High-flux method for researching interface reaction of high-temperature alloy melt and refractory

Abstract

The invention belongs to the technical field of high-throughput preparation in material genetic engineering plans, and particularly relates to a high-throughput method for researching interface reaction of a high-temperature alloy melt and a refractory. The method comprises the following steps: (1) preparing a wax mold; (2) combining a wax mold; (3) preparing a mold shell; (4) cutting high-temperature alloy samples with different chemical components; (5) placing the mold shell filled with the alloy samples with different chemical components in a directional solidification furnace for melting and solidification to obtain an alloy melt and refractory material interface reaction sample; and (6) observing the interface reaction product and reaction degree of the alloy melt and the refractory by using advanced multi-scale characterization equipment, and determining the influence rule of alloy elements on the interface reaction of the melt and the refractory. According to the method, the period and cost of interface reaction experiment research of the high-temperature alloy melt and the refractory can be reduced, the research and development efficiency of high-temperature alloy castings is improved, and engineering application of new materials is promoted.

Description

Technical Field

[0001] The present invention belongs to the technical field of high-throughput preparation in material genetic engineering programs, and in particular relates to a high-throughput method for studying the interface reaction between a high-temperature alloy melt and a refractory material. Background Art

[0002] During the investment casting process of high-temperature alloy castings, the high-temperature alloy melt and the ceramic refractory material are in contact for a long time at high temperature, and complex interactions usually occur at the interface. This interaction includes both thermomechanical penetration and thermophysical and chemical effects, which can easily lead to various types of casting defects on the surface of the casting, of which mechanical sand bonding and chemical sand bonding are the main manifestations.

[0003] The occurrence of the interface reaction between the high-temperature alloy melt and the ceramic refractory material will cause the surface composition of the casting to change, thereby reducing the surface quality and mechanical properties of the casting. However, in actual production, the sand adhesion on the surface of the casting often appears in a comprehensive form. The chemical sand adhesion caused by the interfacial chemical reaction is likely to cause the gas produced in the reaction to form pore-like defects on the surface of the casting, and the penetration of the alloy liquid at high temperature is easy to form a certain amount of mechanical sand adhesion at the interface, thereby expanding the chemical reaction zone, increasing the roughness of the casting surface, reducing the surface quality of the casting, and even affecting the use of the casting. Therefore, in order to improve the surface quality of the casting, it is necessary to study the interface action mechanism and influencing factors between the high-temperature alloy melt and the ceramic refractory material. At present, the research methods of the interface reaction between the high-temperature alloy melt and the ceramic refractory material mainly include the sessile drop method, the leaching method, and the actual pouring sampling analysis. Compared with the sessile drop method and the leaching method, the actual pouring sampling analysis can reflect the real interface reaction products and reaction degree in the casting process of the casting, and is the most widely used in the study of the interface reaction between the melt and the refractory material. However, at present, the actual pouring sampling analysis can only study the interface reaction behavior of one high-temperature alloy and ceramic refractory through one experiment, which undoubtedly increases the experimental cycle and cost.

[0004] In recent years, in order to accelerate the R&D efficiency of new materials, shorten the R&D cycle, reduce R&D costs, and promote the engineering application of new materials, my country has launched the "Material Gene Engineering" project. The basic goal is to achieve "double halving" of R&D costs and cycles, and the way to achieve this is to develop common key technologies and equipment such as material efficient calculation, high-throughput experiments, and big data. Among them, material high-throughput 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 screening of materials and rapid accumulation of experimental data can be achieved, which promotes the process of material R&D and engineering application.

[0005] Therefore, there is an urgent need to develop a high-throughput method to study the interface reaction between high-temperature alloy melts and refractory materials, so as to reduce the cycle and cost of experimental research on the interface reaction between melts and refractory materials and speed up the research and development of high-temperature alloy castings. Summary of the invention

[0006] In view of the problems in the prior art, the present invention provides a high-throughput method for studying the interface reaction between high-temperature alloy melts and refractory materials. Through this method, the interface reaction samples of alloys with various chemical compositions and ceramic refractory materials can be obtained through one experiment, thereby realizing the rapid characterization of the products and reaction degrees of alloys with various chemical compositions and ceramic refractory materials, thereby reducing the experimental cycle and cost, and accelerating the research and development speed of high-temperature alloy castings.

[0007] The technical solution of the present invention is: A high-throughput method for studying the interface reaction between a high-temperature alloy melt and a refractory material comprises the following steps: Step (1) preparing a wax mold for placing a high-temperature alloy sample by injection molding or 3D printing; Step (2) welding the wax mold for placing the high-temperature alloy sample with the connecting column, the supporting column wax mold and the base to complete the wax mold assembly tree; Step (3) cleaning the surface of the assembled wax mold, repeatedly coating the outside with ceramic refractory slurry and repeatedly sprinkling sand to form a wet blank shell, and then performing a dewaxing and roasting process at a high temperature to obtain a high-throughput shell device for studying the interface reaction between high-temperature alloy melt and refractory material; Step (4) cutting high-temperature alloy experimental samples of different chemical compositions by wire cutting according to the size of the wax mold in which the high-temperature alloy sample is placed, and placing the alloy sample in a 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 containing the 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; Step (6) Use advanced multi-scale characterization equipment to observe the products and degree of the interface reaction between the alloy melt and the refractory material, and clarify the influence of alloy elements on the interface reaction between the melt and the refractory material.

[0008] Furthermore, in the above-mentioned high-throughput method for studying the interface reaction between high-temperature alloy melt and refractory material, in step (1), the injection molding process for preparing the wax mold is as follows: melt the paraffin at 50-80°C, inject the molten paraffin 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 1-10 minutes; the size of the wax mold is determined according to the number of high-throughput experiments required.

[0009] Furthermore, in the above-mentioned high-throughput method for studying the interface reaction between high-temperature alloy melt and refractory material, in step (2), according to the number of high-throughput experiments required, when assembling the mold, the wax mold tree is a single-layer or multi-layer wax mold number.

[0010] Furthermore, in step (3) of the above-mentioned high-throughput method for studying the interface 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 coating and sand sprinkling are repeated 5 to 10 times; a dewaxing kettle is used for high-temperature dewaxing at a temperature of 160 to 180°C; a roasting furnace is used for shell sintering at a sintering temperature of 900 to 1000°C and a sintering time of 1 to 3 hours.

[0011] Furthermore, in the above-mentioned high-throughput method for studying the interface reaction between a high-temperature alloy melt and a refractory material, in step (4), after the high-temperature alloy sample is cut by wire cutting, the oxide scale on the alloy surface is polished with sandpaper to ensure the cleanliness of the alloy.

[0012] Furthermore, in the above-mentioned high-throughput method for studying the interface reaction between high-temperature alloy melt and refractory material, in step (5), the melting and solidification process is as follows: the vacuum degree is 0.01~10Pa, and then the temperature is raised to 1400~1650℃ at 5~30℃ / min, and kept at this temperature for 10~60min to melt the alloy sample, and then the shell is lowered to the water-cooled copper ring area at a pulling speed of 5~20mm / min for cooling and solidification, and then taken out of the furnace after cooling.

[0013] Furthermore, in the above-mentioned high-throughput method for studying the interface reaction between high-temperature alloy melt and refractory material, 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.

[0014] The design concept of the present invention is: The occurrence of the interface reaction between the high-temperature alloy melt and the ceramic refractory will cause the surface composition of the casting to change, thereby reducing the surface quality and mechanical properties of the casting. Therefore, it is necessary to study the interface mechanism and influencing factors between the high-temperature alloy melt and the ceramic refractory, so as to provide theoretical guidance for the development of the casting process of high-temperature alloy castings. However, traditional experimental methods such as the sessile drop method, leaching method and actual pouring sampling analysis method can only study the interface reaction behavior of one high-temperature alloy melt and ceramic refractory through one experiment, which undoubtedly increases the experimental cycle and cost.

[0015] High-throughput material experiments refer to experimental techniques and methods including high-throughput preparation, high-throughput characterization, and efficient evaluation of service performance. Through high-throughput material preparation, a batch of samples, that is, dozens or hundreds of samples, can be prepared or processed at one time, thereby significantly improving the research and development efficiency of new materials. Therefore, developing a high-throughput device and method for studying the interface reaction between high-temperature alloy melts and refractory materials can obtain interface reaction samples of alloys with various chemical compositions and ceramic refractory materials through one experimental study, thereby significantly reducing the cycle and cost of experimental research on the interface reaction between melts and refractory materials, and accelerating the research and development of high-temperature alloy castings, which has important theoretical research significance and application value.

[0016] Advantages and beneficial effects of the present invention: 1. The process design of the present invention is reasonable. By designing a high-throughput device and method for studying the interface reaction between high-temperature alloy melts and refractory materials, interface reaction samples of alloys with various chemical compositions and ceramic refractory materials can be obtained through one experiment, thereby realizing rapid characterization of the interface reaction products and reaction degrees of alloys with various chemical compositions and ceramic refractory materials, thereby reducing the experimental cycle and cost, avoiding the waste of manpower and resources caused by traditional experimental methods, and effectively improving the research and development efficiency of the casting process of high-temperature alloy castings.

[0017] 2. The present invention is simple to operate, reasonably designed, and highly operable, and can provide methodological guidance for the high-throughput research and characterization of interface reactions between other types of alloy melts and a variety of ceramic refractory materials.

[0018] 3. The method of the present invention is simple and easy to implement, and is suitable for engineering application and promotion. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 The schematic diagram of the high-throughput device structure for studying the interface reaction between high-temperature alloy melt and refractory material of the present invention is shown in FIG. Figure 1 (a) is the front view, Figure 1 (b) is a top view; Figure 2 The surface morphology and Hf element distribution of the refractory material after the interface reaction between the high-temperature alloy melt with Hf content of 1.3wt% and the refractory material; Figure 3 The surface morphology and Hf element distribution of the refractory material after the interface reaction between the high-temperature alloy melt with Hf content of 1.4wt% and the refractory material; Figure 4 The surface morphology and Hf element distribution of the refractory material after the interface reaction between the high-temperature alloy melt with Hf content of 1.5wt% and the refractory material; In the figure, 1-wax mold for placing high-temperature alloy samples; 2-connecting column; 3-support column; 4-base. DETAILED DESCRIPTION

[0020] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. Example 1

[0021] This embodiment studies a high-throughput method for the interface reaction between a high-temperature alloy melt and a refractory material, comprising the following steps: (1) A wax mold for placing a high-temperature alloy sample was prepared by injection molding. The process of preparing the wax mold by injection molding is as follows: melt the paraffin at 60°C, inject the molten paraffin into the metal mold through a wax injection machine, the injection pressure is 1 MPa, and the pressure is maintained at room temperature for 5 min; the diameter of the wax mold is 30 mm and the height is 30 mm.

[0022] (2) The wax mold 1 used to place the high-temperature alloy sample is welded to the connecting column 2, the supporting column 3 wax mold and the base 4 to complete the wax mold assembly tree. According to the number of high-throughput experiments required, the number of layers is set to 3 when assembling the mold, and the number of single-layer wax molds used to place the high-temperature alloy sample is 6.

[0023] (3) Clean the surface of the assembled wax mold, repeatedly apply ceramic refractory slurry on the outside and repeatedly sprinkle sand. The ceramic refractory slurry is prepared from corundum sand and silica sol base materials. Repeat the slurry application and sanding for 6 times to form a wet blank shell. Use a dewaxing kettle for high-temperature dewaxing at a temperature of 170°C; use a roasting furnace to sinter the shell at a sintering temperature of 980°C and a sintering time of 2h to obtain a high-throughput shell device for studying the interface reaction between high-temperature alloy melt and refractory material. The schematic diagram of the high-throughput shell device is shown in the figure. Figure 1 shown.

[0024] (4) Wire cutting was used to cut high-temperature alloy experimental samples with different Hf content. The sample size was 10×10×10 mm, and the mass fraction of Hf was 1.3%, 1.4% and 1.5%, respectively. The surface oxide scale of the alloy was polished with 400# sandpaper to ensure the cleanliness of the alloy, and 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.

[0025] (5) The mold shell containing high-temperature alloy samples with different Hf element contents was placed in a directional solidification furnace for melting and solidification. The melting and solidification process was as follows: the vacuum degree was 0.1 Pa, and then the temperature was raised to 1550°C at 20°C / min and kept at this temperature for 20 minutes to melt the alloy sample. Then, the mold shell was lowered to the water-cooled copper ring area at a pulling speed of 10 mm / min for cooling and solidification. After the end, it was taken out of the furnace with cooling to obtain the interface reaction samples of high-temperature alloy melts with different Hf element contents and ceramic refractory materials.

[0026] (6) The products and extent of the interface reaction between the high-temperature alloy melt and the refractory material with different Hf element contents were observed using a scanning electron microscope. The results are as follows: Figure 2-Figure 4 It can be found that the method of the present invention achieves high-throughput preparation and observation of melt-ceramic refractory interface reaction samples, proving the feasibility of the method of the present invention.

[0027] Based on the above results, it can be seen that the present invention, by establishing a high-throughput device and method for studying the interface reaction between high-temperature alloy melts and refractory materials, can achieve high-throughput preparation and observation of melt-refractory interface reaction samples, thereby reducing the cycle and cost of experimental research on the interface reaction between high-temperature alloy melts and refractory materials, speeding up the research and development efficiency of high-temperature alloy castings, and providing methodological guidance for accelerating the development and engineering application of new metal materials.

[0028] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. However, these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A high-throughput method for studying the interface reaction between high-temperature alloy melt and refractory material, characterized in that: The following steps are involved: Step (1) preparing a wax mold for placing a high-temperature alloy sample by injection molding or 3D printing; Step (2) welding the wax mold for placing the high-temperature alloy sample with the connecting column, the supporting column wax mold and the base to complete the wax mold assembly tree; Step (3) cleaning the surface of the assembled wax mold tree, repeatedly coating the outside with ceramic refractory slurry and repeatedly sprinkling sand to form a wet blank shell, and then performing a dewaxing and roasting process at a high temperature to obtain a high-throughput shell device for studying the interface reaction between high-temperature alloy melt and refractory material; Step (4) cutting high-temperature alloy experimental samples of different chemical compositions by wire cutting according to the size of the wax mold in which the high-temperature alloy sample is placed, and placing the high-temperature alloy sample in a 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 containing the 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; Step (6) Use advanced multi-scale characterization equipment to observe the products and extent of the interface reaction between the alloy melt and the refractory material, and clarify the influence of alloy elements on the interface reaction between the melt and the refractory material.

2. A high-throughput method for studying the interface reaction between high-temperature alloy melt and refractory material according to claim 1, characterized in that: In step (1), the process of preparing a wax mold for placing a high-temperature alloy sample by injection molding is as follows: melt the paraffin at 50-80°C, inject the molten paraffin into the metal mold by a wax injection machine, the injection pressure is 0.5-2MPa, and the pressure is maintained at room temperature for 1-10 minutes; the size of the wax mold is determined according to the number of high-throughput experiments required.

3. A high-throughput method for studying the interface reaction between high-temperature alloy melt and refractory material according to claim 1, characterized in that: In step (2), according to the number of high-throughput experiments required, when assembling the model, the wax model tree is composed of single-layer or multi-layer wax models.

4. A high-throughput method for studying the interface reaction between a high-temperature alloy melt and a refractory material according to claim 1, characterized in that: In step (3), the ceramic refractory slurry is prepared from corundum sand and silica sol, and the slurry coating and sand sprinkling are repeated 5 to 10 times; a dewaxing kettle is used for high-temperature dewaxing at a temperature of 160 to 180°C; a roasting furnace is used for shell sintering at a sintering temperature of 900 to 1000°C and a sintering time of 1 to 3 hours.

5. A high-throughput method for studying the interface reaction between high-temperature alloy melt and refractory material according to claim 1, characterized in that: In step (4), after the high-temperature alloy sample is cut by wire cutting, the oxide scale on the surface of the alloy is polished with sandpaper to ensure the cleanliness of the alloy.

6. A high-throughput method for studying the interface reaction between high-temperature alloy melt and refractory material according to claim 1, characterized in that: In step (5), the melting and solidification process is as follows: the vacuum degree is 0.01~10Pa, then the temperature is raised to 1400~1650℃ at a rate of 5~30℃ / min, and the temperature is kept for 10~60min to melt the alloy sample, and then the shell is lowered to the water-cooled copper ring area at a pulling speed of 5~20mm / min for cooling and solidification, and then taken out of the furnace after cooling.

7. A high-throughput method for studying the interface reaction between high-temperature alloy melt and refractory material 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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