Method for screening alloy fatigue resistance based on high flux and fatigue-resistant amorphous alloy

Abstract

The application discloses a method for screening alloy fatigue resistance based on high flux and a Cu-Zr-Al ternary anti-fatigue amorphous alloy. The method for screening alloy fatigue resistance based on high flux comprises the following steps: setting a mask plate on a substrate to divide the surface of the substrate into multiple sub-regions; adopting a physical vapor deposition co-sputtering method to deposit different metal element targets on the surface of the substrate at one time to obtain an alloy whose metal element content changes with the position of the surface of the substrate, and the alloy compositions of different sub-regions are different; performing dynamic nanoindentation tests on each sub-region under the same condition, recording the first mutation time of the displacement amplitude of each test point, and screening the alloy composition of the sub-region with the maximum first mutation time. The atomic ratio composition of the Cu-Zr-Al ternary anti-fatigue amorphous alloy is Cu 74.4 Zr 17.9 Al 7.7 or Cu 75.9 Zr 17.1 Al7.

Description

Technical Field

[0001] This invention relates to the field of alloy fatigue resistance testing, specifically to a method for high-throughput screening of alloy fatigue resistance and fatigue-resistant amorphous alloys. Background Technology

[0002] Amorphous alloys are special metallic alloy materials obtained by ultra-rapid cooling of high-temperature melts. Structurally, amorphous alloys lack a long-range ordered crystalline structure, exhibiting instead an amorphous, non-crystalline structure. Amorphous alloys exhibit many excellent mechanical properties, such as high elastic strain, high specific strength, high fracture toughness, and high wear resistance.

[0003] Fatigue is a phenomenon in which the mechanical properties of engineering materials decrease with external loads during use, severely affecting their service life. For metallic alloys, fatigue failure refers to the failure phenomenon where the alloy undergoes irreversible permanent deformation and eventually fractures under cyclic stress. Fatigue failure typically occurs after a material has repeatedly experienced a certain number of stress cycles, and can even occur when the stress is far below the fracture strength.

[0004] Before the development of a series of bulk amorphous alloy systems, it was difficult to prepare bulk samples that met national or ASTM standards for fatigue testing, thus hindering the systematic study of the fatigue properties of amorphous alloys. Only after the development of bulk amorphous alloys did researchers begin to conduct extensive studies on their fatigue performance. However, currently only a few amorphous alloy compositions exhibit high fatigue performance, which significantly limits the industrialization of bulk amorphous alloys in engineering applications.

[0005] Excellent fatigue resistance is one of the key prerequisites for the application of engineering materials in aerospace and industrial fields. Therefore, the development of amorphous alloy systems with excellent fatigue resistance has become one of the difficulties and hot topics in this field. It is urgent to accelerate the development process of new amorphous alloy materials with excellent fatigue resistance.

[0006] Currently, numerous studies have been conducted on the fatigue behavior of Zr-based bulk amorphous alloys, primarily using bending deformation and uniaxial tensile or compressive deformation loading conditions for fatigue testing. Due to the influence of glass-forming ability on amorphous alloys and their more difficult machining compared to traditional alloys, three-point and four-point bending fatigue testing methods are widely used in the study of the fatigue properties of bulk amorphous alloys. Traditional fatigue testing typically requires a sufficient number of samples with well-defined geometries, which is sometimes difficult to achieve. Therefore, in the past few decades of fatigue research on amorphous alloys, these traditional experimental methods have been based on a trial-and-error approach. Characterizing only one composition at a time is time-consuming and inefficient, and with changes in alloy composition and the increase in the number of elements in the alloy, these trial-and-error methods significantly increase research costs.

[0007] In contrast to trial and error, high-throughput experiments, as a crucial component of the Materials Genome New Materials Development Program, transform the traditional sequential iterative process into parallel experiments. Through rapid multi-component material preparation, high-throughput characterization of properties and structures, phase diagrams can be constructed, material properties optimized, and new materials rapidly screened—a novel strategy for new material development. Although current high-throughput methods primarily utilize thin-film samples, considering the long-range disordered atomic arrangement and dislocation-free grain boundaries of amorphous alloys, thin-film samples can essentially reflect the physical properties, particularly mechanical properties, of bulk samples. This provides a unique advantage for high-throughput experimental strategies in developing new amorphous alloy materials with excellent mechanical properties.

[0008] However, current high-throughput characterization of the mechanical properties of amorphous alloy thin film samples focuses on elastic modulus and hardness. Due to the size limitations of thin film samples and the inapplicability of traditional fatigue testing methods, a high-throughput characterization method suitable for the fatigue resistance of amorphous alloy thin film samples remains unknown. Summary of the Invention

[0009] In view of the above-mentioned technical problems and the shortcomings of the field, the present invention provides a method for high-throughput screening of alloy fatigue resistance, which can efficiently measure the fatigue resistance of alloys with different chemical compositions and quickly screen out alloy chemical compositions with excellent fatigue resistance.

[0010] The specific technical solution is as follows:

[0011] A method for high-throughput screening of alloy fatigue resistance includes:

[0012] A mask is set on the substrate to divide the substrate surface into multiple sub-regions;

[0013] Using physical vapor deposition (PVD) co-sputtering, alloys with varying metal element content across different substrate locations are deposited on the substrate surface in a single deposition process using targets with different metal elements. The alloy compositions deposited on different sub-regions of the substrate surface are different.

[0014] Dynamic nanoindentation tests were performed on each sub-region under the same conditions. The time of the first abrupt change in displacement amplitude at each test point was recorded, and the alloy composition of the sub-region where the maximum value of the first abrupt change time was selected.

[0015] The method for screening the fatigue resistance of alloys based on high throughput can be described in which the dynamic nanoindentation test can be achieved by applying a periodic fluctuating load to a constant static load.

[0016] In the method for screening the fatigue resistance of alloys based on high throughput, the maximum value of the additional periodic fluctuation load is preferably less than the static load.

[0017] The method for screening the fatigue resistance of alloys based on high throughput can have all sub-regions having the same shape and area.

[0018] In the method for screening the fatigue resistance of alloys based on high throughput, the alloy thickness deposited in each sub-region can be equal.

[0019] The method for screening the fatigue resistance of alloys based on high throughput can deposit alloys with a thickness of 0.05 to 10 micrometers in each sub-region.

[0020] The method for screening the fatigue resistance of alloys based on high throughput can achieve an alloy surface roughness of less than 1 nanometer in each sub-region.

[0021] The method for high-throughput screening of alloy fatigue resistance, wherein the alloy may include at least two of the following constituent elements: Cu, Zr, Fe, Co, Ni, Ti, and Al.

[0022] As a general inventive concept, this invention also provides a Cu-Zr-Al ternary fatigue-resistant amorphous alloy, the atomic ratio of which is Cu 74.4 Zr 17.9 Al 7.7 or Cu 75.9 Zr 17.1 Al7.

[0023] Compared with the prior art, the beneficial effects of this invention are as follows:

[0024] This invention utilizes a dynamic nanoindentation testing method, which can perform fatigue tests with an arbitrary number of cycles. By obtaining the curve of the number of cycles (time) versus the displacement amplitude, the fatigue resistance of each indentation test point is obtained. Based on the set indentation test points, the corresponding atomic ratios of alloying elements are obtained, forming a one-to-one correspondence between alloy composition and fatigue resistance. This allows for the rapid and efficient screening of the atomic ratios of alloying elements with the best fatigue resistance, i.e., the alloy with the best fatigue resistance. Attached Figure Description

[0025] Figure 1 A schematic diagram of the apparatus for physical vapor deposition co-sputtering deposition of a high-throughput sample library provided in the embodiment;

[0026] Figure 2 The spatial distribution map of different elements in the high-throughput sample library prepared for the example is shown below.

[0027] Figure 3 A schematic diagram showing the distribution of 16 circular regions on the high-throughput sample library provided for this embodiment;

[0028] Figure 4 A schematic diagram of the indentation test process provided for an embodiment;

[0029] Figure 5 The image shows the contour plot of the fatigue resistance of the high-throughput sample prepared for the example, as a function of elemental composition. Detailed Implementation

[0030] The present invention will be further described below with reference to the accompanying drawings and specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention.

[0031] A method for high-throughput screening of fatigue resistance properties of amorphous alloys includes:

[0032] A high-throughput sample library was obtained by using physical vapor deposition co-sputtering to deposit corresponding alloy elements on a substrate based on targets of different elements.

[0033] Multiple indentation test points were set on the surface of the high-throughput sample library. The content of alloy elements corresponding to each indentation test point was measured by energy dispersive spectroscopy, thereby obtaining the alloy composition corresponding to the indentation test point.

[0034] Dynamic nanoindentation is used to perform indentation tests at each indentation test point. This method can add a sinusoidal dynamic load component to the quasi-static load and then probe the sample surface. In order to perform fatigue tests with an arbitrary number of cycles, the cycle number-displacement amplitude curve obtained from the indentation test results is used to determine the cycle number corresponding to the sudden change in displacement amplitude at each indentation test point. The maximum cycle number corresponding to the sudden change in displacement amplitude is selected, which is the one with the best fatigue resistance.

[0035] The indentation test point corresponding to the maximum fatigue resistance is used as the screening indentation test point, and the alloy composition corresponding to the screening indentation test point is the alloy composition with the highest fatigue resistance in the high-throughput sample library.

[0036] This invention employs a dynamic nanoindentation method to perform indentation tests at each indentation test point. Based on the results of the dynamic nanoindentation test, a continuously determined displacement amplitude is obtained. Any sudden change in amplitude can be associated with nano-failure. The displacement amplitude change at each indentation test point is obtained, the number of cycles corresponding to the sudden change in displacement amplitude is recorded, and the maximum value with fatigue resistance is selected.

[0037] Furthermore, multiple indentation test points were set on the surface of the high-throughput sample library, including:

[0038] Multiple horizontal regions are divided on the surface of the high-throughput thin film sample library. Within each horizontal region, multiple sub-regions are further divided, and indentation test points are selected from each sub-region. Setting sub-regions facilitates the plotting of coordinate points on the high-throughput sample library, ensuring accurate correlation between fatigue resistance and alloy element content. The division process can be achieved by setting a mask.

[0039] The dynamic nanoindentation method provides an opportunity to continuously determine the displacement amplitude. Furthermore, the indentation test result is a sample time-displacement amplitude curve. Based on a set frequency, time is converted into the number of cycles, resulting in a curve of cycle count versus displacement amplitude. Locations where abrupt changes in displacement amplitude occur are identified, and the corresponding cycle counts are recorded.

[0040] Furthermore, the dynamic nanoindentation method is used to perform indentation tests at each indentation test point. The parameters for the indentation test are as follows: to ensure overall stable mechanical contact between the indenter and the sample surface, the load amplitude of the sinusoidal load component must be selected to be less than the quasi-static load of the indenter. There is no fixed indentation rate; the static indentation load is 100 μN, the dynamic load is 70 μN, the holding time is 1800 seconds, and the loading frequency during the test is 220 Hz. Therefore, the total number of cycles during the holding time is 3.96 × 10⁻⁶. 5 .

[0041] Furthermore, the nanoindentation indenter used in the indentation test is a Berkovich indenter.

[0042] Furthermore, the physical vapor deposition co-sputtering method for depositing corresponding elements on a substrate based on different elemental targets includes: depositing elements with different atomic ratios on the substrate by adjusting the sputtering power and / or sputtering angle of different elemental targets to obtain a high-throughput sample library, wherein the element content of the high-throughput sample library shows an increasing or decreasing trend along a set method.

[0043] Furthermore, the alloys in the high-throughput sample library are any of the following: binary alloys, ternary alloys, quaternary alloys, pentagonal alloys, hexagram alloys, heptagonal alloys, octagonal alloys, or even alloys containing more chemical elements.

[0044] Preferably, the alloys in the high-throughput sample library are ternary alloys, and the ternary alloys are Cu-Zr-Al ternary alloys.

[0045] Furthermore, the alloy thickness in the high-throughput sample library is 50 nanometers to 10 micrometers.

[0046] Furthermore, the roughness of the high-throughput sample library is less than 1 nanometer.

[0047] Furthermore, the elements in the high-throughput sample library are any two or more of Cu, Zr, Fe, Co, Ni, Ti, Al, etc.

[0048] Furthermore, the substrate material is any one of single-crystal silicon and quartz, but is not limited to these. The purpose of selecting the substrate material is to ensure that the prepared high-throughput sample library has smooth and flat properties, meeting the mechanical property testing conditions.

[0049] Furthermore, the physical vapor deposition co-sputtering can be any one of magnetron sputtering, vapor deposition, or ink printing, and is not limited to this.

[0050] In view of the lack of current high-throughput methods for characterizing the fatigue resistance of thin film alloy samples, this invention provides specific embodiments.

[0051] A method for high-throughput screening of fatigue resistance properties of amorphous alloys includes:

[0052] (1) Obtain a substrate and at least two targets capable of forming an alloy.

[0053] (2) A high-throughput sample library is formed by depositing alloying elements with different atomic ratios on the substrate surface using physical vapor deposition co-sputtering technology. The alloying elements with different atomic ratios are arranged in an increasing or decreasing trend from top to bottom in the sample library. The various positions on the surface of the high-throughput sample library are represented by horizontal and vertical axes.

[0054] In a preferred embodiment, the increasing or decreasing trend is arranged according to a compositional gradient, i.e., the atomic percentage of different elements. Taking a copper-zirconium-aluminum ternary alloy as an example, the alloy composition can continuously vary from 100% Cu-0% Zr-0% Al to 33% Cu-33% Zr-33% Al and then to 0% Cu-100% Zr-0% Al.

[0055] (3) Multiple indentation test points were set based on the horizontal and vertical coordinates of the surface of the high-throughput sample library, and the alloy element content corresponding to each indentation test point was measured by energy dispersive spectroscopy.

[0056] (4) Divide the above high-throughput sample library into several circular regions arranged according to elemental composition. Perform nanoindentation tests on each region, check each curve, find the places where the displacement amplitude changes abruptly, and record the corresponding number of cycles. Select the region with the maximum number of cycles, which is the region with the best fatigue resistance.

[0057] (5) The indentation test point corresponding to the maximum number of cycles is used as the screening indentation test point. The alloy elements and their contents corresponding to the screening indentation test point constitute the alloy with the best fatigue resistance in the high-throughput sample library.

[0058] Example:

[0059] 1. Preparation of a high-throughput sample library of Cu-Zr-Al ternary alloys:

[0060] A high-throughput sample library was synthesized via physical vapor deposition co-sputtering. Three sputtering targets were used: pure zirconium (C target), copper (D target), and aluminum (A target). Figure 1 As shown, copper (target D) metal faces the substrate, while aluminum (target A) and pure zirconium (target C) are at 60-degree angles to the substrate. The elemental gradient distribution is achieved by adjusting the sputtering power of each target: 40W for target A, 120W for target C, and 80W for target D. Alternatively, at the same sputtering power, the gradient distribution is achieved by adjusting the distance between the substrate and the sputtering target.

[0061] The sputtering parameters provided in the specific embodiments of the present invention are such that the basic pressure in the chamber is less than 10. -5 The working pressure was 0.5 Pa, and the argon flow rate was 30 standard cubic centimeters per minute (SCCM). Deposition was carried out for 120 minutes.

[0062] The alloy element content of the indentation test points in the high-throughput sample library obtained by deposition was measured by energy-dispersive spectroscopy (EDS). To meet the requirements for mechanical property testing, atomic force microscopy (AFM) was used for measurement. The roughness of the sample library was approximately 0.816 nm, and the thickness was approximately 800 nm. Figure 2 This is a chemical composition gradient coverage map of the high-throughput sample library prepared in this embodiment, as shown below. Figure 2 As shown, copper is 81–74 at.%, zirconium is 20–13 at.%, and aluminum is 9–4 at.%.

[0063] The method provided in this application for dividing the surface of a high-throughput sample library into circular sub-regions is as follows: the high-throughput sample library is divided into 16 circular sub-regions with a diameter of 5 mm, and three indentation test points are selected from each circular sub-region. Figure 3 This is a schematic diagram of the high-throughput sample library region division provided by the present invention, as shown below. Figure 3 As shown, the center distance between two adjacent circular regions is 7 mm. The 16 regions are symmetrically and evenly distributed on the sample library. The sample library has 4 horizontal regions from top to bottom, and each horizontal region has 4 sub-regions.

[0064] 2. Perform high-throughput screening, such as... Figure 4 As shown:

[0065] 2.1 Place the high-throughput sample library obtained in step 1 flat into the nanoindentation tester to fix it on the test platform and prevent the sample from sliding during the test.

[0066] 2.2 The surface of the sample library was observed to be smooth and flat using a nanoindentation instrument, ensuring that the mechanical property test was carried out normally.

[0067] 2.3. Adjusting test parameters: To ensure stable mechanical contact between the indenter and the sample surface, the amplitude of the sinusoidal load component must be less than the quasi-static load of the indenter. No fixed indentation rate is used; the static indentation load is 100 μN, the dynamic load is 70 μN, the holding time is 1800 seconds, the loading frequency is 220 Hz, and the corresponding number of cycles is 3.96 × 10⁻⁶. 5 .

[0068] 2.4, such as Figure 4 The indentation cycle count-displacement amplitude curve shown is based on the curve obtained in step 2.3. It represents the cycle count corresponding to the first abrupt change in displacement amplitude at each indentation test point. The maximum cycle count corresponding to the first abrupt change in displacement amplitude is selected, indicating the region with the best fatigue resistance. The cycle count results corresponding to the first abrupt change in dynamic nanoindentation testing of the 16 sub-regions are shown in Table 1.

[0069] Table 1

[0070] <![CDATA[1.10×10 5 ]]> <![CDATA[1.11×10 5 ]]> <![CDATA[1.24×10 4 ]]> <![CDATA[4.96×10 4 ]]> <![CDATA[9.99×10 4 ]]> <![CDATA[3.79×10 4 ]]> <![CDATA[1.74×10 5 ]]> <![CDATA[1.19×10 5 ]]> <![CDATA[1.57×10 5 ]]> <![CDATA[1.28×10 5 ]]> <![CDATA[1.74×10 5 ]]> <![CDATA[1.39×10 5 ]]>

[0071] 2.5. Statistically analyze the number of cycles at each indentation test point. By integrating the data, obtain a distribution map of the fatigue resistance performance of the high-throughput sample library. The height represents the magnitude of fatigue resistance; the higher the height, the better the fatigue resistance performance. Figure 5 The fatigue resistance at the indentation test points at coordinates (8, 12) and (10, 8) in the high-throughput sample library is 1.74 × 10⁻⁶. 5It has the best fatigue resistance. Figure 2 As can be seen from the data, when the coordinates of the high-throughput sample library are (8, 12) and (10, 8), the content of the alloying element is Cu. 74.4 Zr 17.9 Al 7.7 at.% and Cu 75.9 Zr 17.1 Al7 at.%, therefore the alloy in this high-throughput sample library is Cu. 74.4 Zr 17.9 Al 7.7 and Cu 75.9 Zr 17.1 Al7 exhibits the best fatigue resistance, thus completing the screening for fatigue resistance performance.

[0072] In addition, the inventors of this case also conducted experiments with other raw materials, process operations, and process conditions described in this specification, referring to the aforementioned implementation process, and obtained relatively ideal results in all of them.

[0073] This invention's method, besides being applicable to amorphous alloys, is also suitable for single-crystal and polycrystalline alloys, as well as various other material samples. This is because the method employs dynamic nanoindentation and the MATLAB function (findchangepts) to obtain the fatigue resistance of each indentation test point. Based on the set indentation test points, alloy elements with different atomic ratios in a high-throughput thin-film sample library are matched one-to-one with the measured fatigue resistance, thus quickly and efficiently screening out the alloy element atomic ratio with the best fatigue resistance from the high-throughput sample library. This dynamic nanoindentation method for obtaining fatigue resistance is not limited to the sample's properties, but is based solely on the sample's inherent properties. Furthermore, the displacement amplitude is related to the sample's properties, particularly its hardness and elastic modulus. Moreover, the method employed in this invention is applicable not only to thin-film samples but also to small-sized bulk samples and small-sized devices. Currently, this invention appears to have a wide range of applications, few limitations, high development efficiency, and a foundation for industrial application, making it suitable for appropriate promotion.

[0074] Furthermore, it should be understood that after reading the above description of the present invention, those skilled in the art can make various alterations or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims.

Claims

1. A method for screening the fatigue resistance of alloys based on high-throughput screening, characterized in that, include: A mask is set on the substrate to divide the substrate surface into multiple sub-regions; Using physical vapor deposition co-sputtering, alloys with varying metal element content across different substrate locations are obtained by depositing metal elements onto the substrate surface in a single step using targets with different metal elements. The alloy compositions deposited on different sub-regions of the substrate surface are different. Dynamic nanoindentation tests were performed on each sub-region under the same conditions: static load was 100 μN, dynamic load was 70 μN, holding time was 1800 seconds, loading frequency was 220 Hz, the first abrupt change time of displacement amplitude at each test point was recorded, and the alloy composition of the sub-region where the first abrupt change time was the maximum was selected. The dynamic nanoindentation test is achieved by applying a periodic fluctuating load to a constant static load; The maximum value of the additional periodic fluctuating load is less than the static load.

2. The method for screening the fatigue resistance of alloys based on high-throughput screening according to claim 1, characterized in that, Each sub-region has the same shape and area.

3. The method for screening the fatigue resistance of alloys based on high-throughput screening according to claim 1, characterized in that, The alloy thickness deposited in each sub-region is equal.

4. The method for assessing the fatigue resistance of alloys based on high-throughput screening according to claim 1 or 3, characterized in that, The thickness of the alloy deposited in each sub-region is 0.05~10 micrometers.

5. The method for screening the fatigue resistance of alloys based on high-throughput screening according to claim 1, characterized in that, The surface roughness of the alloy deposited in each sub-region is less than 1 nanometer.

6. The method for screening the fatigue resistance of alloys based on high-throughput screening according to claim 1, characterized in that, The alloy comprises at least two of the following elements: Cu, Zr, Fe, Co, Ni, Ti, and Al.

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