Alloy powder internal hole defect sample, characterization method, device, medium and equipment thereof

Abstract

This invention discloses a characterization method, apparatus, medium, and equipment for an alloy powder sample with internal pore defects, belonging to the field of alloy powder technology. The sample includes a non-metallic container, alloy powder, and a curing material. The alloy powder is spherical and contained within the container, with the curing material filling the spaces between the alloy powder particles. Under X-ray imaging conditions, the alloy powder exhibits a first color (contrast), the curing material exhibits a second color, and the internal pore defects of the alloy powder exhibit a third color. The first, second, and third colors are clearly distinguishable. The characterization method, apparatus, medium, and equipment for this alloy powder sample with internal pore defects can characterize these defects with high accuracy, high efficiency, and strong applicability.

Description

Technical Field

[0001] This invention relates to the field of alloy powder technology, and in particular to a characterization method, apparatus, medium and equipment for an alloy powder sample with internal pore defects. Background Technology

[0002] High-temperature alloys are currently widely used in aero-engines, ground-based gas turbines, nuclear power, chemical industry, and deep-sea oil extraction. High-temperature alloy powders can confine elemental segregation to the micrometer scale and form fine spherical particles. These particles can then be formed through hot isostatic pressing (HIP) into powder metallurgy or additive manufacturing, and can also be used as support frameworks for brazing materials. Currently, the most efficient mainstream high-temperature alloy powder preparation method is gas atomization. However, this type of powder is prone to hollow powder defects—single or multiple pore defects within the spherical alloy powder—due to the complexity of the gas atomization powder preparation process. These pore defects can be spherical or non-spherical, i.e., irregular shapes. In powder metallurgy high-temperature alloys, the powder and powder surface are bonded through diffusion solid-solid bonding. The pore defects in the hollow powder will be inherited by the bulk alloy, adversely affecting the alloy. Summary of the Invention

[0003] In view of this, the present invention provides a sample of internal pore defects in alloy powder, and its characterization method, apparatus, medium and equipment can characterize the internal pore defects of the alloy powder. Its characterization accuracy is high, efficiency is high and applicability is strong, thus making it more suitable for practical use.

[0004] To achieve the first objective mentioned above, the technical solution for alloy powder samples with internal pore defects provided by this invention is as follows:

[0005] The alloy powder internal pore defect sample provided by this invention includes a non-metallic container, alloy powder, and a curing material.

[0006] The alloy powder is spherical and is contained in the container.

[0007] The solidified material is filled between the alloy powders within the container;

[0008] The alloy powder has a first color (contrast) under X-ray imaging conditions, the cured material has a second color under X-ray conditions, and the internal pore defects of the alloy powder have a third color under X-ray conditions, wherein the first color, the second color, and the third color can be clearly distinguished.

[0009] The alloy powder sample with internal pore defects provided by this invention can be further improved using the following technical measures.

[0010] Preferably, the container is cylindrical or tapered.

[0011] Preferably, the components in the cured material are: epoxy resin: 90-110 g / m³, dibutyl phthalate: 15-25 g / m³, and ethylenediamine: 1-3 g / m³, wherein the density of the epoxy resin is in the range of 1.5-2.5 g / m³. 3 .

[0012] Preferably, the particle size of the alloy powder ranges from 1 μm to 355 μm, and the density of the alloy powder ranges from 7.0 to 9.5 g / m³. 3 .

[0013] Preferably, the X-ray generating mechanism is a synchrotron X-ray machine or an X-ray three-dimensional microscope.

[0014] To achieve the second objective mentioned above, the technical solution for preparing alloy powder samples with internal pore defects provided by this invention is as follows:

[0015] The method for preparing alloy powder samples with internal pore defects provided by the present invention includes the following steps:

[0016] Obtain alloy powders of various particle size grades;

[0017] The curing material is added to the non-metallic container, and the curing material is in a fluid state;

[0018] The alloy powders of various particle sizes are added to a non-metallic container containing the cured material, so that the alloy powders are distributed in the cured material and form dense stacks to obtain an intermediate product;

[0019] The intermediate product was left to stand to obtain a sample with internal pore defects in the alloy powder.

[0020] The method for preparing alloy powder samples with internal pore defects provided by the present invention can be further implemented using the following technical measures.

[0021] Preferably, during the step of adding the curing material to the non-metallic container and the curing material being in a flowing state, the time for which the curing material is left to stand is greater than or equal to 10 minutes.

[0022] Preferably, in the step of adding the alloy powder of various particle sizes to a non-metallic container containing the cured material, so that the alloy powder is distributed in the cured material and forms a dense stack to obtain an intermediate product, the alloy powder of various particle sizes is added to the non-metallic container in multiple batches. The time interval between two consecutive additions of the alloy powder of various particle sizes to the non-metallic container is greater than or equal to 5 minutes. The addition height of the alloy powder of various particle sizes is less than 5 mm each time it is added to the non-metallic container of the cured material. After the dense stack is formed, the standing time is greater than or equal to 24 hours.

[0023] To achieve the third objective mentioned above, the technical solution for characterizing alloy powder samples with internal pore defects provided by this invention is as follows:

[0024] The method for characterizing internal pore defects in alloy powder provided by the present invention is characterized by comprising the following steps:

[0025] Obtain an image of the alloy powder sample with internal pore defects provided by the present invention under X-ray conditions;

[0026] Based on the X-ray image of the alloy powder sample with internal pore defects, distinguish the colors of each region in the X-ray image;

[0027] Based on the color of each region in the image under the X-ray conditions, the properties of the region corresponding to each color are determined, and the internal pore defect characteristics of the alloy powder are obtained.

[0028] The characterization method for alloy powder samples with internal pore defects provided by the present invention can be further implemented using the following technical measures.

[0029] Preferably, the step of determining the properties of the regions corresponding to each color based on the color of each region in the image under the X-ray conditions, and obtaining the internal pore defect characteristics of the alloy powder, specifically includes the following steps:

[0030] The color of the spherical region within the non-metallic container under the X-ray conditions is taken as the first color;

[0031] The second color is the color of the area between the spherical regions in the non-metallic container under the X-ray conditions.

[0032] The color of the region located in the middle of each spherical region in the non-metallic container under the X-ray conditions is taken as the third color;

[0033] Among them, the first color, the second color, and the third color can be clearly distinguished;

[0034] The corresponding regions of the first color, the second color, and the third color are characterized to obtain the internal pore defect characteristics of the alloy powder.

[0035] Preferably, in the step of distinguishing the colors of different regions in the X-ray image based on the image of the alloy powder with internal pore defects under X-ray conditions, the pixel size is 0.7 to 10 μm, the field of view is Φ0.5×0.5 mm to Φ10×10 mm, and the voltage range is 50 kV to 150 kV.

[0036] To achieve the fourth objective mentioned above, the technical solution of the characterization device for alloy powder internal pore defects provided by the present invention is as follows:

[0037] The alloy powder internal pore defect sample characterization device provided by the present invention includes:

[0038] The image acquisition module is used to acquire images of the alloy powder internal pore defect sample provided by the present invention under X-ray conditions.

[0039] The color differentiation module is used to differentiate the colors of different regions in the X-ray image based on the image of the alloy powder sample with internal pore defects under X-ray conditions.

[0040] The characterization module is used to determine the properties of the regions corresponding to each color based on the color of each region in the image under the X-ray conditions, and to obtain the internal pore defect characteristics of the alloy powder.

[0041] To achieve the fifth objective mentioned above, the present invention provides the following technical solution for a computer-readable storage medium:

[0042] The present invention provides a program storing a method for characterizing an alloy powder internal pore defect sample on a computer-readable storage medium. When the program for characterizing an alloy powder internal pore defect sample is executed by a processor, it implements the steps of the method for characterizing an alloy powder internal pore defect sample provided by the present invention.

[0043] To achieve the sixth objective mentioned above, the technical solution for the electronic device provided by this invention is as follows:

[0044] The electronic device provided by the present invention includes a memory and a processor. The memory stores a program for characterizing alloy powder internal pore defect samples. When the program for characterizing alloy powder internal pore defect samples is executed by the processor, it implements the steps of the alloy powder internal pore defect sample characterization method provided by the present invention.

[0045] The beneficial effects of this invention are:

[0046] First, compared with traditional two-dimensional characterization, quantitative characterization of powder internal pore defects is not affected by the cutting location, and the detection accuracy is higher while ensuring resolution.

[0047] Second, compared to traditional two-dimensional characterization, powder sampling rate is higher and statistical results are better;

[0048] Third, compared with traditional two-dimensional characterization, in addition to statistically analyzing the size and volume fraction of pore defects, it is also possible to observe the morphological information of pore defects.

[0049] Fourth, compared to traditional two-dimensional characterization, it has higher detection efficiency;

[0050] Fifth, compared to traditional three-dimensional characterization, it offers higher imaging resolution for fine-diameter powder and pore defects;

[0051] Sixth, it abandons the traditional three-dimensional characterization method of using shape to distinguish and identify powder internal pore defects and powder stacking gaps, and uses low-density flowable curable material to fill powder gaps. It distinguishes powder gaps and powder internal pore defects by different X-ray imaging contrast (color), and can use computers to automatically identify grayscale thresholds, thus improving detection speed and accuracy.

[0052] Seventh, the present invention adopts the method of first putting the flowable filling material into the container, and then adding the alloy powder, letting it stand and then solidifying. By utilizing the high density and natural settling characteristics of the powder, better powder gap filling can be achieved.

[0053] Eighth, compared with traditional three-dimensional characterization, such as powder pore defects that are non-spherical and irregular in shape, they cannot be distinguished from powder gap regions by shape recognition. This invention can form a good contrast distinction during X-ray imaging by using a low-density filling method for powder gaps, which is not affected by the shape of the defect.

[0054] Ninth, compared with traditional three-dimensional characterization, different instrument parameter tests require different thicknesses and corresponding sample cross-sectional dimensions, requiring the preparation of multiple samples of different sizes. This invention, by using a variable cross-section tapered integral solidified sample, can obtain multiple different experimental parameters and results from a single sample, further improving detection efficiency.

[0055] Tenth, the powder gap filling material formulation should use a material with good flowability and curability. High curing strength is not required. As long as a density difference and imaging contrast difference (color differentiation) can be formed, the sample preparation requirements can be met.

[0056] Eleventh, the interstitial filling curing material can completely fix the relative position of the originally loose powder. In some important products, it is required that the sample be preserved for the same life as the product. For such applications, if there is a need for retesting later, X-ray three-dimensional imaging of fixed powder samples has a greater advantage than loose and unfixed powder samples.

[0057] Twelfth, using tapered specimens allows for the characterization of pore defects in thin-section imaging, as well as the characterization of the microstructure of powder alloys (such as precipitates), while thick-section imaging provides a higher sampling rate and better statistical results for pore defects. Attached Figure Description

[0058] Various other advantages and benefits will become apparent to those skilled in the art upon reading the following detailed description of preferred embodiments. The accompanying drawings are for illustrative purposes only and are not intended to limit the invention. Furthermore, the same reference numerals denote the same parts throughout the drawings. In the drawings:

[0059] Appendix Figure 1 The diagram shows the sample shape and X-ray imaging of three alloy powder samples with internal pore defects: where a-alloy powder region, b-spherical hollow pore defects in hollow powder, c-non-spherical hollow pore defects in hollow powder, d-powder gap region (with the same imaging contrast / color as pore defects b or c in hollow powder under X-ray imaging, and with a similar shape to non-spherical hollow pore defects c), and e-powder gap region filled with flowable curable material (with different imaging contrast / color than internal pore defects b or c).

[0060] Appendix Figure 2 A flowchart illustrating the steps of preparing an alloy powder sample with internal pore defects according to an embodiment of the present invention;

[0061] Appendix Figure 3 A flowchart illustrating the steps of the alloy powder internal pore defect sample characterization method provided in this embodiment of the invention;

[0062] Appendix Figure 4 A schematic diagram showing the signal flow relationship between the functional modules of the alloy powder internal pore defect sample characterization device provided in an embodiment of the present invention;

[0063] Appendix Figure 5 This is a schematic diagram of an alloy powder internal pore defect sample characterization device for the hardware operating environment involved in an embodiment of the present invention. Detailed Implementation

[0064] In view of this, the present invention provides a sample of internal pore defects in alloy powder, and its characterization method, apparatus, medium and equipment can characterize the internal pore defects of the alloy powder. Its characterization accuracy is high, efficiency is high and applicability is strong, thus making it more suitable for practical use.

[0065] Through arduous and persistent efforts, the inventors discovered that in powder metallurgy high-temperature alloys, the powder and its surface are bonded through diffusion solid-solid bonding. The porosity of the hollow powder is inherited by the bulk alloy, negatively impacting its properties. In additive manufacturing, although the alloy powder is usually completely melted, the varying local melting and solidification conditions near the original porosity defects also affect subsequent alloy forming. When used as a brazing support framework, only the brazing filler metal melts, while the high-temperature alloy powder remains completely in the solid phase, ultimately retaining the porosity defects of the hollow powder in the part, adversely affecting the alloy's mechanical properties. Therefore, how to accurately and efficiently quantitatively characterize the hollow powder defects in high-temperature alloy powder is a key issue that deserves attention. Existing technologies for characterizing hollow powder defects typically employ traditional metallographic sample preparation methods to obtain two-dimensional planar images of high-temperature powders. When the cut surface accidentally passes through a hollow hole defect, it will be displayed on the metallographic sample. The advantage of this method is that it uses microscopy, which has high resolution. However, its disadvantages are: (1) The cut surface position is random. For the same hole defect, the size difference between the center and the edge of the hole on the two-dimensional image is huge, which will seriously affect the accuracy of the detection results; (2) Only one cut surface can be obtained from a sample, and the probability of obtaining hollow powder is relatively low; (3) Since there is only one two-dimensional plane, the sampling rate of single-layer powder on one plane is also relatively low; (4) The detection efficiency is relatively low, and manual identification is required. With the development of three-dimensional characterization technology, in recent years, traditional three-dimensional characterization techniques such as X-ray micro-nano CT have also begun to be used to characterize hollow powder defects in alloy powders. The advantage of three-dimensional characterization for two-dimensional defect characterization is that it reduces the inaccuracy of results caused by the randomness of sampling. However, it still has certain limitations in the field of high-temperature alloy powder characterization: (1) The imaging resolution is much lower than that of a microscope. The particle size of alloy powder is generally on the order of micrometers, while the size of its internal pore defects is smaller than the particle size of the powder. Compared with titanium alloy and aluminum alloy powders, high-resolution characterization of high-temperature alloy powders with higher density is more difficult; (2) The identification of gaps between powders and internal pores in powders mainly adopts shape recognition, which has a high error rate and low efficiency; (3) The shape recognition and differentiation of non-spherical irregular internal pore defects and powder gaps in powders is worse than that of spherical pore defects; (4) CT imaging is related to the thickness and resolution of the sample. Reducing the thickness can appropriately improve the resolution but affect the sampling rate. Increasing the thickness will significantly reduce the resolution. Different cross-sectional sizes of samples need to be prepared for different requirements. The detection efficiency of single-size samples is low; (5) Characterizing internal pore defects in powders cannot simultaneously characterize the microstructure of the alloy.

[0066] To further illustrate the technical means and effects adopted by the present invention to achieve the intended purpose, the following, in conjunction with the accompanying drawings and preferred embodiments, details the characterization method, apparatus, medium, and equipment for alloy powder internal pore defect samples according to the present invention, as well as its specific implementation methods, structures, features, and effects. In the following description, different "an embodiment" or "an embodiment" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics in one or more embodiments can be combined in any suitable form.

[0067] In this article, the term "and / or" is merely a description of the relationship between related objects, indicating that there can be three relationships, such as A and / or B. Specifically, it can mean that A and B can be included at the same time, A can exist alone, or B can exist alone, and any of the above three situations can be met.

[0068] Example of an alloy powder sample with internal pore defects

[0069] See appendix Figure 1 The alloy powder internal pore defect sample provided in this embodiment of the invention includes a non-metallic container, alloy powder, and a curing material. The alloy powder is spherical and is contained in the container, with the curing material filling the spaces between the alloy powder particles. The alloy powder exhibits a first color under X-ray conditions, the curing material exhibits a second color under X-ray conditions, and the alloy powder internal pore defect exhibits a third color under X-ray conditions, wherein the first, second, and third colors are clearly distinguishable.

[0070] The container is cylindrical or tapered. In this embodiment, the diameter of the cross-sectional circle at different heights of the conical non-metallic container ranges from 0.5 mm to 10 mm, and the height ranges from 10 mm to 50 mm. This allows for the one-time preparation of hollow powder samples with high regional contrast, suitable for efficient and accurate measurement of different X-ray imaging parameters (different penetration depths).

[0071] The curing material comprises the following components by weight: epoxy resin: 90-110 g / m³, dibutyl phthalate: 15-25 g / m³, and ethylenediamine: 1-3 g / m³. The density of the epoxy resin ranges from 1.5 to 2.5 g / m³. 3 .

[0072] The particle size of the alloy powder ranges from 1 μm to 355 μm, and the density of the alloy powder material ranges from 7.0 to 9.5 g / m³. 3 .

[0073] The X-ray generating mechanism is either synchrotron X-ray radiation or an X-ray three-dimensional microscope. Example of a method for preparing alloy powder samples with internal pore defects.

[0074] See appendix Figure 2 The method for preparing an alloy powder sample with internal pore defects provided in this embodiment of the invention includes the following steps:

[0075] Obtain alloy powders of various particle size grades;

[0076] A curing material is added to a non-metallic container; the curing material is in a fluid state.

[0077] Various particle size grades of alloy powder are added to a non-metallic container containing a curing material, so that the alloy powder is distributed in the curing material and forms a dense stack to obtain an intermediate product.

[0078] The intermediate product was left to stand to obtain an alloy powder sample with internal pore defects.

[0079] In the step of adding curing material to a non-metallic container and allowing the curing material to flow, the curing time is greater than or equal to 10 minutes.

[0080] In the step of adding alloy powder of various particle sizes to a non-metallic container containing curing material, so that the alloy powder is distributed in the curing material and forms a dense stack to obtain an intermediate product, the alloy powder of various particle sizes is added to the non-metallic container in multiple batches. The time interval between two consecutive additions of the alloy powder of various particle sizes to the non-metallic container is greater than or equal to 5 minutes. The addition height of the alloy powder of various particle sizes to the non-metallic container of curing material each time is less than 5 mm. After forming a dense stack, the standing time is greater than or equal to 24 hours.

[0081] Example of a characterization method for internal pore defects in alloy powder samples

[0082] See appendix Figure 3 The method for characterizing internal pore defects in alloy powder provided in this embodiment of the invention includes the following steps:

[0083] Step S1: Obtain an image of the alloy powder sample with internal pore defects provided by the present invention under X-ray conditions;

[0084] Step S2: Based on the X-ray image of the alloy powder sample with internal pore defects, distinguish the colors of each region in the X-ray image.

[0085] Step S3: Based on the color of each region in the image under X-ray conditions, determine the nature of the region corresponding to each color. Among them, the third color region is the powder internal pore defect. Under the condition of three-dimensional morphology, accurately count its volume fraction and size to obtain the internal pore defect characteristics of alloy powder.

[0086] Specifically, step S3, which involves determining the properties of the regions corresponding to each color in the X-ray image and obtaining the internal pore defect characteristics of the alloy powder, includes the following steps:

[0087] Step S301: The color of the spherical region in the non-metallic container under X-ray conditions is taken as the first color;

[0088] Step S302: Use the color of the area between each spherical region in the non-metallic container under X-ray conditions as the second color;

[0089] Step S303: Use the color of the region in the middle of each spherical region in the non-metallic container under X-ray conditions as the third color;

[0090] Among them, the first color, the second color, and the third color can be clearly distinguished;

[0091] Step S304: Characterize the corresponding regions of the first color, the second color, and the third color to obtain the internal pore defect characteristics of the alloy powder.

[0092] In the step of distinguishing the colors of different regions in an X-ray image based on an image of an alloy powder sample with internal pore defects, the pixel size is 0.7–10 μm, the field of view is Φ0.5×0.5 mm–Φ10×10 mm, and the voltage range is 50 kV–150 kV.

[0093] Example of a characterization apparatus for internal pore defects in alloy powder samples

[0094] See appendix Figure 4 The alloy powder internal pore defect sample characterization device provided by the present invention includes:

[0095] The image acquisition module is used to acquire images of the alloy powder internal pore defect sample provided by the present invention under X-ray conditions.

[0096] The color differentiation module is used to differentiate the colors of different regions in an X-ray image based on the image of an alloy powder sample with internal pore defects under X-ray conditions.

[0097] The characterization module is used to determine the properties of each region corresponding to each color based on the color of each region in the image under X-ray conditions, and to obtain the internal pore defect characteristics of the alloy powder.

[0098] Computer-readable storage medium embodiments

[0099] The present invention provides a program storing a method for characterizing an alloy powder internal pore defect sample on a computer-readable storage medium. When the program for characterizing an alloy powder internal pore defect sample is executed by a processor, it implements the steps of the method for characterizing an alloy powder internal pore defect sample provided by the present invention.

[0100] Electronic device examples

[0101] The electronic device provided by the present invention includes a memory and a processor. The memory stores a program for characterizing alloy powder internal pore defect samples. When the program for characterizing alloy powder internal pore defect samples is executed by the processor, it implements the steps of the alloy powder internal pore defect sample characterization method provided by the present invention.

[0102] Reference Figure 5 , Figure 5 This is a schematic diagram of the structure of an alloy powder internal pore defect sample characterization device for the hardware operating environment involved in the embodiments of the present invention.

[0103] like Figure 5 As shown, the alloy powder internal pore defect sample characterization device may include: a processor 1001, such as a central processing unit (CPU), a communication bus 1002, a user interface 1003, a network interface 1004, and a memory 1005. The communication bus 1002 is used to enable communication between these components. The user interface 1003 may include a display screen and an input unit such as a keyboard; optionally, the user interface 1003 may also include a standard wired interface or a wireless interface. The network interface 1004 may optionally include a standard wired interface or a wireless interface (such as a Wi-Fi interface). The memory 1005 may be a high-speed random access memory (RAM) or a stable non-volatile memory (NVM), such as a disk drive. The memory 1005 may also optionally be a storage device independent of the aforementioned processor 1001.

[0104] Those skilled in the art will understand that Figure 5 The structure shown does not constitute a limitation on the equipment for characterizing samples with internal pore defects in alloy powders. It may include more or fewer components than shown, or combine certain components, or have different component arrangements.

[0105] like Figure 5 As shown, the memory 1005, which serves as a storage medium, may include an operating system, a data storage module, a network communication module, a user interface module, and a sample characterization program for internal pore defects in alloy powder.

[0106] exist Figure 5In the alloy powder internal pore defect sample characterization device shown, the network interface 1004 is mainly used for data communication with the network server; the user interface 1003 is mainly used for data interaction with the user; the processor 1001 and memory 1005 in the alloy powder internal pore defect sample characterization device of the present invention can be set in the alloy powder internal pore defect sample characterization device. The alloy powder internal pore defect sample characterization device calls the alloy powder internal pore defect sample characterization program stored in the memory 1005 through the processor 1001 and executes the alloy powder internal pore defect sample characterization method provided in the embodiment of the present invention.

[0107] Example 1

[0108] Step 1: The prepared nickel-based superalloy powder with the composition 21Cr-9Mo-5Nb-0.5Al-0.5Ti-5Fe-0.02C-Ni (balance) (mass fraction, %) is sieved into a particle size range of 1-150μm using a mechanical vibrating sieve.

[0109] Step 2: Add the flowable, curable filler to a hollow, cone-shaped non-metallic container and allow it to stand in a liquid state. The addition ratio is 100g epoxy resin: 25g dibutyl phthalate: 1g ethylenediamine. The cone-shaped container has a minimum cross-sectional circle diameter of 1mm, a maximum cross-sectional circle diameter of 3mm, a height of 20mm, and the filler is allowed to stand for 15 minutes.

[0110] Step 3: Add the high-temperature alloy powder to a conical container containing a flowable, curable filler liquid. The powder slides down the sloping inner wall of the container to the bottom for natural particle gradation and dense stacking. The alloy powder is added to the conical container with epoxy resin filler in multiple stages, with each addition being a quantitative amount of 5 mm in height, for a total of 4 additions, with an interval of 5 minutes between each addition.

[0111] Step 4: Let the sample containing alloy powder and filler in the gaps between the powder particles stand still for 24 hours to allow the filler in the gaps to cure naturally, forming a tapered sample of alloy powder with gaps and pores of different cross-sectional sizes filled with filler from top to bottom.

[0112] Step 5: X-ray three-dimensional microscopy imaging was performed with a pixel size of 1 μm, a field of view of Φ1×1 mm, and an X-ray voltage of 100 kV. X-ray imaging and three-dimensional reconstruction were performed on the integral conical variable cross-section sample of the alloy powder with interstitial filler. The alloy region of the alloy powder was the brightest (white), the interstitial parts of the powder were darker (gray), and the pore defects in the center of the powder had the darkest contrast (black). Computer software was used to efficiently, automatically, and accurately obtain the morphology, volume, and size of the powder's external shape and internal pore defects through contrast difference, and quantitative statistics were performed. The volume fraction of internal pore defects in the powder accounted for 0.13% of the volume of the high-temperature alloy powder, with an average size of 5.1 μm.

[0113] Example 2

[0114] Step 1: The prepared nickel-based superalloy powder with the composition 21Cr-9Mo-5Nb-0.5Al-0.5Ti-5Fe-0.02C-Ni (balance) (mass fraction, %) is sieved into a particle size range of 75-150μm using a mechanical vibrating sieve.

[0115] Step 2: Add the flowable, curable filler to a hollow, cone-shaped non-metallic container and allow it to stand in a liquid state. The addition ratio is 100g epoxy resin: 20g dibutyl phthalate: 2g ethylenediamine. The cone-shaped container has a minimum cross-sectional circle diameter of 1mm, a maximum cross-sectional circle diameter of 3mm, a height of 20mm, and the filler is allowed to stand for 15 minutes.

[0116] Step 3: Add the high-temperature alloy powder to a conical container containing a flowable curing filler liquid. The powder slides down the sloping inner wall of the container to the bottom for natural particle gradation and dense stacking. The alloy powder is added to the conical container with epoxy resin filler in multiple batches, with each addition being a quantitative amount of 5 mm in height, for a total of 4 additions, with an interval of 10 minutes between each addition.

[0117] Step 4: Let the sample containing alloy powder and filler in the gaps between the powder particles stand still for 24 hours to allow the filler in the gaps to cure naturally, forming a tapered sample of alloy powder with gaps and pores of different cross-sectional sizes filled with filler from top to bottom.

[0118] Step 5: X-ray three-dimensional microscopy imaging was performed with a pixel size of 0.7 μm, a field of view of Φ0.7×0.7 mm, and an X-ray voltage of 90 kV. X-ray imaging and three-dimensional reconstruction were performed on the integral conical variable cross-section sample of the alloy powder with interstitial filler. The alloy region of the alloy powder was the brightest (white), the interstitial parts of the powder were darker (gray), and the pore defects in the center of the powder had the darkest contrast (black). Computer software was used to efficiently, automatically, and accurately obtain the morphology, volume, and size of the powder's external shape and internal pore defects through contrast difference, and quantitative statistics were performed. The volume fraction of internal pore defects in the powder accounted for 0.2% of the volume of the high-temperature alloy powder, with an average size of 6.5 μm.

[0119] Example 3

[0120] Step 1: The prepared nickel-based superalloy powder with the composition 21Cr-9Mo-5Nb-0.5Al-0.5Ti-5Fe-0.02C-Ni (balance) (mass fraction, %) is sieved into a particle size range of 105-150μm using a mechanical vibrating sieve.

[0121] Step 2: Add the flowable, curable filler to a hollow, cone-shaped non-metallic container and allow it to stand in a liquid state. The addition ratio is 100g epoxy resin: 20g dibutyl phthalate: 2g ethylenediamine. The cone-shaped container has a minimum cross-sectional circle diameter of 1mm, a maximum cross-sectional circle diameter of 3mm, a height of 20mm, and the filler is allowed to stand for 15 minutes.

[0122] Step 3: Add the high-temperature alloy powder to a conical container containing a flowable curing filler liquid. The powder slides down the sloping inner wall of the container to the bottom for natural particle gradation and dense stacking. The alloy powder is added to the conical container with epoxy resin filler in multiple batches, with each addition being a quantitative amount of 5 mm in height, for a total of 4 additions, with an interval of 10 minutes between each addition.

[0123] Step 4: Let the sample containing alloy powder and filler in the gaps between the powder particles stand still for 24 hours to allow the filler in the gaps to cure naturally, forming a tapered sample of alloy powder with gaps and pores of different cross-sectional sizes filled with filler from top to bottom.

[0124] Step 5: X-ray three-dimensional microscopy imaging was performed with a pixel size of 0.7 μm, a field of view of Φ0.7×0.7 mm, and an X-ray voltage of 90 kV. X-ray imaging and three-dimensional reconstruction were performed on the integral conical variable cross-section sample of the alloy powder with interstitial filler. The alloy region of the alloy powder was the brightest (white), the interstitial parts of the powder were darker (gray), and the pore defects in the center of the powder had the darkest contrast (black). Computer software was used to efficiently, automatically, and accurately obtain the morphology, volume, and size of the powder's external shape and internal pore defects through contrast difference, and quantitative statistics were performed. The volume fraction of internal pore defects in the powder accounted for 0.24% of the volume of the high-temperature alloy powder, with an average size of 7.1 μm.

[0125] Although preferred embodiments of the invention have been described, those skilled in the art, upon learning the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the appended claims are intended to be interpreted as including both the preferred embodiments and all changes and modifications falling within the scope of the invention.

[0126] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims of this invention and their equivalents, this invention also intends to include these modifications and variations.

Claims

1. An alloy powder internal bore defect sample, characterized by, The non-metallic container, the alloy powder and the solidified material are included, The alloy powder is spherical, and the alloy powder is contained in the container, The solidified material is filled between the alloy powders in the container; The alloy powder has a first color under X-ray imaging conditions, the solidified material has a second color under X-ray imaging conditions, and the hole defect in the alloy powder has a third color under X-ray imaging conditions, wherein the first color, the second color and the third color can be distinguished. The container is a circular cone with a taper, and the diameter of the cross-sectional circle at different heights ranges from 0.5 mm to 10 mm, and the height ranges from 10 mm to 50 mm. The weight parts of each component in the solidified material include: epoxy resin: 90-110, dibutyl phthalate: 15-25, ethylenediamine: 1-3, wherein the density of the epoxy resin is in the range of 1.5-2.5 g / m 3 , The preparation method of the alloy powder hole defect sample includes the following steps: Obtain alloy powders of multiple particle size grades; Add the solidified material to the non-metallic container, and the solidified material is in a flowing state; Add the alloy powders of multiple particle size grades to the non-metallic container with the solidified material, so that the alloy powders are distributed in the solidified material to form a dense stack, and obtain an intermediate product; Rest the intermediate product to obtain the alloy powder hole defect sample, In the step of adding the alloy powders of multiple particle size grades to the non-metallic container with the solidified material, so that the alloy powders are distributed in the solidified material to form a dense stack, and obtain an intermediate product, the alloy powders of multiple particle size grades are added to the non-metallic container in multiple times, and the time interval between the addition of the alloy powders of multiple particle size grades to the non-metallic container in adjacent two times is greater than or equal to 5 min, and the addition height of the alloy powders of multiple particle size grades to the non-metallic container with the solidified material each time is less than 5 mm, and after the formation of the dense stack, the resting time is greater than or equal to 24 h.

2. The alloy powder internal bore flaw sample of claim 1, wherein, The particle size of the alloy powder ranges from 1 μm to 355 μm, and the density of the material of the alloy powder ranges from 7.0 to 9.5 g / m 3 .

3. The alloy powder internal bore flaw sample of claim 1, wherein, The X-ray generating mechanism is a synchrotron X-ray, or an X-ray three-dimensional microscope.

4. The alloy powder internal bore flaw sample of claim 1, wherein, In the step of adding the solidified material to the non-metallic container, and the solidified material is in a flowing state, the resting time of the solidified material is greater than or equal to 10 min.

5. The method of characterizing internal porosity defects in an alloy powder sample of any of claims 1-4, wherein the method further comprises: The method includes the following steps: Obtain the image of the alloy powder hole defect sample under X-ray conditions according to any one of claims 1-4; According to the image of the alloy powder hole defect sample under X-ray conditions, distinguish the colors of each region in the image under X-ray conditions; According to the colors of each region in the image under X-ray conditions, determine the properties of each color corresponding region, and obtain the hole defect characteristics of the alloy powder.

6. The method of claim 5, wherein the alloy powder internal porosity defect sample characterization method is characterized by, The step of determining the properties of each color corresponding region according to the colors of each region in the image under X-ray conditions, and obtaining the hole defect characteristics of the alloy powder specifically includes the following steps: The color of the spherical region in the non-metallic container under the X-ray conditions is the first color; The color of the region between each spherical region in the non-metallic container under the X-ray conditions is the second color; The color of the region between each spherical region in the non-metallic container under the X-ray conditions is the third color; The first color, the second color, and the third color can be obviously distinguished. The corresponding areas of the first color, the second color, and the third color are characterized to obtain the internal hole defect characteristics of the alloy powder.

7. The method of claim 5, wherein the alloy powder internal porosity defect sample characterization method is characterized by, In the process of distinguishing the colors of the areas in the image under the X-ray condition according to the image of the internal hole defect sample of the alloy powder under the X-ray condition, the pixel size is 0.7-10 μm, the field of view range is Φ 0.5*0.5 mm-Φ 10*10 mm, and the voltage range is 50 kV-150 kV.

8. The apparatus for characterizing internal porosity defects in a sample of alloy powder as recited in any of claims 1-4, wherein, The method comprises the steps of: An image acquisition module is configured to acquire an image of the internal hole defect sample of the alloy powder under an X-ray condition. A color distinguishing module is configured to distinguish the colors of the areas in the image under the X-ray condition according to the image of the internal hole defect sample of the alloy powder under the X-ray condition. A characterization module is configured to determine the properties of the areas corresponding to the colors according to the colors of the areas in the image under the X-ray condition, and obtain the internal hole defect characteristics of the alloy powder.

9. A computer-readable storage medium, characterized in that, The computer readable storage medium stores a program of an internal hole defect sample characterization method of an alloy powder, and the program of the internal hole defect sample characterization method of the alloy powder, when executed by the processor, realizes the steps of the internal hole defect sample characterization method of the alloy powder according to any one of claims 5-7.

10. An electronic device, comprising: The memory stores a program of an internal hole defect sample characterization method of an alloy powder, and the program of the internal hole defect sample characterization method of the alloy powder, when executed by the processor, realizes the steps of the internal hole defect sample characterization method of the alloy powder according to any one of claims 5-7.

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