阅读说明：本技术 一种高通量合金制备、表征及成分设计方法 (High-throughput alloy preparation, characterization and component design method ) 是由 刘锋 王子 秦子珺 王泽鑫 于 2019-08-30 设计创作，主要内容包括：本申请公开了一种高通量合金及其制备方法、表征方法与测试方法,其中,测试方法包括：获取测试合金,测试合金包括基础合金块体、外围元素体与多种组合合金块体,每一组合合金块体包括变量元素以及定量元素,其中变量元素由一种添加元素和一种适应元素组成,定量元素包括至少一种元素；将测试合金进行预定处理；将处理后的测试合金进行切割、制样以及分析检测,以获取多种合金的物理及化学性能。本申请通过一个测试合金设置多种组合合金块体,并且每中组合合金块体中均设置有一个变量元素,能够同时获取大量的不同的合金组分,从而通过一次实验即可分析大量的合金,缩短实验时间以及资源,进一步加快合金的设计与优化。(The application discloses a high-throughput alloy and a preparation method, a characterization method and a test method thereof, wherein the test method comprises the following steps: obtaining a test alloy, wherein the test alloy comprises a basic alloy block body, a peripheral element body and a plurality of combined alloy block bodies, each combined alloy block body comprises a variable element and a quantitative element, the variable element comprises an additive element and an adaptive element, and the quantitative element comprises at least one element; carrying out predetermined treatment on the test alloy; and cutting, sampling, analyzing and detecting the treated test alloy to obtain the physical and chemical properties of various alloys. This application sets up multiple combination alloy block through a test alloy to all be provided with a variable element in every combination alloy block, can acquire a large amount of different alloy components simultaneously, thereby can analyze a large amount of alloys through once the experiment, shorten experimental time and resource, further accelerate the design and the optimization of alloy.)

1. A method for testing a high throughput alloy, the method comprising:

obtaining a test alloy, wherein the test alloy comprises a basic alloy block body, a peripheral element body and a plurality of combined alloy block bodies, the combined alloy block bodies are arranged by being attached to the basic alloy block body, the peripheral element body is arranged by surrounding the basic alloy block body and the combined alloy block bodies, each combined alloy block body comprises a variable element and a quantitative element, the variable element is composed of an additive element and an adaptive element, and the quantitative element comprises at least one element;

subjecting the test alloy to a predetermined treatment;

and cutting, sampling, analyzing and detecting the treated test alloy to obtain the physical and chemical properties of various alloys.

2. The method of claim 1, wherein said base alloy blocks in said test alloy are provided in two and juxtaposed relation, said composite alloy block being provided between or on a side of said base alloy blocks remote from each other.

3. The method according to any one of claims 1 or 2, characterized in that the step of obtaining a test alloy is in particular:

according to an isothermal section phase diagram to be researched, carrying out combined design on the combined alloy block, and determining the variable elements and the quantitative elements;

smelting the combined alloy block, and processing, grinding and assembling the base alloy block and the combined alloy block;

welding the sheath by using vacuum electron beam welding equipment to ensure that the interior of the sheath is in a vacuum state, and placing the basic alloy block and the combined alloy block in the sheath;

and (3) tightly combining the basic alloy blocks and the combined alloy blocks together by adopting high-temperature hot isostatic pressing on the welded sheath.

4. The method according to claim 1, characterized in that said step of subjecting said test alloy to a predetermined treatment comprises in particular:

carrying out short-time first-stage aging on the test alloy after thermal consolidation to enable the alloy to quickly diffuse to form a long-range ordered continuous component gradient;

and carrying out secondary aging on the test alloy for a long time to ensure that the alloy reaches local equilibrium to form the test alloy, wherein the temperature requirement in the secondary aging is lower than that of the primary aging.

5. The method according to claim 1, wherein the additive element of the variable elements in the bulk of the combined alloy is an element of the quantitative elements in the other bulk of the combined alloy in a different amount than the amount of the element of the quantitative elements in the other bulk of the combined alloy; or an element not present in said quantitative elements in the other composite alloy blocks; the adaptive element in the variable element changes according to the change of the added element so as to ensure that the element content in the quantitative element in the combined alloy block is unchanged; at least one piece of each of the composite alloy pieces is present in the test alloy.

6. A method of making a high throughput alloy, the method comprising:

according to an isothermal section phase diagram to be researched, carrying out combined design on the combined alloy block, and determining a basic alloy block, variable elements and quantitative elements, wherein the variable elements comprise an additive element and an adaptive element, and the quantitative elements comprise at least one element;

smelting the combined alloy block, and processing, grinding and assembling the base alloy block and the combined alloy block;

welding the sheath by using vacuum electron beam welding equipment to ensure that the interior of the sheath is in a vacuum state, and placing the basic alloy block and the combined alloy block in the sheath;

and (3) tightly combining the basic alloy blocks and the combined alloy blocks together to form the test alloy by adopting high-temperature hot isostatic pressing on the welded sheath.

7. A high-throughput alloy comprising a base alloy mass, a peripheral element matrix disposed against said base alloy mass, and a plurality of composite alloy masses, each of said composite alloy masses comprising a variable element and a quantitative element, wherein said variable element is comprised of an additive element and an adaptive element, and said quantitative element comprises at least one element.

8. The high-throughput alloy of claim 7, wherein the high-throughput alloy is prepared by the method for preparing the high-throughput alloy of claim 6.

9. A method of characterizing a high throughput alloy, the method comprising:

obtaining a high-flux alloy;

selecting a region to be characterized of the high-flux alloy;

dividing the region to be characterized into a plurality of sub-regions, wherein the number of rows and columns of the sub-regions is not less than 10;

regarding each sub-area as an independent alloy area, and performing automatic component acquisition by using a micro-area X-ray fluorescence spectrometer;

analyzing the chemical and physical properties of the high-flux alloy in each sub-region;

respectively characterizing the high-flux alloy in each sub-region through analysis results;

wherein the high-throughput alloy is the high-throughput alloy of claim 7 or 8.

10. The method for characterizing a high-throughput alloy according to claim 9, wherein after the step of analyzing the chemical and physical properties of the high-throughput alloy in each of the sub-regions, the chemical and physical properties of the high-throughput alloy are further established as a data set.

Technical Field

The application relates to the field of chemical materials, in particular to a high-flux alloy and a preparation method, a characterization method and a test method thereof.

Background

Alloy development design often relies on phase diagram measurement, and the development of a phase diagram measurement method realizes a diffusion couple method. The phase diagram, i.e. the phase equilibrium state diagram, can reflect the phase composition and phase change information of a certain material system under certain conditions of temperature, pressure, composition and the like, and is the basis of the relationship of composition-phase-structure-performance in alloy design. At present, experimental phase diagram documents of a multi-component system are rarely reported, so that alloy design and optimization still depend on a trial and error method, and the strengthening effect of alloy elements cannot be fully exerted except for long experimental period and high cost.

There are generally two methods for establishing a phase diagram: experimental determination and thermodynamic calculation. Aiming at the determination of a binary system phase diagram and a ternary system phase diagram, 4 experimental determination methods have been developed; balanced alloy method, diffusion couple method, diffusion ternary node and diffusion multicomponent node method. However, in the experimental determination of the multi-component system phase diagram, even the isothermal section of the local space is a lot of experimental points. If the multi-component alloy phase diagram is determined by using the 4 experimental methods, the traditional diffusion couple method, diffusion ternary node and diffusion multi-component node method are only suitable for binary and ternary alloy block systems, and cannot be applied to the multi-component alloy block system in an expanded way. The balanced alloy method requires preparation and detection of a large amount of multi-element alloy, and is high in cost and low in efficiency. At present, a relevant phase diagram is mainly established by thermodynamic calculation aiming at a multi-element alloy block system, such as a phase diagram calculation method.

The core of the phase diagram calculation method is to predict information such as phase balance in a multi-component system based on experimental results of a binary system and a ternary system, so that the method is difficult to avoid the existence of considerable errors, still needs experimental data verification of the multi-component system, and cannot pass the experimental data verification of a component system.

When the alloy experiment is carried out, particularly the preparation-detection of a large amount of multi-component alloy requires a large amount of time and resources, and the experimental data verification of a multi-component system requires multiplied time and resources, thereby seriously influencing the design and optimization of the alloy.

Disclosure of Invention

The application provides a high-throughput alloy, a preparation method and a test method thereof, which can solve the problem that the design and optimization of the alloy are seriously influenced because experimental data verification of a multi-component system is required when a large amount of alloy data is acquired, namely, multiple times of time and resources are required.

In order to solve the technical problem, the application adopts a technical scheme that: a method for testing a high throughput alloy is provided, the method comprising: obtaining a test alloy, wherein the test alloy comprises a basic alloy block body, a peripheral element body and a plurality of combined alloy block bodies, the combined alloy block bodies are arranged by being attached to the basic alloy block body, the peripheral element body is arranged by surrounding the basic alloy block body and the combined alloy block bodies, each combined alloy block body comprises a variable element and a quantitative element, the variable element comprises an additive element and an adaptive element, and the quantitative element comprises at least one element; carrying out predetermined treatment on the test alloy; and cutting, sampling, analyzing and detecting the treated test alloy to obtain the physical and chemical properties of various alloys.

Wherein, the basic alloy block among the test alloy is provided with two to set up side by side, the combination alloy block sets up in one side that two basic alloy blocks or two basic alloy blocks kept away from each other between the block.

The method comprises the following steps of: according to an isothermal section phase diagram to be researched, carrying out combined design on a combined alloy block, and determining variable elements and quantitative elements; smelting the combined alloy block, and processing, polishing and assembling the basic alloy block and the combined alloy block; welding the sheath by using vacuum electron beam welding equipment to ensure that the interior of the sheath is in a vacuum state, and placing the basic alloy block and the combined alloy block in the sheath; and (4) tightly combining the basic alloy blocks and the combined alloy blocks together by adopting high-temperature hot isostatic pressing on the welded sheath.

The method specifically comprises the following steps of performing preset treatment on the test alloy: carrying out short-time first-stage aging on the test alloy after thermal solidification to enable the alloy to quickly diffuse to form a long-range ordered continuous component gradient; and carrying out long-time secondary aging on the test alloy to ensure that the alloy reaches local balance to form the test alloy, wherein the temperature requirement in the secondary aging is lower than that of the primary aging.

The additive elements in the variable elements in the combined alloy block are elements in quantitative elements in other combined alloy blocks, and the content of the additive elements is different from the content of the elements in the quantitative elements in other combined alloy blocks; or elements not present in the quantitative elements in the other combined alloy blocks; adaptive elements in the variable elements are changed according to the change of the added elements so as to ensure that the content of the elements in the quantitative elements in the combined alloy block is unchanged; at least one block of each alloy combination appears in the test alloy.

In order to solve the above technical problem, another technical solution adopted by the present application is: a method for preparing a high-throughput alloy is provided, which comprises the following steps: according to an isothermal section phase diagram to be researched, carrying out combined design on a combined alloy block, and determining a basic alloy block, variable elements and quantitative elements, wherein the variable elements comprise an additive element and an adaptive element, and the quantitative elements comprise at least one element; smelting the combined alloy block, and processing, polishing and assembling the basic alloy block and the combined alloy block; welding the sheath by using vacuum electron beam welding equipment to ensure that the interior of the sheath is in a vacuum state, and placing the basic alloy block and the combined alloy block in the sheath; and (4) tightly combining the basic alloy blocks and the combined alloy blocks together to form the test alloy by adopting high-temperature hot isostatic pressing on the welded sheath.

In order to solve the above technical problem, the present application adopts another technical solution: the utility model provides a high flux alloy, includes basic alloy block, peripheral element body and multiple combination alloy block, and the combination alloy block pastes and leans on basic alloy block to set up, and peripheral element body encircles basic alloy block and combination alloy block and sets up, and each combination alloy block includes variable element and quantitative element, and wherein variable element comprises an additive element and an adaptation element, and quantitative element includes at least one element.

The length directions of the alloy block body basic alloy block body, the alloy block body combined alloy block body and the element body on the periphery of the alloy block body are consistent.

In order to solve the above technical problem, another technical solution adopted by the present application is: a method of characterizing a high-throughput alloy is provided, the method comprising: obtaining a high-flux alloy; selecting a region to be characterized of the high-flux alloy; dividing a region to be characterized into a plurality of sub-regions, wherein the number of rows and columns of the sub-regions is not less than 10; regarding each sub-area as an independent alloy area, and performing automatic component acquisition by using a micro-area X-ray fluorescence spectrometer; analyzing the chemical property and the physical property of the high-flux alloy in each subregion; respectively characterizing the high-flux alloy in each sub-area through an analysis result; wherein the high-flux alloy is the high-flux alloy.

After the step of analyzing the chemical properties and the physical properties of the high-flux alloy in each sub-area, the chemical properties and the physical properties of the high-flux alloy are further established as a data set, so that the alloy design is guided.

Through the mode, the high-flux alloy, the preparation method and the test method of the high-flux alloy set the combined alloy blocks through one test alloy, and each combined alloy block is provided with one variable element, so that a large number of different alloy components can be obtained simultaneously, a large number of alloys can be analyzed through one-time experiment, the experiment time and resources can be shortened, and the design and optimization of the alloys are further accelerated.

Drawings

FIG. 1 is a schematic view of a planar structure of a high flux alloy according to an embodiment of the present application along a direction perpendicular to its length;

FIG. 2 is a flow chart of a method of making a high throughput alloy according to an embodiment of the present application;

FIG. 3 is a flow chart of a method of testing a high throughput alloy according to an embodiment of the present application;

FIG. 4 is a flow chart of a method of characterizing a high throughput alloy according to an embodiment of the present application.

Detailed Description

In the following description, for purposes of explanation and not limitation, specific details are set forth such as particular system structures, interfaces, techniques, etc. in order to provide a thorough understanding of the present application. It will be apparent, however, to one skilled in the art that the present application may be practiced in other embodiments that depart from these specific details. In other instances, detailed descriptions of well-known devices and methods are omitted so as not to obscure the description of the present application with unnecessary detail.

The testing method of the high-flux alloy is extended by an alloy diffusion ternary junction, wherein the application of the experimental determination method of the phase diagram is extremely important.

Experimental determination method of phase diagram:

common phase diagram measuring methods for binary and ternary alloy block systems mainly include a balanced alloy method, a diffusion couple method and a diffusion multi-element method developed based on a diffusion three-element node.

a. Equilibrium alloy method

The equilibrium alloy method is a conventional and widely used phase diagram measurement method. Preparing an alloy of selected composition by vacuum melting or powder metallurgy; carrying out homogenization heat treatment on the obtained alloy at a certain higher temperature lower than the solidus temperature to eliminate the phenomenon of non-uniform alloy components; then carrying out long-time aging heat treatment on the alloy after the homogenization annealing at certain temperature to form a microstructure containing a balance relation at the corresponding heat treatment temperature; and finally, combining analysis and detection equipment such as X-ray diffraction, an optical microscope, a scanning electron microscope, electron probe micro-area analysis and the like to obtain the information such as the structure, the components and the like of the equilibrium phase at the temperature, and further establishing the phase equilibrium relationship of the detected system. For each formulated alloy, a knit line or a three-phase region knit triangle can be obtained if the nominal composition of the alloy is in the two-phase region or the three-phase region; if the composition of the alloy is in the single-phase region, no tie line can be obtained. The accurate determination of an isothermal section of a ternary phase diagram usually requires a large number of tie lines and three-phase region tie lines, and thus a large number of alloy samples need to be prepared. The equilibrium alloy method is an important phase diagram measuring method, and each alloy sample needs to be subjected to smelting preparation, heat treatment and characterization analysis, so that the efficiency is very low, and the urgent need of perfecting an experimental phase diagram database of a multi-component alloy block system in a short time, such as nickel-based high-temperature alloy, is difficult to meet.

b. Diffusion couple method

The diffusion couple method is used for the phase diagram measurement based on the assumption of local equilibrium, that is, at a certain temperature and pressure, a system does not reach the minimum state of free energy as a whole, but a state in which the free energy is minimum appears in a local region near the interface of the diffusion layer, and thus it can be considered that the system is in an equilibrium state in this local region. The basic preparation process of the diffusion couple is that the surfaces of two or more solid block materials are ground, polished, cleaned and the like, and then form close interface contact under the action of external force. Then, a diffusion layer having a certain thickness is formed by interdiffusion between atoms at a set temperature, that is, a solid solution and a compound phase having a continuous composition change within a certain composition range are formed, so that thousands of alloy compositions having a microscopic resolution can be obtained in one sample. And finally, by combining analysis detection tools such as a scanning electron microscope and electron probe micro-area analysis, a large amount of information such as connecting lines and three-phase area connecting lines required by phase diagram drawing can be obtained, and the rapid determination of the phase diagram is further realized.

c. Diffusion multi-section method

The diffusion multi-element method is updated and developed by the traditional diffusion even and diffusion three-element technology. The diffusion multi-node is a method of arranging a plurality of bulk metals in a predetermined manner to form a plurality of binary diffusion couple and ternary diffusion nodes, and thus has higher efficiency than the conventional diffusion couple method. The ternary nodes in the diffusion polynary nodes can be used for measuring the isothermal section of the ternary phase diagram very quickly, and reliable experimental data are provided for establishing a multi-element thermodynamic database. Through the practice of a plurality of alloy block systems, the high-flux measurement of the ternary system phase diagram by adopting the diffusion multi-element method shows good reliability.

d. Phase diagram calculation method

With the development of computing material science, a powerful tool has been developed for the important branch of material science and material design, and is widely applied to the fields of scientific research and engineering. The core of the phase diagram calculation method is to use experimental results, mainly including a binary phase diagram and a ternary equilibrium correlation system or a phase diagram, and the formation enthalpy, the mixing enthalpy, the specific heat, the activity and the like of the correlation phases to fit/optimize a relational expression of the Gibbs free energy of each phase along with the change of components, temperature and pressure in the whole component range and the range from room temperature to ultrahigh temperature, and form a thermodynamic database according to the relational expression. The phase diagram calculation method is combined with a multi-element alloy thermodynamic database, and thermodynamic calculation of phase fraction, phase composition and lattice fraction of each phase in the multi-element alloy can be realized, so that alloy composition design and process optimization are guided.

Development of diffusion multiplex section:

aiming at binary and ternary alloy block systems, the diffusion multi-element method updates and develops the traditional diffusion even and diffusion ternary element technology. A single diffusion multi-element section comprises a plurality of binary diffusion couple and ternary diffusion sections, so that the preparation-characterization efficiency is higher. Aiming at the selection of the heat treatment system, double aging diffusion multi-element joints are developed.

a. Diffusion multi-element joint

Conventional diffusion cells employ only a primary aging heat treatment after hot isostatic pressing, i.e., a continuous compositional gradient and different microstructures are formed by aging heat treatment at a temperature, e.g., 1000 c/1000 h, for an extended period of time, followed by domain composition and tissue characterization. According to the method, the alloy elements are rapidly diffused to reach a local equilibrium state under the high-temperature condition, such as a nickel alloy block system, of more than or equal to 1000 ℃, so that an isothermal section phase diagram under the temperature condition is measured, but for an intermediate temperature, such as 600-900 ℃, the isothermal section phase diagram needs longer heat treatment time, and the efficiency of the method is reduced under the intermediate temperature condition.

b. Double-aging diffusion multi-element joint

The double-aging diffusion multi-element adopts two-stage aging heat treatment, thus solving the dilemma of the traditional diffusion multi-element under the condition of medium temperature. The basic principle is that the diffusion multi-element is firstly subjected to primary aging (higher temperature) to enable alloy elements to be rapidly diffused to form a long-range continuous component gradient, which is equivalent to the preparation of a large number of alloy samples, and then secondary aging (intermediate temperature) is carried out, which is equivalent to the long-term aging in the traditional diffusion multi-element to achieve local balance, so that the overall heat treatment time is reduced, and the material preparation efficiency is improved. The double-aging diffusion multi-element joint can obtain the phase transformation information while obtaining the isothermal section phase diagram.

c. Zero phase fraction line

Isothermal cross-sectional phase diagrams contain a series of lines that demarcate different phase regions, i.e., phase boundaries. Morral et al superimpose phase boundaries that contain a phase to form a zero phase fraction line for that phase. One component interval of the zero phase fraction line contains this phase and the other component interval does not. On the zero phase fraction line, the mole fraction of this phase is 0. The zero phase fraction line more clearly defines the composition interval in which a certain phase (harmful phase or beneficial phase) exists in the isothermal section phase diagram, and the zero phase fraction line has great guiding significance for the design and optimization of the multicomponent alloy.

At present, under the normal isobaric condition (1 standard atmospheric pressure is 1.01 × 105Pa), the binary system phase diagram in the periodic table is basically measured, the ternary system phase diagram is continuously measured, but the measurement of the multi-component system (the component number n is more than or equal to 4) phase diagram is rarely reported. Taking a 3-element system as an example, a phase diagram needs to be drawn in a three-dimensional coordinate by adding a variable of the temperature T, and an isothermal section (fixed temperature value) of the phase diagram is two-dimensional data. The multi-component system phase diagram needs to be drawn in an n-dimensional space, the isothermal section is (n-1) -dimensional data, and a large number of data points needed by the isothermal section cannot be determined one by one through an experimental mode.

Therefore, it is practical to draw a two-dimensional isothermal cross section of a multi-component alloy block system, which only allows the content of 3 elements including the matrix element to change while ensuring the content of other elements to be unchanged.

Gupta et Al adjusted the contents of Fe, C and B in a Fe-Mn-Cr-Mo-Nb-Al-Si-C-B9-element alloy block system, co-smelted 45 alloys, and drawn an isothermal cross-sectional phase diagram of (Fe-Mn-Cr-Mo-Nb-Al-Si) -C-B by a balanced alloy method. The isothermal cross section is mapped by using a balanced alloy method in a multi-component alloy block system, and two main defects exist, namely the alloy smelting quantity is large, and the analysis and detection work is heavy; secondly, even if the zero phase fraction line drawn by smelting 45 alloys is still inaccurate, the designed composition points are difficult to accurately fall near the zero phase fraction line because the position of the zero phase fraction line is unknown.

Heckl adjusts the contents of three elements of Ni, Re and Ru aiming at a Ni-Co-W-Mo-Cr-Al-Ta-Re-Ru 9-element high-temperature alloy block system, smelts 6 alloys together, draws an NiX-Re-Ru (X represents other 6 elements) isothermal section phase diagram, roughly measures a zero phase fraction line of a TCP phase, but the accuracy is not enough.

In conclusion, the quality and quantity of the data points (i.e., the quantity of the melted alloy) determine the drawing accuracy of the zero phase fraction line, so that the high-throughput preparation and characterization of the alloy are the key points for improving the efficiency and the data consistency.

Referring to fig. 1, fig. 1 is a schematic view of a planar structure of a high flux alloy along a direction perpendicular to a length direction of the high flux alloy according to an embodiment of the present disclosure. In the present application, the high-flux alloy includes a base alloy block W1, a plurality of combined alloy blocks W2-W8, and a peripheral element body W9.

Wherein each of the composite alloy blocks W2-W8 includes a variable element composed of an additive element and an adaptive element, and a quantitative element including at least one element. The peripheral element body W9 is provided around the base alloy block body W1 and the combined alloy block bodies W2-W8, and the length directions of the base alloy block body W1, the combined alloy block bodies W2-W8 and the peripheral element body W9 are the same. In the present embodiment, the number of the basic alloy block bodies W1 is set to 2, and the number of the combined alloy block bodies W2-W8 is set to 15, although there are only 7. Therefore, the number of each combined alloy block W2-W8 can be one or more. For example, the combined alloy blocks W2 are provided with 4 blocks in total, and are respectively adjacent to the other six combined alloy blocks W3-W8. This arrangement allows different diffusion to be provided for different experimental samples because of the different diffusion of the adjacent composite alloy masses W2-W8.

Taking a nickel-based alloy as an example, please refer further to the following table (multicomponent series alloy composition table):

wt％	Ni	Co	W	Mo	Cr	Al	Ti	Ta	Nb	Hf
											W1	Bal.	13	3	3	12	3	4	3	-	0.2
W2	Bal.	28	3	3	12	3	4	3	-	0.2
											W3	Bal.	13	6	3	12	3	4	3	-	0.2
W4	Bal.	13	3	6	12	3	4	3	-	0.2
											W5	Bal.	13	3	3	12	3	6	3	-	0.2
W6	Bal.	13	3	3	12	3	4	8	-	0.2
											W7	Bal.	13	3	3	12	3	4	3	4	0.2
W8	Bal.	13	3	3	12	3	4	3	-	2

in the table, the basic alloy mass W1 includes various elements of the fixed composition. In this embodiment, since the matrix element of the alloy is Ni, the peripheral element body W9 is Ni, and the Ni content in each of the combined alloy blocks W2 to W8 is increased or decreased in accordance with the change of the additive element among the variable elements, and the quantitative element content is kept constant. Therefore, in the present example, the Ni element is an adaptive element among the variable elements of the respective composite alloy masses W2 to W8, and the content thereof is adaptively changed. Co is taken as an additive element in variable elements in the combined alloy block W2, and other parts are quantitative elements, so that the content of Co is changed relative to the content of the basic alloy block W1; in the combined alloy block W3, W is taken as an additive element in variable elements, and the other parts are quantitative elements, so that the content of W is changed relative to the content of W1 in a basic alloy block W1; mo is taken as an additive element in variable elements in the combined alloy block W4, and the other parts are quantitative elements, so that the content of Mo is changed relative to the content of the basic alloy block W1; ti is taken as an additive element in variable elements in the combined alloy block W5, other parts are quantitative elements, and the content of Ti is changed relative to the content of the basic alloy block W1; ta is taken as an additive element in variable elements in the combined alloy block W6, other parts are quantitative elements, and the content of Ta is changed relative to the content of the basic alloy block W1; in the combined alloy block W7, Nb is taken as an additive element in variable elements, and the other parts are quantitative elements, so that a new element Nb is added relative to the basic alloy block W1; in the combined alloy block W8, Hf is an additive element among variable elements, and the other parts are quantitative elements, and the Hf content is changed from that of the base alloy block W1.

In summary, the elements in the variable elements in the combined alloy blocks W2-W6 and W8 are additive elements in quantitative elements in other combined alloy blocks, and the content of the elements is different from the content of the elements in quantitative elements in other combined alloy blocks W2-W8 and in basic alloy block W1; or the variable elements in the combined alloy block W7 are the quantitative elements in the other combined alloy blocks or the elements not present in the basic alloy block W1. The adaptive elements in the variable elements are changed according to the change of the added elements so as to ensure that the element content in the quantitative elements in the combined alloy blocks W2-W8 is unchanged. Of course, in other embodiments, the quantitative element content of each of the composite alloy masses W2-W8 may differ slightly from the basic alloy mass W1, but by an amount less than the amount of the variable element content compared to the same element content in the basic element mass.

The content may be a common content unit such as a weight ratio content, a volume ratio content, an atomic or molecular number ratio content, and the like, and is not limited herein.

By the method, when an alloy performance experiment is required, the high-flux alloy is directly used as a test alloy for the experiment, and the prepared high-flux alloy can be subjected to double aging treatment and then can be subjected to multiple detection characterization methods to extract the alloy material performance. 8 alloys are subjected to diffusion smelting by one alloy, 12 groups of ternary diffusion nodes and 28 groups of binary diffusion nodes can be obtained from the prepared high-flux alloy, and a large number of different alloy components can be obtained simultaneously, so that a large number of alloys can be analyzed through one experiment, the experiment time and resources can be shortened, and the design and optimization of the alloys are further accelerated.

Referring to fig. 2, fig. 2 is a flow chart of a method for preparing a high throughput alloy according to an embodiment of the present disclosure. In this embodiment, the method for preparing the high-throughput alloy comprises:

and step S11, carrying out combined design of the combined alloy blocks according to the isothermal section phase diagram to be researched, and determining variable elements and quantitative elements in the basic alloy blocks and the combined alloy blocks. Wherein the variable element is composed of an additive element and an adaptive element, and the quantitative element includes at least one element. In addition, in this step, it is necessary to design the kind and number of the combined alloy blocks and the positional relationship between the combined alloy blocks and the base alloy blocks, and to determine the arrangement order of the combined alloy blocks.

And step S12, smelting the combined alloy block, and processing, grinding and assembling the basic alloy block and the combined alloy block. It should be noted that, in this step, the base alloy block and the combined alloy block need to be tightly attached to each other, and can be extruded if necessary. The surface of the basic alloy block body in contact with the combined alloy block body needs to be as smooth as possible, so that the basic alloy block body can be better attached. In this step, the preparation of the combined alloy block may be performed using a multi-target magnetron sputtering technique or a high-energy beam laser additive manufacturing technique. The multi-target magnetron sputtering technology is to magnetron sputter 3 alloys onto a substrate simultaneously, and can prepare a component-changing metal coating. Because the component gradient has already been formed during the magnetron sputtering process, the testing of the micro-domain components and structures can be performed only by long-term aging at the temperature of interest. The high-energy beam laser additive manufacturing technology prepares a series of alloys into metal powder in advance. By using the multi-channel powder feeding technology and combining with the set program, the powder proportioning content is prepared, and the block material with gradient components is manufactured. For example, in the above embodiment, if three alloy powders of W1, W2 and W7 are subjected to additive manufacturing according to a set program, alloy samples with varying Co and Nb element contents can be rapidly prepared in large batches.

And step S13, welding the sheath by using vacuum electron beam welding equipment to ensure that the interior of the sheath is in a vacuum state, and placing the basic alloy block and the combined alloy block in the sheath.

And step S14, adopting high-temperature hot isostatic pressing to the welded sheath, and tightly combining the basic alloy blocks and the combined alloy blocks together to form the high-flux alloy. For example, if the nickel-based alloy in the previous embodiment needs to be prepared, 1180 ℃/150MPa/8h process parameters are adopted to ensure that the base alloy block and the combined alloy block are tightly combined together.

In addition, in the above step, design and treatment of a peripheral element body may be further added. The peripheral element body can completely wrap the base alloy block body and the combined alloy block body.

The additive elements in the variable elements in the combined alloy block are elements in quantitative elements in other combined alloy blocks, and the content of the additive elements is different from the content of the elements in the quantitative elements in other combined alloy blocks; or elements not present in the quantitative elements in the other combined alloy blocks. The adaptive elements in the variable elements are changed according to the change of the added elements so as to ensure that the element content in the quantitative elements in the combined alloy block is unchanged. At least one block of each alloy combination appears in the test alloy.

Through the mode, for example, the diffusion multi-element joint in the previous embodiment can be prepared, so that the diffusion multi-element joint is provided with a plurality of alloy samples, and a large number of different alloy components can be obtained at the same time, so that a large number of alloys can be analyzed through one experiment, the experiment time and resources can be shortened, and the design and optimization of the alloys can be further accelerated.

Referring to fig. 3, fig. 3 is a flowchart of a method for testing a high throughput alloy according to an embodiment of the present application. In this embodiment, the method for testing a high-throughput alloy comprises:

step S21: and obtaining a test alloy. The test alloy comprises a basic alloy block body, a peripheral element body and a plurality of combined alloy block bodies, wherein the combined alloy block bodies are arranged by being attached to the basic alloy block body, the peripheral element body surrounds the basic alloy block body and the combined alloy block bodies, each combined alloy block body comprises a variable element and a quantitative element, the variable element is composed of an additive element and an adaptive element, and the quantitative element comprises at least one element. Wherein at least one side of each composite alloy block abuts the test alloy. Wherein, the basic alloy block among the test alloy is provided with two to set up side by side, the combination alloy block sets up in one side that two basic alloy blocks or two basic alloy blocks kept away from each other between the block. This test alloy may be the high throughput alloy in the above-described embodiment. In addition, the test alloy further comprises a peripheral element body, the peripheral element body is arranged around the base alloy block body and the combined alloy block body, the length directions of the base alloy block body, the combined alloy block body and the peripheral element body are consistent, and when the processed test alloy is cut, the test alloy is cut along the length direction perpendicular to the test alloy.

Step S22: the test alloy is subjected to a predetermined treatment. The method specifically comprises the following steps of performing preset treatment on the test alloy: and placing the test alloy in an environment with preset temperature or/and pressure for preset time. In this step, a double aging heat treatment process regime can be designed according to the characteristics of the test alloy. For example, this step can be specifically divided into the following two steps: firstly, carrying out short-time first-stage aging on the test alloy after thermal solidification to quickly diffuse the alloy to form a long-range ordered continuous component gradient; and carrying out long-time secondary aging on the test alloy to ensure that the alloy reaches local balance to form the test alloy. Wherein the temperature requirement in the secondary ageing is lower than the temperature requirement of the primary ageing. The first-order aging is solid solution heat treatment and rapid formation of continuous component gradient, which is equivalent to simultaneously preparing a large amount of alloy through testing the alloy; and (3) secondary aging, namely a long-term thermal exposure experiment, and researching the phase composition of the alloy under the service temperature condition. The temperature and time in each stage of aging can be adjusted according to the requirements, for example, the high-flux alloy in the above embodiment adopts a first-stage aging system of 1180 ℃/1000h, and a second-stage aging system of 700-. It should be noted that the heat treatment schedule is not limited to secondary aging, and can be adjusted according to the system characteristics of the alloy to be tested.

Step S23: and cutting, sampling, analyzing and detecting the treated test alloy to obtain the physical and chemical properties of various alloys. Analytical testing may include microscopic texture and compositional analysis, plotting the zero phase fraction. Besides the traditional phase diagram drawing for thermodynamic simulation, the diffusion coefficient of the tested alloy can be detected for kinetic simulation; detecting the solid solution strengthening and precipitated phase strengthening mechanisms of the analysis alloy such as hardness, elasticity, strength and the like; characterizing the heat conduction coefficient of the alloy to research the orderliness, point defect, element substitution and the like of the alloy; detecting specific heat, thermal expansion coefficient, magnetism and other physical and chemical properties of the tested alloy; and the alloy structure can be represented, and the precise detection of the alloy structure can be carried out to carry out some theoretical simulation to obtain a new phenomenon and the like. The detection is combined, so that a new alloy material can be rapidly developed.

The step S21 can be steps S11-S14 in the previous embodiment.

In fact, in step S22, the mutual diffusion of the component elements at high temperature is utilized by the test alloy to form a continuous component gradient and a corresponding microstructure, which is equivalent to high-throughput measurement of the alloy samples in each micro-area, and the continuous distribution of the alloy samples improves the consistency and reliability of the detection data. In step S23, a large number of high quality data points (corresponding to the number of alloy samples) can be obtained using advanced micro-region characterization techniques, ensuring accurate mapping of the isothermal cross-sectional phase diagram (zero phase fraction line). In addition, the mechanical property of the micro-area under the condition of continuously changing components can be tested by combining the micro-area mechanical testing technology, and the thermal physical parameters of the micro-area can be determined by utilizing a femtosecond laser.

Further combining fig. 1 with the corresponding embodiment, in step S23, the method may include:

step 1, photographing the whole surface of the sample by using the large-area jigsaw function of the scanning electron microscope, and positioning the position of the alloy block.

And 2, magnifying and shooting a diffusion ternary node, such as W1-W2-W7 diffusion ternary node (namely the position where W1, W2 and W7 are attached to each other), wherein a white bright phase exists in a W7 region rich in Nb, and further magnifying to find a region in which the four phases of eta + sigma + gamma' coexist.

And 3, dividing the W1-W2-W7 diffusion three-node interdiffusion area into 80 independent areas, and photographing each area and acquiring components.

In another embodiment, the W1-W2-W7 diffusion three-element mutual diffusion region is divided into a plurality of small regions in a row and column mode, the number of the small regions in the row and column direction is not less than 36, the number of the small regions in the row and column direction is preferably the same, and the number of the small regions in the row and column direction is not less than 6, and the number of the small regions in the row and column direction is the square of a positive integer. Of course, the number of small regions in the row and column directions can be adjusted according to the actual element diffusion situation. Then, the respective small regions are numbered in a predetermined order. The predetermined sequence may be from left to right and then from top to bottom, or other sequences, and only a certain rule is required for the number arrangement. Each small region is considered to be a separate alloy region. And preferably, two-dimensional plane coordinates are established, corresponding to each small area one to one. The division of the small regions can be that the mutual diffusion regions are uniformly dotted through microhardness and the like to obtain nano-indentations distributed in rows and columns, and each nano-indentation is a small region so as to obtain a plurality of small regions. And then, automatically acquiring each small area by using a component characterization device, an organization acquisition device and a performance characterization device, wherein the organization picture is subjected to numerical processing by using a machine learning picture identification technology, and the organization-component-performance data are in one-to-one correspondence according to the coordinates of a two-dimensional plane. Specifically, each small area is subjected to automatic component acquisition by using a micro-area X-ray fluorescence spectrometer, a full-field search engine performs continuous tissue characterization on the whole interdiffusion area, then all tissue photos are spliced into a whole large picture, and each area is subjected to automatic component acquisition by using nano-indentation.

And 4, corresponding the components to the microstructure, drawing a corresponding phase diagram, such as an isothermal section phase diagram of NiX-Co-Nb800 ℃, and obtaining zero phase fraction lines of eta phase and sigma phase. Specifically, the spliced tissue pictures correspond to chemical components and hardness results thereof one by one according to coordinates, a component-tissue-performance relation is established, a data set is established, and more material characterization is performed as required, so that alloy design is guided.

In the above embodiments, the content of the element may be an atomic percentage or a weight percentage.

In addition, in the above embodiments, the nickel-based superalloy is taken as an example for explanation, and besides the nickel-based superalloy, the nickel-based superalloy can also be applied to a multi-component alloy block system with components of not less than 3, such as a cobalt-based superalloy, a high-entropy alloy, a titanium alloy, an aluminum alloy, and the like.

Referring to fig. 4, fig. 4 is a flow chart of a method for characterizing a high throughput alloy according to an embodiment of the present application.

In step S31, a high-throughput alloy is acquired. The high-flux alloy is the high-flux alloy in the embodiment or the high-flux alloy prepared by the preparation method of the high-flux alloy in the embodiment. Taking fig. 1 as an example, in the present embodiment, the following table is assigned:

CSU	Ni	Co	W	Mo	Cr	Al	Ti	Ta	Nb	Hf
											W1	Bal.	13	3	2.9	12.2	3.03	3.96	3.1	-	0.21
W2	Bal.	27.8	3	2.9	12	3.05	4.06	3	-	0.21
											W3	Bal.	13	6.1	2.9	11.8	3.05	3.92	3	-	0.22
W4	Bal.	13.1	3	5.9	12.1	3.05	4.08	3.1	-	0.19
											W5	Bal.	13	2.9	3	12	3.07	6.01	3	-	0.19
W6	Bal.	13	3	2.9	12	3.1	4.04	8.1	-	0.2
											W7	Bal.	13	3	3	11.9	2.98	4.12	3	4.2	0.22
W8	Bal.	12.9	2.9	2.9	12	3.07	4.12	3.1	-	1.99

in step S32, a region to be characterized of the high-flux alloy is selected. For example, in the present embodiment, a cube region is selected at the intersection of W1, W7 and W2 as the region to be characterized.

In step S33, the region to be characterized is divided into a plurality of sub-regions, and the number of rows and columns of the sub-regions is not less than 10. For example, in the present embodiment, the region to be characterized is divided into 81 × 81 regions, that is, 6561 sub-regions in total. Each sub-area is divided by nano-indentation, so that the subsequent steps are convenient to carry out. Each subregion is preferably square and should have an edge length greater than the diffusion distance of the alloying variable. In addition, it should be noted that the number of rows and columns of the plurality of sub-regions need not be equal, and the sub-regions may be divided according to specific situations.

In step S34, each sub-region is treated as an independent alloy region, and automated composition collection is performed using a micro-region X-ray fluorescence spectrometer. The micro-area X-ray fluorescence spectrometer can perform phase identification of a full field of view, and only a few seconds are needed for performing photographing analysis of local components, and the like, so that one sub-area can be processed, the speed is high, and the whole area is obtained.

In step S35, the high-throughput alloy in each sub-region is analyzed for chemical and physical properties. Through the step, the chemical property and the physical property of the alloy represented by each sub-region can be obtained, and the diffusion condition of each element can be analyzed. After this step is performed, the high throughput alloy is further subjected to chemical and physical properties building up as a data set to guide the alloy design. Generally, a full-field SEM is required to perform continuous tissue characterization on the entire area, then all the tissue photographs are stitched into one large integral picture, and automated component acquisition is performed on each area by using nanoindentation. And finally, the spliced tissue pictures correspond to chemical components and hardness results thereof one by one according to coordinates, a component-tissue-performance relation is established, and a data set is established. The following table shows the partial values of the composition, tissue and hardness, corresponding to the intersection of W1, W7 and W2 in this example after establishing coordinates:

the above table is only a partial example, and the composition data and the microstructure data of the alloy in a partial sub-area are included, and the microstructure data includes, for example, the composition, the performance data, and the like of the alloy. It is also desirable to have a microscopic view of the alloy. The micro-hardness, isothermal section phase diagram and micro-structure evolution law of the alloy can be obtained through the composition data and the micro-structure data, and a material database of the alloy can be established through the composition data, the micro-structure data and the micro-hardness of the alloy. Of course, the way of the method is more, and the description is not repeated here.

In step S36, the high-throughput alloy in each sub-region is characterized by the analysis results. Through the steps, high-flux characterization of the high-flux alloy can be realized, a large number of results are obtained through one-time characterization, and a data basis is provided for works such as phase diagram drawing, alloy development and design and the like.

Through the mode, high-flux experiments can be realized, and a large amount of data can be obtained by using one piece of test alloy.

In the above embodiments, there is one and only one variable element in each composite alloy mass, and there is one and only one element in each variable element. If the variable elements are too many, inaccurate test results are easily obtained when the gold diffusion polynary is tested, and the stability is too poor.

Through the mode, the high-flux alloy, the preparation method and the test method of the high-flux alloy set the combined alloy blocks through one test alloy, and each combined alloy block is provided with one variable element, so that a large number of different alloy components can be obtained simultaneously, a large number of alloys can be analyzed through one-time experiment, the experiment time and resources can be shortened, and the design and optimization of the alloys are further accelerated.

In the description above, for purposes of explanation and not limitation, specific details are set forth such as particular system structures, interfaces, techniques, etc. in order to provide a thorough understanding of the present application. It will be apparent, however, to one skilled in the art that the present application may be practiced in other embodiments that depart from these specific details. In other instances, detailed descriptions of well-known devices, circuits, and methods are omitted so as not to obscure the description of the present application with unnecessary detail.