Measurement method of high-temperature alloy texture

Abstract

The invention discloses a method for measuring a high-temperature alloy texture, and belongs to the technical field of metal texture measurement. The measuring method comprises the following steps: performing coarse grinding, coarse polishing and fine polishing on a high-temperature alloy sample formed by additive manufacturing to prepare a to-be-analyzed sample; carrying out image data acquisition on the to-be-analyzed sample by adopting a scanning electron microscope equipped with an EBSD probe; post-processing software is adopted to complete correction and analysis of the image data, and texture and grain orientation information of the sample to be analyzed is obtained; the image data acquisition area is 40-50 mm < 2 >, and the acquisition step length is 2-10 [mu] m. The calibration rate of the high-temperature alloy sample applying the measurement method is higher than 99%, the maximum texture strength is stable, the texture and orientation information of the high-temperature alloy sample can be accurately obtained, meanwhile, the structure morphology of the area can be completely reserved, and the measurement accuracy is high. The problems that the EBSD detection range is small, the high-temperature alloy sample formed through additive manufacturing cannot be accurately and completely characterized, and the alloy texture measurement accuracy is low are solved.

Description

Technical Field

[0001] The invention belongs to the technical field of metal texture measurement, and in particular relates to a method for measuring high-temperature alloy texture. Background Art

[0002] Additive manufacturing (AM) can quickly prepare parts with high dimensional accuracy by melting and solidifying layer by layer based on 3D model data. Nickel-based high-temperature alloys such as GH3536 are widely used in aero engines due to their high high-temperature strength, good oxidation resistance, strong corrosion resistance and excellent fatigue performance. However, the microstructure of alloys formed by AM is usually composed of columnar crystals with high aspect ratios growing along the deposition direction. This directional growth will form a strong texture, resulting in anisotropy of mechanical properties. In order to improve the performance of the material, it is necessary to elaborate the relationship between texture and mechanical properties.

[0003] At present, the main methods for measuring texture include X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). Among them, the XRD sample preparation method is simple, requiring only simple mechanical grinding, and the measurement results are relatively macroscopic, but it cannot directly reflect the grain orientation and texture information; while the EBSD sample preparation is relatively complex, requiring strict polishing of the sample surface, the test structure is more microscopic, and can directly give information such as organizational morphology and grain orientation, but there are problems such as small detection range and inapplicability to additive manufacturing of high-temperature alloy samples. Because the columnar crystals of AM-formed high-temperature alloys usually span several printing layers and can reach millimeter levels in length. Small-scale detection or measurement of multiple different areas cannot accurately or intuitively characterize the organization and texture completely. In practical applications, there are also some that combine XRD and EBSD to achieve a comprehensive analysis from macro to micro.

[0004] The invention patent with publication number CN106908461A discloses a method for measuring in-plane polycrystalline texture. The method irradiates the product to be inspected with X-rays and collects and analyzes the intensity changes of the X-rays to achieve the measurement of in-plane polycrystalline texture. However, this method cannot intuitively reflect the orientation information of a single grain.

[0005] The invention patent with publication number CN102680502A discloses a method for measuring the texture of metal bars, which is used to solve the difficulty that the shape of the curved sample cannot correct the influence of the X-ray diffraction intensity, and realize the direct and accurate measurement of the texture of the metal bar. However, this method is relatively complicated to operate, and each measurement requires the preparation of a non-textured standard sample to calibrate the test sample.

[0006] The invention patent with publication number CN103389316A discloses a method for measuring silicon steel texture. It uses EBSD equipment to measure the orientation distribution diagram of multiple different thickness areas in the longitudinal section of the sample and eliminates the influence of errors caused by the EBSD measurement area being too small by measuring the data of multiple areas. However, this method has the problem of complex sampling and sample preparation, and the ESBD measurement needs to be performed on multiple different areas in multiple times, which takes a long time to measure. In order to obtain accurate texture distribution data, it is also necessary to perform complex post-processing calculations on the measurement results. In addition, this method is mainly aimed at the problem of uneven distribution of the structure of oriented silicon steel itself in the radial direction, such as: the texture in the middle of the oriented silicon steel sample will be quite different from that in the edge, and a single area cannot represent the overall situation of the sample. It is necessary to measure multiple different areas. Due to the different properties of oriented silicon steel and high-temperature alloys, there is inevitably incompatibility and difference in the sample preparation and measurement requirements between the two. Summary of the invention

[0007] The present invention provides a method for measuring the texture of a high-temperature alloy. The method adopts a method based on large area stitching technology (LAM) and electron backscatter diffraction (EBSD) to solve the problem of low texture measurement accuracy of nickel-based high-temperature alloys such as GH3536 alloy formed by additive manufacturing (AM), and can also accurately and completely reflect the columnar crystal morphology, crystal structure and orientation information. Since the measurement accuracy and reliability are affected by EBSD image acquisition and stitching errors, nickel-based high-temperature alloy stress and surface quality. In addition to requiring appropriate EBSD image acquisition parameters, large-area stitching EBSD characterization has high requirements on sample surface quality. While increasing the EBSD acquisition area, the difficulty of sample preparation is also greatly increased. Poor surface quality will lead to a decrease in calibration rate, affecting the measurement results. Therefore, preparing a sample with a smooth surface without scratches and low residual stress, as well as appropriate image acquisition methods and parameters are key factors to ensure the accuracy of high-temperature alloy texture measurement.

[0008] The present invention is achieved through the following technical solutions: A method for measuring a high temperature alloy texture comprises the following steps: Step 1: Roughly grind, roughly polish, and finely polish the high-temperature alloy sample formed by additive manufacturing to prepare a sample to be analyzed; Step 2: Use a scanning electron microscope equipped with an EBSD probe to collect image data of the sample to be analyzed; Step 3: Use post-processing software to complete the correction and analysis of image data to obtain the texture and grain orientation information of the sample to be analyzed; Among them, the image data acquisition area is 40-50mm 2 , the acquisition step size is 2-10μm.

[0009] For example, the image data acquisition area is 40 mm2 , 41 mm 2 , 42 mm 2 , 43 mm 2 , 44 mm 2 , 45 mm 2 、46mm 2 , 47 mm 2 , 48 mm 2 , 49 mm 2 or 50 mm 2 .

[0010] For example, the acquisition step size is 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm or 10 μm.

[0011] Furthermore, the working voltage of the scanning electron microscope is 15-20 kV, the tilt angle of the sample to be analyzed is 60-70°, and the working distance is 16-20 mm.

[0012] For example, the operating voltage of the scanning electron microscope is 15 kV, 16 kV, 17 kV, 18 kV, 19 kV or 20 kV; the tilt angle of the sample to be analyzed is 60°, 62°, 65°, 67° or 70°; the working distance is 16 mm, 17 mm, 18 mm, 19 mm or 20 mm.

[0013] Furthermore, the high temperature alloy is a nickel-based high temperature alloy.

[0014] Furthermore, the nickel-based high-temperature alloy includes GH3536 and GH4169.

[0015] Furthermore, the rough grinding includes grinding the high-temperature alloy sample with 400-2000 mesh silicon carbide sandpaper until the surface is smooth.

[0016] Preferably, the rough grinding includes sequentially using 400 mesh, 800 mesh, 1200 mesh, 1500 mesh and 2000 mesh silicon carbide sandpaper to grind the high-temperature alloy sample until the surface is smooth.

[0017] Furthermore, the rough polishing includes polishing the high-temperature alloy sample with 5 μm and 1.5 μm diamond polishing liquids in sequence for 5-10 min, wherein the polishing disc has a rotation speed of 150-200 r / min and a pressure of 20-30N.

[0018] Preferably, the rough polishing comprises polishing the high-temperature alloy sample with 5 μm and 1.5 μm diamond polishing liquids in sequence for 5 minutes, with a polishing disc speed of 150 r / min and a pressure of 25N.

[0019] Furthermore, after each rough polishing, the high-temperature alloy sample is cleaned ultrasonically for 5-10 minutes, the frequency of ultrasonic cleaning is 40-50 kHz, and the temperature is 30-50° C.; the cleaning agent of the ultrasonic cleaning is a mixture of water and anhydrous ethanol, and the volume ratio of water to anhydrous ethanol is 5-6:1.

[0020] Optionally, after each rough polishing, the high-temperature alloy sample is ultrasonically cleaned for 5-10 minutes, the frequency of ultrasonic cleaning is 40 kHz, and the temperature is 30-50°C; the cleaning agent of the ultrasonic cleaning is a mixture of 85 ml of deionized water and 15 ml of anhydrous ethanol to remove residual diamonds on the sample surface and in the pores.

[0021] Furthermore, the polishing time of the fine polishing is 10-20 min, the polishing disc rotation speed is 150-200 r / min, the polishing pressure range is 5-30 N, the polishing time is divided into 2-4 sections, and the polishing pressure decreases step by step in different time periods.

[0022] Preferably, the polishing agent for fine polishing is a mixed solution of 80% OPS and 20% H2O2, the polishing time is 15 minutes, the polishing disk speed is 150r / min, and the polishing pressure decreases step by step in different time periods, including 30N pressure in the first 1 / 3 of the time, 20N pressure in the middle 1 / 3 of the time, and 5N pressure in the last 1 / 3 of the time.

[0023] Furthermore, after the fine polishing is completed, the high-temperature alloy sample is cleaned with ultrasound for 5-10 minutes, the frequency of the ultrasonic cleaning is 40-50 kHz, and the temperature is 30-50° C.; the cleaning agent for the ultrasonic cleaning is a mixture of water and anhydrous ethanol, and the volume ratio of water to anhydrous ethanol is 8-10:1.

[0024] Optionally, after the fine polishing, the high-temperature alloy sample is cleaned with ultrasound for 5 minutes, the frequency of the ultrasonic cleaning is 40 kHz, and the temperature is 50° C.; the cleaning agent for the ultrasonic cleaning is a mixture of 90 ml of deionized water and 10 ml of anhydrous ethanol to remove the OPS remaining on the sample surface and in the pores.

[0025] Furthermore, the post-processing software includes OIM Analysis software, AZtecCrystal software, MTEX ​​and ATEX software.

[0026] Furthermore, the additive manufacturing forming is any one of selective laser melting (SLM), electron beam selective melting (EBSM), and direct energy deposition (DED).

[0027] Compared with the prior art, the present invention has the following beneficial effects: The present invention provides a mechanical polishing sample preparation method with good surface quality and low residual stress suitable for large-area splicing EBSD characterization of high-temperature alloy samples, and provides a collection area and step length of a large-area splicing EBSD method suitable for high-temperature alloy samples, solving the problem that the EBSD detection range is small and it is not suitable for accurate or intuitive complete characterization of the organization and texture of high-temperature alloy samples formed by additive manufacturing. The calibration rate of the high-temperature alloy sample using the method of the present invention is higher than 99%, and the maximum texture strength is stable, so that the texture and orientation information of the high-temperature alloy sample can be accurately obtained, and the organizational morphology of the area can be completely retained.

[0028] Other features and advantages of the present invention will be described in the following description, and partly become obvious from the description, or be understood by practicing the present invention. The purpose and other advantages of the present invention can be realized and obtained by the specific embodiments pointed out in the description. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 The SLM GH3536 alloy collection area in Example 1 of the present invention is 40mm 2 EBSD image data, including (a) IPF map, (b) PF map; Figure 2 The SLM GH3536 alloy collection area in Example 2 of the present invention is 45mm 2 EBSD image data, including (a) IPF map, (b) PF map; Figure 3 The SLM GH3536 alloy collection area in Example 3 of the present invention is 50mm 2 EBSD image data, including (a) IPF map, (b) PF map; Figure 4 The SLM GH3536 alloy collection area in Comparative Example 1 of the present invention is 1mm 2 EBSD image data, including (a) IPF map, (b) PF map; Figure 5 The SLM GH3536 alloy collection area in Comparative Example 2 of the present invention is 16mm2 EBSD image data, including (a) IPF map, (b) PF map; Figure 6 The collection area of ​​SLM GH3536 alloy in comparative example 3 of the present invention is 36mm 2 EBSD image data, including (a) IPF map, (b) PF map; Figure 7 It is a graph showing the relationship between the collection area and the texture strength of the embodiments and comparative examples. DETAILED DESCRIPTION

[0030] In order to make the purpose, technical scheme and advantages of the present invention clearer, the implementation scheme of the present application will be described in detail below in conjunction with specific examples. The technical terms and scientific terms used in the present invention have the meanings generally understood by those of ordinary skill in the art to which the present invention belongs, without other definitions. Without departing from the concept of the present invention, those skilled in the art may make various improvements and changes to the specific implementation methods of the present invention specification, which all belong to the protection scope of the present invention. The raw materials used in the present invention are all commercially available unless otherwise specified.

[0031] Example 1 A method for measuring the texture of GH3536 nickel-based high-temperature alloy comprises the following steps: Step 1: The nickel-based high-temperature alloy sample GH3536 formed by selective laser melting SLM additive manufacturing is subjected to rough grinding, rough polishing, and fine polishing to prepare a sample to be analyzed. The GH3536 alloy is composed of the following components by mass percentage: Cr21.5%, Fe 19.2%, Mo 9.3%, Co 1.6%, W 0.75%, Mn 0.41%, Si 0.32%, C 0.05%, and the balance is Ni; Rough grinding: Use 400 mesh, 800 mesh, 1200 mesh, 1500 mesh and 2000 mesh silicon carbide sandpaper to grind the nickel-based high-temperature alloy sample GH3536 in sequence until the surface is flat.

[0032] Rough polishing: 5μm and 1.5μm diamond polishing liquid (model XY-350) were used to rough polish the nickel-based high-temperature alloy sample GH3536 for 5 minutes, with a polishing disk speed of 150r / min and a pressure of 25N. After each rough polishing, the nickel-based high-temperature alloy sample GH3536 was cleaned with ultrasonic waves for 5 minutes. The frequency and temperature of ultrasonic cleaning were 40kHZ and 30℃ respectively, and the cleaning agent was a mixed solution of 85ml deionized water and 15ml anhydrous ethanol to remove diamond residues on the sample surface and in the pores.

[0033] Fine polishing: polishing for 15 minutes with a mixed solution of 80% OPS (model Struers-OP-S-0.25μm) and 20% H2O2. The polishing disc speed is 150r / min, the pressure is 30N for 0-5min, 20N for 5-10min, and 5N for 10-15min to reduce the residual stress on the surface.

[0034] After fine polishing, ultrasonic cleaning was used for 5 minutes. The frequency and temperature of ultrasonic cleaning were 40 kHz and 30°C, respectively. The cleaning agent was a mixed solution of 10 ml deionized water and 90 ml anhydrous ethanol to remove the residual OPS on the sample surface and in the pores.

[0035] The length, width and thickness of the sample to be analyzed are 10 mm×6 mm×4 mm.

[0036] Step 2: Use a scanning electron microscope equipped with an EBSD probe to collect image data of the sample to be analyzed; The scanning electron microscope model used for EBSD is TESCAN CLARA GMH, the operating voltage of the scanning electron microscope is 15 kV, the tilt angle of the sample to be analyzed is 70°, and the working distance is 20 mm.

[0037] Image data acquisition area is 40mm 2 , the acquisition step size is 5μm.

[0038] Step 3: Use the guided alignment function in Aztec 6.2 software to stitch and correct the EBSD image data, and then use Aztec Crystal 2.1 software to analyze the texture and grain orientation of the BESD image data.

[0039] Figure 1 The area of ​​the GH3536 alloy formed by SLM in Example 1 of the present invention is 40mm 2 EBSD image data diagram, including (a) IPF map (Inverse Pole Figure map) and (b) PF map (Pole Figure).

[0040] The IPF diagram is a graph used to represent the parallel relationship between the crystal direction and the sample direction. It uses color coding to display the directional distribution of a set of reference vectors under a fixed lattice framework. It is mainly used to analyze the crystal orientation of materials, especially the relationship between the crystal direction and the sample direction. The PF diagram is a graph used to represent the orientation of grains in various directions in a material. It shows the orientation density distribution under a specific crystal plane index and is used to analyze the texture of the material, that is, the distribution characteristics of the crystal orientation. It uses colors or markings to indicate the orientation density under different crystal plane indices. Usually red indicates the highest orientation strength.

[0041] In this example, the sample calibration rate is 99.12%, see Figure 1 (a) A large number of complete columnar crystals growing along the deposition direction can be observed. The maximum texture strength calculated by the software is 4.46, see Figure 1 (b).

[0042] Example 2 A method for measuring the texture of GH3536 nickel-based high-temperature alloy comprises the following steps: Step 1: The nickel-based high-temperature alloy sample GH3536 formed by selective laser melting SLM additive manufacturing is subjected to rough grinding, rough polishing, and fine polishing to prepare a sample to be analyzed. The GH3536 alloy is composed of the following components by mass percentage: Cr21.5%, Fe 19.2%, Mo 9.3%, Co 1.6%, W 0.75%, Mn 0.41%, Si 0.32%, C 0.05%, and the balance is Ni; Rough grinding: Use 400 mesh, 800 mesh, 1200 mesh, 1500 mesh and 2000 mesh silicon carbide sandpaper to grind the nickel-based high-temperature alloy sample GH3536 in sequence until the surface is flat.

[0043] Rough polishing: 5μm and 1.5μm diamond polishing liquid XY-350 were used to rough polish the nickel-based high-temperature alloy sample GH3536 for 5 minutes, the polishing disk speed was 150r / min, and the pressure was 25N. After each rough polishing, the nickel-based high-temperature alloy sample GH3536 was cleaned with ultrasonic waves for 7 minutes. The frequency and temperature of ultrasonic cleaning were 50kHZ and 40℃ respectively, and the cleaning agent was a mixed solution of 85ml deionized water and 15ml anhydrous ethanol to remove the residual diamonds on the sample surface and in the pores.

[0044] Fine polishing: polishing for 18 minutes with a mixed solution of 80% OPS (Struers-OP-S-0.25μm) and 20% H2O2. The polishing disc speed is 200r / min, the pressure is 30N for 0-6min, 20N for 6-12min, and 5N for 12-18min to reduce the surface residual stress. After fine polishing, ultrasonic cleaning is used for 7 minutes. The frequency and temperature of ultrasonic cleaning are 50kHZ and 30-50℃ respectively. The cleaning agent is a mixed solution of 10ml deionized water and 90ml anhydrous ethanol to remove the OPS residue on the sample surface and in the pores.

[0045] The size of the sample to be analyzed was 10 mm×6 mm×4 mm.

[0046] Step 2: Use a scanning electron microscope equipped with an EBSD probe to collect image data of the sample to be analyzed; The scanning electron microscope model used for EBSD is TESCAN CLARA GMH, the operating voltage of the scanning electron microscope is 15 kV, the tilt angle of the sample to be analyzed is 70°, and the working distance is 20 mm.

[0047] Image data acquisition area is 45mm 2 , the acquisition step size is 5μm.

[0048] Step 3: Use the guided alignment function in Aztec 6.2 software to stitch and correct the EBSD image data, and then use Aztec Crystal 2.1 software to analyze the texture and grain orientation of the BESD image data.

[0049] Figure 2 The area of ​​the GH3536 alloy formed by SLM in Example 2 of the present invention is 45mm 2 EBSD image data diagram, including (a) IPF map (Inverse Pole Figure map), (b) PF map (Pole Figure).

[0050] In this case, the sample calibration rate reached 99.11%. Figure 2 (a) A large number of complete columnar crystals growing along the deposition direction can be observed. The maximum texture strength calculated by the software is 4.43, see Figure 2 (b).

[0051] Example 3 A method for measuring the texture of GH3536 nickel-based high-temperature alloy comprises the following steps: Step 1: The nickel-based high-temperature alloy sample GH3536 formed by selective laser melting SLM additive manufacturing is subjected to rough grinding, rough polishing, and fine polishing to prepare a sample to be analyzed. The GH3536 alloy is composed of the following components by mass percentage: Cr21.5%, Fe 19.2%, Mo 9.3%, Co 1.6%, W 0.75%, Mn 0.41%, Si 0.32%, C 0.05%, and the balance is Ni; Rough grinding: Use 400 mesh, 800 mesh, 1200 mesh, 1500 mesh and 2000 mesh silicon carbide sandpaper to grind the nickel-based high-temperature alloy sample GH3536 in sequence until the surface is flat.

[0052] Rough polishing: 5μm and 1.5μm diamond polishing liquid XY-350 were used to rough polish the nickel-based high-temperature alloy sample GH3536 for 5 minutes, the polishing disc speed was 200r / min, and the pressure was 25N. After each rough polishing, the nickel-based high-temperature alloy sample GH3536 was cleaned with ultrasonic waves for 10 minutes. The frequency and temperature of ultrasonic cleaning were 50kHZ and 50℃ respectively, and the cleaning agent was a mixed solution of 85ml deionized water and 15ml anhydrous ethanol to remove the residual diamonds on the sample surface and in the pores.

[0053] Fine polishing: polishing for 12 minutes with a mixed solution of 80% OPS (Struers-OP-S-0.25μm) and 20% H2O2. The polishing disc speed is 150r / min, the pressure is 30N for 0-4min, 20N for 4-8min, and 5N for 8-12min to reduce the surface residual stress.

[0054] After fine polishing, ultrasonic cleaning was used for 10 minutes. The frequency and temperature of ultrasonic cleaning were 50 kHz and 30-50 °C, respectively. The cleaning agent was a mixed solution of 10 ml deionized water and 90 ml anhydrous ethanol to remove OPS residues on the sample surface and in the pores.

[0055] The size of the prepared sample to be analyzed is 10 mm×6 mm×4 mm.

[0056] Step 2: Use a scanning electron microscope equipped with an EBSD probe to collect image data of the sample to be analyzed; The scanning electron microscope model used for EBSD is TESCAN CLARA GMH, the operating voltage of the scanning electron microscope is 20 kV, the tilt angle of the sample to be analyzed is 70°, and the working distance is 18 mm.

[0057] Image data acquisition area is 50mm 2 , the acquisition step size is 5μm.

[0058] Step 3: Use the guided alignment function in Aztec 6.2 software to stitch and correct the EBSD image data, and then use Aztec Crystal 2.1 software to analyze the texture and grain orientation of the BESD image data.

[0059] Figure 3 The area of ​​the GH3536 alloy formed by SLM in Example 3 of the present invention is 50mm 2 EBSD image data diagram, including (a) IPF map (Inverse Pole Figure map), (b) PF map (Pole Figure).

[0060] In this example, the sample calibration rate is 99.15%, see Figure 3 (a) A large number of complete columnar crystals growing along the deposition direction can be observed. The maximum texture strength calculated by the software is 4.42, see Figure 3 (b).

[0061] Comparative Example 1 A method for measuring the texture of GH3536 nickel-based high-temperature alloy comprises the following steps: Step 1: The nickel-based high-temperature alloy sample GH3536 formed by selective laser melting SLM additive manufacturing is subjected to rough grinding, rough polishing, and fine polishing to prepare a sample to be analyzed. The GH3536 alloy is composed of the following components by mass percentage: Cr21.5%, Fe 19.2%, Mo 9.3%, Co 1.6%, W 0.75%, Mn 0.41%, Si 0.32%, C 0.05%, and the balance is Ni; Rough grinding: Use 400 mesh, 800 mesh, 1200 mesh, 1500 mesh and 2000 mesh silicon carbide sandpaper to grind the nickel-based high-temperature alloy sample GH3536 in sequence until the surface is flat.

[0062] Rough polishing: 5μm and 1.5μm diamond polishing liquid XY-350 were used to rough polish the nickel-based high-temperature alloy sample GH3536 for 5 minutes, the polishing disk speed was 200r / min, and the pressure was 25N. After each rough polishing, the nickel-based high-temperature alloy sample GH3536 was cleaned with ultrasonic waves for 5 minutes. The frequency and temperature of ultrasonic cleaning were 50kHZ and 30℃ respectively, and the cleaning agent was a mixed solution of 85ml deionized water and 15ml anhydrous ethanol to remove the residual diamonds on the sample surface and in the pores.

[0063] Fine polishing: polishing for 15 minutes with a mixed solution of 80% OPS (Struers-OP-S-0.25μm) and 20% H2O2. The polishing disc speed is 200r / min, the pressure is 30N for 0-5min, 20N for 5-10min, and 5N for 10-15min to reduce the surface residual stress. After fine polishing, ultrasonic cleaning is used for 5 minutes. The frequency and temperature of ultrasonic cleaning are 50kHZ and 30℃ respectively. The cleaning agent is a mixed solution of 10ml deionized water and 90ml anhydrous ethanol to remove the residual OPS on the sample surface and in the pores.

[0064] The size of the prepared sample to be analyzed is 10 mm×6 mm×4 mm.

[0065] Step 2: Use a scanning electron microscope equipped with an EBSD probe to collect image data of the sample to be analyzed; The scanning electron microscope model used for EBSD is TESCAN CLARA GMH, the operating voltage of the scanning electron microscope is 15 kV, the tilt angle of the sample to be analyzed is 70°, and the working distance is 18 mm.

[0066] The image data acquisition area is 1mm 2 , the acquisition step size is 5μm.

[0067] Step 3: Use the guided alignment function in Aztec 6.2 software to stitch and correct the EBSD image data, and then use Aztec Crystal 2.1 software to analyze the texture and grain orientation of the BESD image data.

[0068] Figure 4 The collection area of ​​GH3536 alloy formed by SLM in Comparative Example 1 of the present invention is 1mm 2 EBSD image data diagram, including (a) IPF map (Inverse Pole Figure map), (b) PF map (Pole Figure).

[0069] In this case, the sample calibration rate reached 98.83%. Figure 4 (a) A large number of complete columnar crystals growing along the deposition direction can be observed. The maximum texture strength calculated by the software is 5.23, see Figure 4 (b).

[0070] Comparative Example 2 A method for measuring the texture of GH3536 nickel-based high-temperature alloy comprises the following steps: Step 1: The nickel-based high-temperature alloy sample GH3536 formed by selective laser melting SLM additive manufacturing is subjected to rough grinding, rough polishing, and fine polishing to prepare a sample to be analyzed. The GH3536 alloy is composed of the following components by mass percentage: Cr21.5%, Fe 19.2%, Mo 9.3%, Co 1.6%, W 0.75%, Mn 0.41%, Si 0.32%, C 0.05%, and the balance is Ni; Rough grinding: Use 400 mesh, 800 mesh, 1200 mesh, 1500 mesh and 2000 mesh silicon carbide sandpaper to grind the nickel-based high-temperature alloy sample GH3536 in sequence until the surface is flat.

[0071] Rough polishing: 5μm and 1.5μm diamond polishing liquid XY-350 were used to rough polish the nickel-based high-temperature alloy sample GH3536 for 5 minutes, the polishing disk speed was 150r / min, and the pressure was 25N. After each rough polishing, the nickel-based high-temperature alloy sample GH3536 was cleaned with ultrasonic waves for 5 minutes. The frequency and temperature of ultrasonic cleaning were 40kHZ and 40℃ respectively, and the cleaning agent was a mixed solution of 85ml deionized water and 15ml anhydrous ethanol to remove the residual diamonds on the sample surface and in the pores.

[0072] Fine polishing: polishing for 18 minutes with a mixed solution of 80% OPS (Struers-OP-S-0.25μm) and 20% H2O2. The polishing disc speed is 150r / min, the pressure is 30N for 0-6min, 20N for 6-12min, and 5N for 12-18min to reduce the surface residual stress. After fine polishing, ultrasonic cleaning is used for 5 minutes. The frequency and temperature of ultrasonic cleaning are 40kHZ and 30℃ respectively. The cleaning agent is a mixed solution of 10ml deionized water and 90ml anhydrous ethanol to remove the OPS residue on the sample surface and in the pores.

[0073] The size of the prepared sample to be analyzed is 10 mm×6 mm×4 mm.

[0074] Step 2: Use a scanning electron microscope equipped with an EBSD probe to collect image data of the sample to be analyzed; The scanning electron microscope model used for EBSD is TESCAN CLARA GMH, the operating voltage of the scanning electron microscope is 15 kV, the tilt angle of the sample to be analyzed is 70°, and the working distance is 20 mm.

[0075] Image data acquisition area is 16mm 2 , the acquisition step size is 5μm.

[0076] Step 3: Use the guided alignment function in Aztec 6.2 software to stitch and correct the EBSD image data, and then use Aztec Crystal 2.1 software to analyze the texture and grain orientation of the BESD image data.

[0077] Figure 5 The collection area of ​​GH3536 alloy formed by SLM in Comparative Example 2 of the present invention is 16mm 2 EBSD image data diagram, including (a) IPF map (Inverse Pole Figure map), (b) PF map (Pole Figure).

[0078] In this case, the sample calibration rate reached 98.93%. Figure 5(a) A large number of complete columnar crystals growing along the deposition direction can be observed. The maximum texture strength calculated by the software is 4.08, see Figure 5 (b).

[0079] Comparative Example 3 A method for measuring the texture of GH3536 nickel-based high-temperature alloy comprises the following steps: Step 1: The nickel-based high-temperature alloy sample GH3536 formed by selective laser melting SLM additive manufacturing is subjected to rough grinding, rough polishing, and fine polishing to prepare a sample to be analyzed. The GH3536 alloy is composed of the following components by mass percentage: Cr21.5%, Fe 19.2%, Mo 9.3%, Co 1.6%, W 0.75%, Mn 0.41%, Si 0.32%, C 0.05%, and the balance is Ni; Rough grinding: Use 400 mesh, 800 mesh, 1200 mesh, 1500 mesh and 2000 mesh silicon carbide sandpaper to grind the nickel-based high-temperature alloy sample GH3536 in sequence until the surface is flat.

[0080] Rough polishing: 5μm and 1.5μm diamond polishing liquid XY-350 were used to rough polish the nickel-based high-temperature alloy sample GH3536, with a polishing disk speed of 200r / min and a pressure of 25N. After each rough polishing, the nickel-based high-temperature alloy sample GH3536 was cleaned with ultrasonic waves for 10 minutes. The frequency and temperature of ultrasonic cleaning were 40kHZ and 50℃, respectively. The cleaning agent was a mixed solution of 85ml deionized water and 15ml anhydrous ethanol to remove the residual diamonds on the sample surface and in the pores.

[0081] Fine polishing: polishing for 12 minutes with a mixed solution of 80% OPS (Struers-OP-S-0.25μm) and 20% H2O2. The polishing disc speed is 150r / min, the pressure is 30N for 0-4min, 20N for 4-8min, and 5N for 8-12min. After fine polishing, ultrasonic cleaning is performed for 10 minutes. The frequency and temperature of ultrasonic cleaning are 50kHZ and 30℃ respectively. The cleaning agent is a mixed solution of 10ml deionized water and 90ml anhydrous ethanol to remove OPS residues on the sample surface and in the pores.

[0082] The size of the prepared sample to be analyzed is 10 mm×6 mm×4 mm.

[0083] Step 2: Use a scanning electron microscope equipped with an EBSD probe to collect image data of the sample to be analyzed; The scanning electron microscope model used for EBSD is TESCAN CLARA GMH, the operating voltage of the scanning electron microscope is 20 kV, the tilt angle of the sample to be analyzed is 70°, and the working distance is 18 mm.

[0084] Image data acquisition area is 36mm 2 , the acquisition step size is 5μm.

[0085] Step 3: Use the guided alignment function in Aztec 6.2 software to stitch and correct the EBSD image data, and then use Aztec Crystal 2.1 software to analyze the texture and grain orientation of the BESD image data.

[0086] Figure 6 The collection area of ​​GH3536 alloy formed by SLM in Comparative Example 3 of the present invention is 1mm 2 EBSD image data diagram, including (a) IPF map (Inverse Pole Figure map), (b) PF map (Pole Figure).

[0087] In this example, the sample calibration rate is 99.07%. Figure 6 (a) A large number of complete columnar crystals growing along the deposition direction were observed. The maximum texture strength calculated by the software was 4.27. Figure 6 (b).

[0088] It can be seen that the calibration rate of the samples obtained by this sample preparation method exceeds 99%, which provides a crucial guarantee for the subsequent orientation and texture measurement. Figure 1-3 ) shows the same hotspot distribution position of the maximum texture intensity in the PF diagram, while the comparative examples 1-3 ( Figure 4-6 ) will change with the scanning area.

[0089] The maximum texture strength diagrams of Examples 1-3 and Comparative Examples 1-3 under different collection areas were plotted to obtain Figure 7 .from Figure 7 It can be seen that as the EBSD collection area increases, the maximum texture intensity fluctuates dramatically, but when the collection area is between 40-50mm 2 When the value is between 0.04 and 0.17, the maximum texture strength tends to be stable, and the texture information of GH3536 alloy can be accurately obtained. At the same time, the detection in this range has good universality and can cover stable analysis at the macro and micro levels.

[0090] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for measuring high temperature alloy texture, characterized in that: The following steps are involved: The high-temperature alloy sample formed by additive manufacturing is subjected to rough grinding, rough polishing, and fine polishing to prepare a sample to be analyzed; A scanning electron microscope equipped with an EBSD probe was used to collect image data of the sample to be analyzed; Post-processing software is used to complete the correction and analysis of image data to obtain the texture and grain orientation information of the sample to be analyzed; Among them, the image data acquisition area is 40-50mm 2 , the acquisition step size is 2-10μm.

2. The measuring method according to claim 1, characterized in that: The working voltage of the scanning electron microscope is 15-20 kV, the tilt angle of the sample to be analyzed is 60-70°, and the working distance is 16-20 mm.

3. The measuring method according to claim 1, characterized in that: The high temperature alloy is a nickel-based high temperature alloy.

4. The measuring method according to claim 3, characterized in that: The nickel-based high-temperature alloys include GH3536 and GH4169.

5. The measuring method according to claim 1, characterized in that: The rough grinding includes sequentially using 400 mesh, 800 mesh, 1200 mesh, 1500 mesh and 2000 mesh silicon carbide sandpaper to grind the high-temperature alloy sample until the surface is flat.

6. The measuring method according to claim 1, characterized in that: The rough polishing includes polishing the high-temperature alloy sample with 5 μm and 1.5 μm diamond polishing liquids in sequence for 5-10 minutes, wherein the polishing disc has a rotation speed of 150-200 r / min and a pressure of 20-30N.

7. The measuring method according to claim 6, characterized in that: After each rough polishing, the high-temperature alloy sample is cleaned by ultrasonic wave for 5-10 minutes, the frequency of ultrasonic wave cleaning is 40-50 kHz, and the temperature is 30-50° C.; the cleaning agent of ultrasonic wave cleaning is a mixture of water and anhydrous ethanol, and the volume ratio of water to anhydrous ethanol is 5-6:

1.

8. The measuring method according to claim 1, characterized in that: The polishing time of the fine polishing is 10-20 minutes, the rotating speed of the polishing disc is 150-200 r / min, the polishing pressure ranges from 5-30N, and the polishing pressure decreases step by step in different time periods.

9. The measuring method according to claim 1, characterized in that: After the fine polishing is completed, the high-temperature alloy sample is cleaned with ultrasound for 5-10 minutes, the frequency of the ultrasonic cleaning is 40-50 kHz, and the temperature is 30-50° C. The cleaning agent of the ultrasonic cleaning is a mixture of water and anhydrous ethanol, and the volume ratio of water to anhydrous ethanol is 8-10:

1.

10. The measuring method according to claim 1, characterized in that: The post-processing software includes OIM Analysis software, AZtecCrystal software, MTEX ​​and ATEX software.

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