A high-throughput method for the preparation and characterization of amorphous composites

Abstract

The embodiment of the application provides a high-throughput preparation and characterization method of amorphous composite material, and relates to the field of amorphous composite material. The method is that alloy melt is introduced into the conical cavity of the mold through suction casting method to prepare a solid conical sample; the conical sample is cut along the radial direction, and at least one of the following characterization analyses is carried out: the microstructure of the whole section is characterized to obtain the correlation between the microstructure and the diameter size; the section is characterized by X-ray diffraction to obtain the correlation between the phase structure and the diameter size; the mechanical properties of the section are characterized to obtain the correlation between the mechanical properties and the diameter size; the section is characterized to obtain the DSC curve of the corresponding structure to obtain the correlation between the volume fraction of precipitated phase and thermal properties. The method is simple and easy to operate, and can complete the evolution and characterization of the microstructure of a certain composition with the cooling rate at one time, and effectively improves the development efficiency of the optimal composition.

Description

Technical Field

[0001] This application relates to the field of amorphous composite materials, and more specifically, to a high-throughput preparation and characterization method for amorphous composite materials. Background Technology

[0002] To address the issues of room-temperature brittleness and strain softening in amorphous alloys, an amorphous composite material with an austenitic B2-CuZr phase as the in-situ primary crystalline phase has been successfully developed in CuZr-based alloy systems. During tensile deformation, the ordered cubic B2 phase in this amorphous composite material undergoes a martensitic transformation to generate a monoclinic (B19') martensitic phase, resulting in excellent macroscopically uniform tensile plasticity and significant work hardening ability—a phenomenon known as "transformation-induced plasticity" (TRIP). Currently, research on TRIP-toughened amorphous composites mainly focuses on Zr-based, Ti-based, and Mg-based materials. With advancements in technology, research into developing new compositions of TRIP-toughened amorphous composites is attracting significant attention.

[0003] The traditional method involves preparing samples one by one according to different dimensions to obtain the critical size range from amorphous alloys to amorphous composites, and from amorphous composites to fully crystalline materials. This method is not only time-consuming but also wastes a lot of human and material resources. Therefore, the traditional method of obtaining the critical size of amorphous composites based on preparation of samples one by one limits the rate of material development and research.

[0004] It is of great significance to prepare and study the solidification behavior of phase transformation toughened amorphous composites using high-throughput methods, such as determining the critical size range in which the B2-CuZr phase is dispersed in the amorphous matrix without the formation of other brittle phases. Summary of the Invention

[0005] The purpose of this application is to provide a high-throughput preparation and characterization method for amorphous composite materials. This method is simple and easy to implement, and can complete the evolution and characterization of the microstructure of a certain component with cooling rate in a short time, effectively improving the efficiency of optimal component development and facilitating in-depth research on solidification behavior and phase transformation toughening mechanism.

[0006] In a first aspect, embodiments of this application provide a high-throughput preparation and characterization method for amorphous composite materials, which includes the following steps:

[0007] The alloy melt is injected into a conical cavity of a mold using a suction casting method to prepare a solid conical specimen; the conical specimen is then cut radially and subjected to at least one of the following characterization analyses:

[0008] a. Characterize and analyze the microstructure of the entire cross-section to obtain the correlation between the microstructure and diameter of the conical specimen;

[0009] b. Perform X-ray diffraction characterization analysis on different diameter positions of the cross-section to obtain the correlation between the phase structure and diameter of the conical sample;

[0010] c. Characterize and analyze the mechanical properties at different diameter positions of the cross-section to obtain the correlation between the mechanical properties and diameter of the conical specimen;

[0011] d. Samples were taken from different diameter locations on the cross section and DSC tests were performed to obtain the DSC (Differential Scanning Calorimetry) curves of the corresponding tissues, so as to obtain the correlation between the volume ratio of precipitated phase and thermal properties of the conical sample.

[0012] In the above technical solution, the method of this application fully integrates theories such as alloy melt flow and heat transfer during solidification. By adjusting the conical mold cavity, conical samples (amorphous alloys or amorphous composite materials) of different lengths can be obtained. Each conical sample has a different diameter and solidification temperature gradient, and the radial direction is uniform. The radial direction of any diameter position of the conical sample is uniform and isotropic, which can accurately reflect and represent the microstructure uniformity of a cylindrical sample of any diameter, reflecting the characteristics of high-throughput preparation. In contrast, traditional wedge-shaped samples have anisotropic cooling rates, and the microstructure formed by only two-dimensional heat transfer cannot represent the critical formation size of cylindrical samples.

[0013] By cutting the sample along the axial direction, since different diameter positions of the conical sample correspond to different cooling rates, high-throughput and rapid characterization of the microstructure, phase structure and macroscopic properties obtained at different cooling rates can be achieved, and the correlation between microstructure, phase structure, mechanical properties and diameter size can be analyzed.

[0014] Therefore, this method is simple and easy to implement, and can complete the evolution and characterization of the microstructure of a certain component with cooling rate in a short time, effectively improving the efficiency of optimal component development and facilitating in-depth research on solidification behavior and phase transformation toughening mechanism.

[0015] In one possible implementation, characterization analysis a is performed using an optical microscope or a scanning electron microscope;

[0016] By analyzing the microstructure images obtained through characterization, the diameter range corresponding to the all-amorphous microstructure of the conical sample, the diameter range corresponding to the amorphous composite microstructure, and the diameter range corresponding to the all-crystalline phase microstructure can be obtained, thereby determining the critical size for the formation of amorphous composite materials.

[0017] In the above technical solution, the evolution process of the microstructure morphology of alloys with different diameters (corresponding to different cooling rates) can be characterized and analyzed in a single high-throughput manner.

[0018] In one possible implementation, characterization analysis b is performed using an X-ray diffractometer.

[0019] By analyzing the XRD patterns obtained from characterization, the diameter ranges corresponding to the completely amorphous matrix, the mixed matrix, and the completely crystalline precipitation of the conical sample are determined, thus dividing the conical sample into an amorphous material region, an amorphous composite material region, and a crystalline material region along the axial direction.

[0020] The above technical solutions can conveniently and quickly determine the amorphous material forming ability, amorphous composite material forming ability, and crystalline material forming ability of an alloy composition.

[0021] In one possible implementation, characterization analysis c is performed using a hardness tester;

[0022] The hardness distribution of the conical sample and its diameter are analyzed by hardness analysis at different diameter locations; optionally, the preparation size of the amorphous composite material with the target precipitated phase volume percentage is obtained by combining characterization analysis a.

[0023] In the above technical solution, the volume percentage and dispersion degree of the amorphous composite material relative to the crystalline phase at a certain diameter can be conveniently and quickly determined.

[0024] In one possible implementation, characterization analysis d is performed using a differential scanning calorimeter;

[0025] The temperature field distribution was obtained as the volume percentage of solidified phase gradually increased during the cooling process. Combined with characterization analysis c, the mechanical behavior of the amorphous composite material with the target precipitated phase volume percentage was obtained.

[0026] In one possible implementation, the diameter of the conical specimen ranges from 1 to 15 mm.

[0027] In the above technical solution, the conical specimens within this diameter range can reflect the phase transformation of the material.

[0028] In one possible implementation, the mold is a water-cooled copper mold, and the mold cavity includes, from top to bottom, a molten pool area mold cavity, a riser area mold cavity, and a conical mold cavity connected in sequence. The conical mold cavity is vertically arranged, with the upper end being the coarse end and the lower end being the fine end. The alloy melt enters the conical mold cavity from the molten pool area mold cavity through the riser area mold cavity under the suction casting action.

[0029] In the above technical solution, the method of this application is to prepare conical specimens using a copper mold suction casting method. This method utilizes negative pressure to directly draw the alloy melt into a water-cooled copper mold for cooling. Because the time for the alloy melt to transfer into the water-cooled copper mold is short, and the water-cooled copper mold has excellent thermal conductivity and heat dissipation, a high cooling rate can be achieved, enabling rapid cooling of the alloy melt to obtain a conical specimen. Furthermore, the mold cavity design allows the alloy melt to quickly enter the conical mold cavity and rapidly cool to form a conical specimen. The specimen preparation process is relatively simple and easy to operate. The conical mold cavity has its coarse end at the top and its fine end at the bottom. This design is consistent with the main direction of alloy melt flow, which is conducive to the flow of supercooled melt, reduces turbulence and gas inclusions, thereby improving the filling rate and forming alloy samples with fewer pores and full filling. Conversely, if the fine end of the conical mold cavity is at the top and the coarse end is at the bottom, the length of the conical sample must be greatly reduced to obtain a qualified sample with full filling. At the same time, the design of the mold cavity, which is wider at the top and narrower at the bottom, can achieve a large temperature gradient in the vertical direction and ensure the monotonicity of the temperature gradient, so that the microstructure and diameter of the formed composite material are scientifically correlated.

[0030] In one possible implementation, a conical pad is also included, which is disposed within the conical mold cavity, and there is a gap of 0.05 to 0.15 mm between the conical pad and the surface of the conical mold cavity.

[0031] In the above technical solution, the conical mold cavity, located in the conical region above the conical pad, is used to fill the alloy melt to form a conical sample. By adjusting the length of the conical pad and the taper of the conical mold cavity, the diameter and length of the conical region can be controlled, thus obtaining conical samples of amorphous alloys and their composite materials with different lengths and diameters. The sample size can be controlled through a simple mold structure. Moreover, there is a certain gap between the surface of the conical pad and the conical mold cavity to ensure smooth gas flow during suction casting, achieving negative pressure suction casting in the conical mold cavity.

[0032] In one possible implementation, the diameter of the riser cavity is 3–5 mm.

[0033] In the above technical solution, the riser with a diameter of 3 to 5 mm provides tension support for the molten alloy, ensuring that the molten alloy enters the interior of the copper mold through copper mold suction casting to form the microstructure of amorphous alloy and amorphous composite material, rather than the molten alloy flowing into the conical cavity of the copper mold due to gravity after melting because the riser diameter is too large.

[0034] In one possible implementation, the master alloy is weighed proportionally, and the vacuum level is maintained at 10. -3 ~10 -4After Pa, the alloy melt is obtained by fully melting under argon protection using a non-consumable arc melting method.

[0035] In the above technical solution, the method involves rapidly heating the master alloy to a liquid state using an electric arc under inert gas protection, and then using negative pressure to directly draw the molten alloy melt into a water-cooled copper mold for cooling. Attached Figure Description

[0036] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments of this application will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0037] Figure 1 A schematic diagram of the structure of a mold provided in an embodiment of this application;

[0038] Figure 2 A photograph of the conical sample prepared in Example 1;

[0039] Figure 3 The image shows the cross-sectional microstructure of the conical sample prepared in Example 1.

[0040] Figure 4 for Figure 3 Enlarged view of φ5.5;

[0041] Figure 5 for Figure 3 Enlarged view of φ8;

[0042] Figure 6 The XRD patterns of the conical sample prepared in Example 1 at different diameter positions are shown.

[0043] Figure 7 The temperature field distribution inside the mold cavity when the alloy is cooled to a solidified volume percentage of 1.7% during the preparation of the conical sample in Example 1;

[0044] Figure 8 The temperature field distribution inside the mold cavity when the alloy was cooled to a solidified volume percentage of 31.2% during the preparation of the conical specimen in Example 1.

[0045] Figure 9 The temperature field distribution inside the mold cavity when the alloy is cooled to a solidified volume percentage of 84.6% during the preparation of the conical specimen in Example 1.

[0046] Figure 10 The temperature field distribution inside the mold cavity when the alloy is cooled to 100% solidification volume percentage during the preparation of the conical sample in Example 1;

[0047] Figure 11 The image shows the cross-sectional microstructure of the conical sample prepared in Example 2.

[0048] Figure 12 for Figure 11 The diagram shows the hardness variation at the centerline position of the conical sample with different diameters (the inset shows the corresponding amorphous matrix);

[0049] Figure 13 for Figure 11 The diagram shows the hardness distribution of different diameter regions of the conical sample.

[0050] Icons: 100 - Cylindrical body; 110 - Molten pool area cavity; 120 - Riser area cavity; 130 - Conical cavity; 140 - Threaded area cavity; 200 - Conical pad. Detailed Implementation

[0051] Phase formation in amorphous composites toughened by the "phase transformation-induced plasticity" effect is a highly complex thermodynamic and kinetic process. In the development of phase transformation-toughened amorphous composites, mechanical properties are typically improved by controlling the cooling rate or sample size to adjust the size, volume percentage, and distribution of the metastable crystalline parent phase in the amorphous matrix. However, the method of preparing individual samples for large-scale amorphous composite development, characterizing the evolution of material microstructure with cooling rate, determining the precipitation mechanism of the reinforcing phase, and finding the optimal preparation size for reinforcing phase dispersion have revealed significant limitations.

[0052] To address the shortcomings of existing technologies, this application explores a high-throughput preparation and characterization method for large-size phase transformation-induced plasticity amorphous composite materials. The method primarily employs a high-vacuum melting process to prepare the alloy melt. By modifying the inner cavity of a copper mold to a conical shape and inserting a conical copper core of appropriate size, a single conical sample can be prepared. This single conical sample can then exhibit the isomorphic microstructure and morphological characteristics of amorphous alloys and their composites at different sizes. This method is simple, efficient, and has broad application prospects for the development of amorphous composite materials.

[0053] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions in the embodiments of this application will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0054] The high-throughput preparation and characterization method of amorphous composite materials according to embodiments of this application will be described in detail below.

[0055] This application provides a high-throughput preparation and characterization method for amorphous composite materials, which includes the following steps:

[0056] (1) Prepare a mold with a conical cavity.

[0057] Please refer to Figure 1 The mold includes a cylindrical body 100, which has a mold cavity arranged vertically along the axis. The mold cavity consists of the following components connected from top to bottom: molten pool area mold cavity 110, riser area mold cavity 120, conical mold cavity 130, and threaded area mold cavity 140. The molten pool cavity 110 can be a spherical groove located on the upper surface to accommodate a certain amount of alloy melt; the riser cavity 120 can be cylindrical and vertically arranged, with its two ends used to connect the molten pool cavity 110 and the conical cavity 130; the conical cavity 130 is conical and vertically arranged, with a coarse upper end and a fine lower end; the threaded cavity 140 can be cylindrical and vertically arranged, and its surface has threads to facilitate connection with an external suction casting device to form a negative pressure inside the cavity; the alloy melt enters the conical cavity 130 from the molten pool cavity 110 through the riser cavity 120 under suction casting to form a conical sample. Typically, the main body of the mold can be a two-lobed mold, a three-lobed mold, a four-lobed mold, a five-lobed mold, or a six-lobed mold.

[0058] The surfaces of the mold cavity 110 in the molten pool area, the mold cavity 120 in the riser area, and the conical mold cavity must all be polished to a roughness ≤R0.8. This ensures that the crystalline phase in the amorphous composite material is uniformly nucleated and dispersed within the sample, preventing heterogeneous nucleation near the mold cavity surface due to roughness. It also prevents the growth of nuclei on the outer circumference of the sample within the mold cavity, which would result in uneven microstructure and affect the mechanical properties and critical dimension characterization of the alloy. The conical mold cavity 130 can be controlled to have a length range of 50–100 mm and a diameter range of 0.1–15 mm, depending on requirements. The diameter of the riser area mold cavity 120 can be 3–5 mm.

[0059] The mold may also include a conical pad 200 disposed within the conical mold cavity 130. The shape of the conical pad 200 matches the shape of the lower end of the conical mold cavity 130, and there is a gap of 0.05 to 0.15 mm between the placed conical pad 200 and the corresponding surface of the conical mold cavity 130. By placing a conical pad 200 of the required length at the lower end of the conical mold cavity 130, the length requirements of different conical samples can be met.

[0060] In this embodiment, the mold is a circulating water-cooled copper mold. The cylindrical body and the conical pad 200 are both made of oxygen-free copper, and the cylindrical body is provided with a circulating water-cooling channel.

[0061] (2) Preparation of high-throughput conical specimens

[0062] After weighing the master alloy according to the proportion, the vacuum degree is maintained at 10. -3 ~10 -4 After Pa, the alloy melt is fully melted under argon protection using a non-consumable arc melting method to obtain the alloy melt. The alloy melt is then cast into the conical cavity of the mold using a copper mold suction casting method to prepare a solid conical sample.

[0063] As one implementation method, the oxide scale on the surface of the master alloy is ground clean with a grinding wheel and then ultrasonically cleaned in anhydrous ethanol. The master alloy is then weighed according to the specified ratio and placed in an electric arc furnace for complete melting using a non-consumable arc melting method under argon protection. During suction casting, the vacuum level of the electric arc furnace is maintained at 10. -3 ~10 -4 Pa, and fill with 0.02-0.07MPa high-purity argon gas, melt the master alloy and then turn on the suction casting device to allow the alloy melt to fully fill the conical mold cavity.

[0064] After the mold cools, disassembling the copper mold yields conical specimens with a maximum length of 85 mm and a diameter gradient of 1–15 mm. This preparation method is applicable to the preparation of specimens of almost all amorphous alloys and their composites, such as Ti-based, TiCu-based, TiNi-based, CuZr-based, Zr-based, and Mg-based alloys, as well as specimens of other alloy systems.

[0065] Based on the formula for cooling rate and amorphous alloy formation size: d is the sample diameter in cm. Based on the cooling rate (K / s), the critical cooling rate for conical specimens with diameters ranging from 1 to 15 mm can be calculated to be 4.4 K / s to 10 K / s. 3 K / s. The cooling rate at different diameter positions of the conical sample exhibits circumferential isotropic behavior. Therefore, the above-mentioned device and method can prepare samples with different solidification cooling rates in one step, which is convenient for systematically studying the microstructure and property relationship characteristics of amorphous composite materials under different cooling rates. At the same time, the device and preparation method are also applicable to the preparation of samples of all other alloy systems.

[0066] (3) High-throughput characterization of conical specimen properties

[0067] The conical specimen was cut radially and at least one of the following characterization analyses was performed:

[0068] a. Characterize and analyze the microstructure of the entire cross-section to obtain the correlation between the microstructure and diameter of the conical specimen.

[0069] Typically, characterization is performed using an optical microscope or a scanning electron microscope. The diameter range corresponding to the fully amorphous structure, the mixed structure, and the fully precipitated phase structure of the conical sample is analyzed by the microstructure images obtained from the characterization, thereby obtaining the critical size for the formation of the amorphous composite material.

[0070] b. Perform X-ray diffraction characterization analysis on different diameter positions of the cross-section to obtain the correlation between the phase structure and diameter of the conical sample.

[0071] Typically, X-ray diffraction is used for characterization. The XRD patterns obtained from the characterization are analyzed to determine the diameter range corresponding to the completely amorphous matrix, the mixed matrix, and the completely crystalline precipitate of the conical sample. This allows the conical sample to be divided into amorphous material region, amorphous composite material region, and crystalline material region along the axial direction.

[0072] c. Characterize and analyze the mechanical properties at different diameter positions of the cross-section to obtain the correlation between the mechanical properties and diameter of the conical specimen.

[0073] Typically, a hardness tester is used for characterization; the hardness distribution of the conical sample at different diameter locations is analyzed to determine the correspondence between the hardness distribution and the diameter; optionally, combined with characterization analysis a, the fabrication size of the amorphous composite material with the target precipitate volume percentage is obtained; specifically, a hardness tester is used to analyze and characterize the distribution of mechanical properties such as hardness of the precipitate in the amorphous region and the amorphous composite material region at different diameters and their correspondence with the microstructure, thereby directly obtaining the fabrication size of the amorphous composite material with the optimal precipitate volume percentage.

[0074] d. DSC tests were performed on samples taken at different diameter locations of the cross section to obtain the DSC curves of the corresponding tissues, so as to obtain the correlation between the volume ratio of precipitated phase and thermal properties of the conical sample.

[0075] Typically, differential scanning calorimetry (DSC) is used for characterization; the temperature field distribution is obtained as the volume percentage of solidified solids gradually increases during the cooling process. Combined with characterization analysis, the fabrication dimensions and mechanical properties of amorphous composite materials with the target precipitate volume percentage are obtained. Specifically, DSC curves of the microstructure corresponding to different diameter positions are analyzed using DSC to obtain the characteristic temperature of the material and the correlation between the precipitate volume percentage and thermal properties.

[0076] The features and performance of this application will be further described in detail below with reference to the embodiments.

[0077] Example 1

[0078] This embodiment provides a high-throughput preparation and characterization method for amorphous composite materials, the specific process of which is as follows:

[0079] 1. Prepare conical specimens of amorphous alloy composite materials.

[0080] Please refer to Figure 1 In this embodiment, the main body of the copper mold consists of two identical semi-cylinders, which are fixed together by two nuts. Looking at the longitudinal section (the plane along the axial direction of the semi-cylinders) of the main body of the copper mold, the diameter of the riser cavity is 4mm, the length of the conical cavity is 86mm, and the diameter of the thick end is 12mm.

[0081] Select Zr 43 Cu 42.75 Al5Ag5Ti2Hf 0.5 Ni 0.5 Sn 0.5 Co 0.5 Nb 0.25 The alloy was prepared by converting the atomic molar ratios shown in the alloy composition to mass ratios, and selecting pure metallic elements with a purity higher than 99.9% for ingredient mixing. Under an argon protective atmosphere, a pre-alloy of Zr, Hf, Ti, Nb, Ni, and Co was first melted twice, followed by four more meltings with other elements Cu, Ag, Al, and Sn to ensure the homogeneity of the alloy composition. Figure 1 A copper mold is used, and a conical pad with a length of 20 mm and a diameter of approximately 3.5 mm at the thicker end (corresponding to a diameter of 3.6 mm at the conical mold cavity) is placed at the narrow end. The overall diameter of the conical pad is approximately 0.1 mm smaller than the inner surface diameter of the conical mold cavity, forming a gap of approximately 0.05 mm between the conical pad and the inner surface of the conical mold cavity. This ensures smooth flow of the casting gas. Conical samples are obtained using the copper mold suction casting method. Figure 2 As shown. The conical sample has a diameter of 12 mm at the coarse end and 3.5 mm at the fine end, enabling high-throughput preparation of samples with amorphous composite material composition and diameters ranging from 3.5 to 12 mm. This avoids the tedious process of preparing cylindrical samples of different diameters one by one to obtain the optimal volume percentage of precipitated phase + amorphous phase, and also avoids unnecessary waste of raw materials.

[0082] 2. High-throughput characterization of the microstructure and properties of the conical sample.

[0083] The prepared conical specimen is cut open along the axial direction (for vertically set specimens, the longitudinal direction is used), and then cold-mounted with epoxy resin to fix the specimen to be characterized, so that its cross-section can be ground and polished.

[0084] a. High-throughput characterization of tissue morphology.

[0085] The overall morphology of the sample was characterized using confocal microscopy. The morphology of the conical sample from the thin end to the thick end is as follows: Figures 3-5As shown in the image.

[0086] from Figure 3 It can be seen that the conical sample with a diameter of 4 mm or less is almost entirely amorphous; the area with a diameter of 5–9 mm is a mixture of precipitates and amorphous structure, and the volume percentage and size of the precipitates gradually increase with the increase of the alloy preparation diameter; the area with a diameter greater than 10 mm is almost entirely crystalline. Especially based on Figure 4 and Figure 5 The magnified images of the tissue morphology at the 5.5 mm and 8 mm diameter locations show that: Figure 4 The precipitate at the 5.5 mm diameter position shown is diffuse and fine, with a size of less than 100 μm; Figure 5 At the location shown with a diameter of 8 mm, the precipitated phase begins to aggregate and grow, increasing in size to over 200 μm and reaching a volume percentage of 50%.

[0087] b. High-throughput characterization of phase structure.

[0088] XRD characterization was performed on the structural features at the desired diameter locations selected in the longitudinal section of the obtained conical sample. In this embodiment, three diameter locations were selected for XRD characterization, namely regions with diameters of 4 mm, 7 mm, and 10 mm. The XRD patterns are shown below. Figure 6 As shown.

[0089] from Figure 6 As can be seen, the sample at a diameter of 4 mm exhibits a completely amorphous structure, characterized by diffuse scattering peaks typical of amorphous structures. At a diameter of 7 mm, the sample contains a simple cubic B2-CuZr phase, a monoclinic B19'-CuZr martensite phase, and a certain volume percentage of amorphous matrix phase, exhibiting a combination of more significant crystalline phase diffraction peaks on the amorphous peaks, indicating an amorphous composite material. At a diameter of 10 mm, the sample primarily consists of simple cubic B2-CuZr and AlCu2Zr phases, with only a small amount of amorphous matrix phase present, exhibiting very low diffuse scattering peak intensity for the amorphous phase and very high peak intensity for the crystalline phase diffraction peaks. Based on this alloy composition, the optimal preparation size should be between 4 and 7 mm to obtain a microstructure consisting of a single B2-CuZr phase and an amorphous matrix.

[0090] c. High-throughput characterization of mechanical properties such as hardness.

[0091] The hardness distribution at different distances (corresponding to different diameters) at the thinner end of the conical specimen was characterized, with five tests performed at each location and the average value taken. The results show that as the diameter of the conical specimen increases, the hardness value increases from low to high, then decreases again. This is consistent with the "free volume theory" of amorphous alloy formation.

[0092] d. High-throughput characterization of thermal properties.

[0093] To more intuitively describe and understand the temperature gradient changes during the cooling and solidification process of conical amorphous alloys and their composites, differential scanning calorimetry (DSC) was used to test conical samples (3.5 mm diameter at the narrow end and 12 mm diameter at the wide end). The results were analyzed using Procast simulation software. Figures 7-10 As shown. Figures 7-10 After the conical mold cavity was 100% filled with amorphous alloy, the solidification volume percentage during cooling was 1.7% ( Figure 7 ), 31.2% Figure 8 ), 84.6% Figure 9 ) and 100% Figure 10 Temperature field distribution at various locations of the conical sample during the test.

[0094] Depend on Figures 7-10 It can be seen that the transverse temperature gradient distribution is smaller at the thin and thick ends of the conical sample, i.e., at the locations with larger and smaller cooling rates. This result is consistent with the transverse hardness distribution from the center to the edge at diameters of 1.5 mm and 2.5 mm. Within the middle size range of the cone (diameter 5–10 mm), the temperature gradient shows a trend of lower edge temperature than center temperature. This simulation result is the same as the transverse hardness distribution trend (larger hardness value at the center and smaller hardness value at the edge) at the 2 mm diameter location.

[0095] Example 2

[0096] This embodiment provides a high-throughput preparation and characterization method for amorphous composite materials, the specific process of which is as follows:

[0097] 1. Conical specimens were prepared using a method similar to that in Example 1, specifically selecting Zr... 36 Cu 50 Ti 14 The alloy is used to prepare conical specimens with diameters ranging from 1 to 7 mm by placing a 15 mm long conical pad at the lower end of a conical mold cavity. The conical specimens have a coarse end diameter of 7 mm and a fine end diameter of 1 mm.

[0098] 2. High-throughput characterization of the microstructure and properties of the conical sample.

[0099] The prepared conical sample was cut open and processed using a method similar to that in Example 1.

[0100] c. High-throughput characterization of mechanical properties such as hardness.

[0101] Figure 11 This is a cross-sectional microstructure image of the conical specimen (the specimen was photographed at different locations using a laser confocal microscope, and the overall microstructure was obtained by stitching the images together). Figure 12 This section describes the hardness distribution at different distances (corresponding to different diameters) at the narrower end of the conical specimen. Five tests were performed at each location, and the average value was taken. Figure 12 It can be seen that as the diameter of the conical sample increases, the hardness value increases from low to high and then decreases again. This is consistent with the "free volume theory" retained during the formation of amorphous alloys, that is, the content of free volume in the alloy is determined by the cooling rate; the higher the cooling rate, the more free volume is frozen. The relationship between the cooling rate and the critical diameter of the sample is as follows: the cooling rates for sample diameters of 1.5 mm, 2 mm, 2.5 mm, 3 mm, and 5 mm are 444 K / s, 250 K / s, 160 K / s, 111 K / s, and 40 K / s, respectively. As the size of the amorphous alloy increases, the cooling rate decreases exponentially.

[0102] Therefore, as the size of the conical amorphous alloy sample increases, the frozen free volume content is lower than that of samples with smaller diameters, meaning the hardness value of the smaller diameter samples is lower. When the diameter reaches the range of 2 mm to 4 mm (cooling rate decreases), the relaxation degree of the amorphous alloy increases, and the percentage of free volume frozen during solidification decreases relatively, resulting in a higher hardness value for samples of this size. As the diameter increases to 5 mm (cooling rate continues to decrease), crystalline phases precipitate in the amorphous alloy, and its hardness value shows a decreasing trend, indicating that this crystalline phase is a soft phase relative to the amorphous alloy.

[0103] Figure 13 This shows the hardness distribution at the edge and center of a conical specimen at different diameters. Figure 13 It can be seen that the edge of the conical sample is closer to the copper mold, resulting in a faster cooling rate and a higher percentage of free volume, while the center of the sample is farther from the copper mold, resulting in a slower cooling rate and a lower percentage of free volume. This trend is evident at a diameter of 2 mm, where the hardness value is lower at the edge and higher at the center. Due to the smaller diameter of 1.5 mm, the overall cooling rate is higher, the percentage of free volume is more uniform, and the hardness value is lower. As the cooling rate decreases to 111 K / s (diameter 3 mm), the percentage of free volume at the edge and center of the sample becomes more even, and the difference in hardness value between the edge and center is smaller. However, due to the reduced cooling rate, a softer crystalline phase begins to precipitate in the alloy at the center of the 3 mm diameter sample, resulting in a lower hardness value at this size, 0.5 mm from the center.

[0104] In summary, the high-throughput preparation and characterization method of amorphous composite materials in this application is simple and easy to implement. It can complete the evolution and characterization of the microstructure of a certain component with cooling rate in a short time, effectively improve the efficiency of optimal component development, and facilitate in-depth research on solidification behavior and phase transformation toughening mechanism.

[0105] The above description is merely an embodiment of this application and is not intended to limit the scope of protection of this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the scope of protection of this application.

Claims

1. A high-throughput preparation and characterization method for amorphous composite materials, characterized in that, It includes the following steps: The alloy melt is injected into a conical cavity of a mold using a suction casting method to prepare a solid conical specimen. The conical specimen is then cut radially and subjected to the following characterization analysis: a. Characterize and analyze the microstructure of the entire cross-section to obtain the correlation between the microstructure and diameter of the conical specimen; b. Perform X-ray diffraction characterization analysis on different diameter positions of the cross-section to obtain the correlation between the phase structure and diameter of the conical sample; c. Characterize and analyze the mechanical properties at different diameter positions of the cross-section to obtain the correlation between the mechanical properties and diameter of the conical specimen; d. DSC tests were performed on samples taken at different diameter locations of the cross-section to obtain the DSC curves of the corresponding tissues, so as to obtain the correlation between the volume ratio of the precipitated phase and the thermal properties of the conical sample.

2. The high-throughput preparation and characterization method for amorphous composite materials according to claim 1, characterized in that, For characterization analysis a, characterization is performed using an optical microscope or a scanning electron microscope; By analyzing the microstructure images obtained through characterization, the diameter range corresponding to the fully amorphous microstructure, the diameter range corresponding to the mixed microstructure, and the diameter range corresponding to the fully precipitated phase microstructure of the conical sample are determined, thereby obtaining the critical size for the formation of the amorphous composite material.

3. The high-throughput preparation and characterization method for amorphous composite materials according to claim 1, characterized in that, For characterization analysis b, X-ray diffraction was used for characterization. By analyzing the XRD patterns obtained from characterization, the diameter range corresponding to the completely amorphous matrix, the diameter range corresponding to the mixed matrix, and the diameter range corresponding to the completely crystalline precipitation of the conical sample are analyzed, thereby dividing the conical sample into an amorphous material region, an amorphous composite material region, and a crystalline material region along the axial direction.

4. The high-throughput preparation and characterization method for amorphous composite materials according to claim 1, characterized in that, For characterization analysis c, a hardness tester is used for characterization; The hardness distribution of the conical sample was analyzed at different diameter locations to determine the relationship between the hardness distribution and the diameter.

5. The high-throughput preparation and characterization method for amorphous composite materials according to claim 4, characterized in that, Based on characterization analysis a, the preparation dimensions of the amorphous composite material with the target precipitated phase volume percentage were obtained.

6. The high-throughput preparation and characterization method for amorphous composite materials according to claim 4, characterized in that, For characterization analysis d, differential scanning calorimetry was used for characterization; The temperature field distribution was obtained as the volume percentage of solidified phase gradually increased during the cooling process. Combined with characterization analysis c, the mechanical behavior of the amorphous composite material with the target precipitated phase volume percentage was obtained.

7. The high-throughput preparation and characterization method for amorphous composite materials according to claim 1, characterized in that, The diameter of the conical specimen ranges from 1 to 15 mm.

8. The high-throughput preparation and characterization method for amorphous composite materials according to claim 1, characterized in that, The mold is a water-cooled copper mold, and the mold cavity includes, from top to bottom, the following connected components: the molten pool area mold cavity, the riser area mold cavity, and the conical mold cavity. The conical mold cavity is vertically arranged, with the upper end being the thicker end and the lower end being the thinner end. The alloy melt enters the conical mold cavity from the molten pool area mold cavity through the riser area mold cavity under the suction casting action.

9. The high-throughput preparation and characterization method for amorphous composite materials according to claim 8, characterized in that, It also includes a conical pad disposed within the conical mold cavity, wherein the conical pad has a gap of 0.05 to 0.15 mm between it and the surface of the conical mold cavity.

10. The high-throughput preparation and characterization method for amorphous composite materials according to claim 8, characterized in that, The diameter of the riser cavity is 3~5 mm.

11. The high-throughput preparation and characterization method for amorphous composite materials according to claim 1, characterized in that, Weigh the master alloy according to the specified ratio, maintaining a vacuum level of 10. -3 ~10 -4 After Pa, the alloy melt is obtained by fully melting under argon protection using a non-consumable arc melting method.

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