wet green mold shell, and then performing a dewaxing and baking process at high temperature to obtain a high-throughput mold shell device for studying the interface reaction between a high-temperature alloy melt and refractory material; Step (4) cutting high-temperature alloy experimental samples with different chemical compositions by using a wire cutting machine according to the size of the wax mold for placing the high-temperature alloy sample, and placing the high-temperature alloy sample in the high-throughput mold shell device for studying the interface reaction between the high-temperature alloy melt and the refractory material; Step (5) placing the mold shell with the alloy sample with different chemical compositions in a directional solidification furnace to melt and solidify, and obtaining the interface reaction sample between the different alloy melt and the ceramic refractory material; Step (6) observing the interface reaction product and the reaction degree between the alloy melt and the refractory material by using advanced multi-scale characterization equipment, and determining the influence law of alloy elements on the interface reaction between the melt and the refractory material.

2. The high-throughput method for investigating the interfacial reaction between superalloy melt and refractory according to claim 1, characterized in that, In step (1), the process of preparing the wax mold for placing the high-temperature alloy sample by the compression molding method is as follows: melting the paraffin at 50-80 DEG C, injecting the molten paraffin into a metal mold by a wax injection machine, the injection pressure is 0.5-2 MPa, and the pressure is maintained at room temperature for 1-10 min; the size of the wax mold is determined according to the number of high-throughput experiments.

3. The high-throughput method for investigating the interfacial reaction between superalloy melt and refractory according to claim 1, characterized in that, In step (2), according to the number of high-throughput experiments, the number of wax molds in the mold assembly is single-layer or multi-layer.

4. The high-throughput method for investigating the interfacial reaction between superalloy melt and refractory according to claim 1, characterized in that, In step (3), the ceramic refractory slurry is prepared from corundum sand and silica sol, the number of repeated slurry coating and sanding is 5-10 times; the dewaxing is performed in a dewaxing kettle at a temperature of 160-180 DEG C; the mold shell is sintered in a sintering furnace at a sintering temperature of 900-1000 DEG C for 1-3 h.

5. The high-throughput method for investigating the interfacial reaction between superalloy melt and refractory according to claim 1, characterized in that, In step (4), after the high-temperature alloy sample is cut by the wire cutting machine, the alloy surface is polished by using sandpaper to ensure the cleanliness of the alloy.

6. The high-throughput method for investigating the interfacial reaction between superalloy melt and refractory according to claim 1, characterized in that, In step (5), the melting and solidification process is as follows: the vacuum degree is 0.01-10 Pa, then the temperature is raised to 1400-1650 DEG C at a rate of 5-30 DEG C / min, the alloy sample is melted, then the mold shell is lowered to the water-cooled copper ring area at a pulling rate of 5-20 mm / min for cooling and solidification, and after the process is completed, the mold shell is taken out after the furnace is cooled.

7. The high-throughput method for investigating the interfacial reaction between superalloy melt and refractory according to claim 1, characterized in that, In step (6), the advanced multi-scale characterization equipment includes a scanning electron microscope, an X-ray diffractometer and an electron probe X-ray microanalyzer.

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