High-entropy alloy preparation process parameter regulation and control method and system

Abstract

The invention relates to the technical field of high-entropy alloy preparation, and discloses a high-entropy alloy preparation process parameter regulation and control method and system.The method comprises the steps that reactive gas which reacts with soft metal component powder to generate a hard surface layer is introduced into a powder system containing the soft metal component powder, and a reactive initial atmosphere is formed; carrying out first-stage mechanical ball milling in a reactive initial atmosphere, and monitoring the consumption of reactive gas so as to judge the generation completion state of the hard surface layer; after it is judged that the hard surface layer is generated, residual reactive gas in the reactive initial atmosphere is removed, so that an inert atmosphere environment is established; carrying out second-stage mechanical ball milling in an inert atmosphere environment so as to promote the soft metal component powder to form a solid solution; the forming process of a hard surface layer can be accurately controlled, and the formation of a later solid solution is prevented from being hindered while initial adhesion is inhibited, so that the uniformity and alloying degree of powder are improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of high-entropy alloy preparation, in particular to a high-entropy alloy preparation process parameter regulation method and system. BACKGROUND

[0002] When preparing high-entropy alloy powder by mechanical alloying method, especially when the alloy formula contains components with significantly different mechanical properties, such as soft and ductile metals (such as aluminum) and high-hardness and brittle metals, significant technical challenges are faced. High-energy mechanical ball milling is a key means to achieve atomic-scale uniform mixing of components and the formation of solid solutions. However, in this process, the soft metal component is prone to severe plastic deformation and adhesion, such as forming "ball wrapping" and "pot paste" on the ball milling medium and the pot wall, which causes the soft component to exit the effective mixing process and hinders the effective action of other hard components and the grinding medium, ultimately causing serious segregation of the powder composition, making it difficult to obtain a uniform initial mixing state. In order to overcome the adhesion problem of soft components, one attempt is to increase the ball milling energy input. Although this can to some extent peel off the adhesion layer and make it participate in mixing again, the local high temperature and the fresh metal surface with high chemical activity generated by high-energy ball milling will significantly promote the chemical reaction between the powder and even trace amounts of impurity gases (such as nitrogen, oxygen) in the protective atmosphere. These reactions result in the in-situ generation of a hard ceramic phase surface layer, such as nitrides or oxides, on the surface of the metal powder particles.

[0003] In the early or middle stage of ball milling, this in-situ generated hard surface layer can act as a kind of "hard shell" to effectively inhibit the excessive plastic deformation and adhesion of the soft component, thereby improving the mixing uniformity of the powder. However, if this surface reaction continues, when the hard layer completely and densely covers the metal particles, it will form a physical barrier that isolates direct contact between different metal particles, thereby blocking the solid-phase atomic diffusion path that is crucial in the subsequent alloying process. At this time, even if the ball milling time is further extended or the energy input is increased, it is still not effective to promote the formation of a uniform solid solution structure of each component. Therefore, the prior art is trapped in a dilemma when using high-energy mechanical ball milling to prepare high-entropy alloy powder containing soft and highly active components: high-energy input is needed to overcome the initial adhesion and segregation problem, but high-energy input will trigger and continue the harmful surface reaction, forming a diffusion barrier that hinders the later alloying. The prior art lacks a method that can accurately regulate this process, making it difficult to both solve the initial problem using surface reaction and avoid hindering the later alloying, thereby making it difficult to stably and efficiently prepare high-entropy alloy powder with a uniform solid solution structure. SUMMARY

[0004] In order to solve the problems in the prior art, the application provides a high-entropy alloy preparation process parameter regulation method and system, which can accurately control the generation process of the hard surface layer, suppress the initial adhesion, avoid hindering the formation of the later solid solution, and improve the uniformity of the powder and the alloying degree.

[0005] In a first aspect, the application provides a high-entropy alloy preparation process parameter regulation method, comprising: In the powder system containing the soft metal component powder, a reactive gas that reacts with the soft metal component powder to generate the hard surface layer is introduced to form a reactive initial atmosphere; The first stage of mechanical ball milling is performed in the reactive initial atmosphere, and the consumption of the reactive gas is monitored to determine the completion state of the generation of the hard surface layer; After determining that the generation of the hard surface layer is completed, the residual reactive gas in the reactive initial atmosphere is removed to establish an inert atmosphere environment; The second stage of mechanical ball milling is performed in the inert atmosphere environment to promote the soft metal component powder to form a solid solution.

[0006] The above scheme can accurately control the generation process of the hard surface layer, suppress the initial adhesion, avoid hindering the formation of the later solid solution, and improve the uniformity of the powder and the alloying degree.

[0007] The application also provides that the first stage of mechanical ball milling is performed in the reactive initial atmosphere, and the consumption of the reactive gas is monitored to determine the completion state of the generation of the hard surface layer, comprising: The first stage of mechanical ball milling is performed in an intermittent manner comprising a running stage and a stop stage; In the stop stage, the reading of the consumption is obtained; According to the change of the reading obtained in the continuous stop stage, the completion state of the generation of the hard surface layer is determined.

[0008] Through intermittent ball milling and reference reading change determination, the accuracy and reliability of the determination of the completion state of the generation of the hard surface layer are improved.

[0009] The application also provides that the second stage of mechanical ball milling is performed in the inert atmosphere environment to promote the soft metal component powder to form a solid solution, comprising: In the inert atmosphere environment, the initial sub-stage of mechanical ball milling is performed, and a first mechanical energy input is applied in the initial sub-stage to make the atoms between the soft metal component powders diffuse; After the initial sub-stage, a subsequent sub-stage of mechanical milling is performed, a second mechanical energy input is applied in the subsequent sub-stage, the second mechanical energy input is lower than the first mechanical energy input, to form a homogeneous solid solution of the soft metal component powders while maintaining the integrity of the hard surface layer structure.

[0010] By applying different energy inputs in the stages of mechanical milling, the formation of a homogeneous solid solution is promoted after initiating atomic diffusion while maintaining the integrity of the hard surface layer structure, balancing the diffusion requirement and the structure protection.

[0011] The application also proposes that, in the inert atmosphere environment, the initial sub-stage of mechanical milling is performed, the first mechanical energy input is applied in the initial sub-stage to initiate atomic diffusion between the soft metal component powders, including: A series of mechanical energy inputs are applied in an incremental manner in the initial sub-stage, and a physical signal associated with the rupture state of the hard surface layer is monitored; Based on the change of the physical signal, a rupture energy threshold of the hard surface layer is determined, and the first mechanical energy input is set and applied according to the rupture energy threshold to initiate atomic diffusion between the soft metal component powders.

[0012] By monitoring the physical signal to determine the rupture energy threshold, the mechanical energy input required to initiate atomic diffusion can be more accurately set, and excessive energy input to cause excessive rupture of the hard layer can be avoided.

[0013] The application also proposes that, in the initial sub-stage, a series of mechanical energy inputs are applied in an incremental manner, and a physical signal associated with the rupture state of the hard surface layer is monitored, including: The physical signal in a reference period is obtained under one of the series of mechanical energy inputs; According to the physical signal in the reference period, a background noise reference under the mechanical energy input is determined; After the reference period, the physical signal under the mechanical energy input is continuously obtained and compared with the background noise reference, and a signal feature representing the rupture of the hard surface layer in the physical signal is identified.

[0014] By obtaining the background noise in the reference period and comparing it, the signal representing the rupture of the hard surface layer in the physical signal can be more accurately identified, and the sensitivity of the monitoring is improved.

[0015] The application also proposes that, according to the physical signal in the reference period, the background noise reference under the mechanical energy input is determined, including: In the reference period, a plurality of signal features of the physical signal measured at different time points are obtained; According to the change rule of the signal features in the reference period, the change rule of the physical signal in the reference period is determined, and the background noise reference under the mechanical energy input is determined.

[0016] By analyzing the change rule of the signal features in the reference period, the reference of the background noise can be more accurately determined, and the accuracy of signal recognition is improved.

[0017] The application also proposes that determining the change rule of the physical signal in the reference period according to multiple signal features comprises: performing regression analysis on the multiple signal features; obtaining a functional relationship of the physical signal changing with time according to the result of the regression analysis; determining the change rule of the physical signal in the reference period according to the functional relationship.

[0018] The functional relationship obtained by regression analysis can more accurately describe the change rule of the physical signal with time, and provide a more reliable basis for determining the reference.

[0019] The application also proposes that identifying the signal feature representing the rupture of the hard surface layer in the physical signal comprises: obtaining a feature representing the rupture degree or type of the hard surface layer in the physical signal; establishing a discrimination standard for distinguishing the harmfulness of the rupture of the hard surface layer; identifying the signal feature representing the rupture of the hard surface layer in the physical signal according to the discrimination standard.

[0020] By obtaining the rupture degree or type feature and establishing the discrimination standard, the rupture signals of different harmfulness can be distinguished, and more refined rupture monitoring and control can be achieved.

[0021] The application also proposes that obtaining the feature representing the rupture degree or type of the hard surface layer in the physical signal comprises: performing time-frequency domain analysis on the physical signal; obtaining the feature representing the rupture degree or type of the hard surface layer in the physical signal according to the result of the time-frequency domain analysis, the feature being the energy distribution feature of the signal at different time points and frequency ranges.

[0022] By time-frequency domain analysis, the energy distribution feature of the signal can be obtained, which can more comprehensively represent the rupture state of the hard surface layer and provide more abundant information for discrimination.

[0023] In a second aspect, the application provides a high-entropy alloy preparation process parameter regulation system for executing the high-entropy alloy preparation process parameter regulation method, the system comprising: An atmosphere building module is configured to introduce a reactive gas into a powder system containing soft metal component powder, the reactive gas reacting with the soft metal component powder to form a hard surface layer, thereby forming a reactive initial atmosphere; A first stage ball milling module is configured to perform a first stage of mechanical ball milling in the reactive initial atmosphere; A judging module is configured to monitor consumption of the reactive gas to determine a completion state of formation of the hard surface layer; An atmosphere switching module is configured to remove residual reactive gas in the reactive initial atmosphere after determining that formation of the hard surface layer is completed, thereby establishing an inert atmosphere environment; A second stage ball milling module is configured to perform a second stage of mechanical ball milling in the inert atmosphere environment to promote formation of a solid solution of the soft metal component powder.

[0024] In summary, the high-entropy alloy preparation process parameter control method and system provided by the present application can precisely control the formation process of the hard surface layer by introducing a reactive gas in the first stage of ball milling to generate a hard surface layer in situ to inhibit adhesion, and by switching to an inert atmosphere for the second stage of ball milling after online monitoring and determining the completion state to promote the formation of a solid solution. The method and system can precisely control the formation process of the hard surface layer, inhibit initial adhesion, and avoid hindering the formation of a solid solution in the later stage, thereby improving the uniformity and alloying degree of the powder. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 A flowchart of a high-entropy alloy preparation process parameter control method provided by an embodiment of the present application.

[0026] Figure 2 A structural diagram of a high-entropy alloy preparation process parameter control system provided by an embodiment of the present application.

[0027] Label explanation: 210, atmosphere building module; 220, first stage ball milling module; 230, judging module; 240, atmosphere switching module; 250, second stage ball milling module. DETAILED DESCRIPTION

[0028] The technical solutions in the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. The components of the present application described and shown in the drawings herein can be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present application provided in the drawings is not intended to limit the scope of the claimed present application, but only represents selected embodiments of the present application. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without creative work belong to the scope of protection of the present application.

[0029] It should be noted that similar reference numbers and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further defined and explained in subsequent drawings. Meanwhile, in the description of the present application, the terms "first", "second", etc. are only used to distinguish the description, and cannot be understood as indicating or implying relative importance.

[0030] The conventional existing high-energy mechanical ball milling method has the problem that when preparing high-entropy alloy powder containing soft and ductile metal components (such as aluminum), the soft component particles are prone to large-area plastic extension and adhere to the grinding medium and the wall of the tank, resulting in uneven distribution of components and composition segregation. At the same time, in order to overcome adhesion and increase mechanical energy input, the unintended reaction of the powder with trace impurity gases (such as nitrogen and oxygen) in the protective atmosphere will be activated, generating a layer of hard ceramic phase on the surface of the powder particles in situ. This layer will hinder atomic diffusion between different metal particles in the later stage of ball milling, making it difficult to form a uniform solid solution structure.

[0031] For example, a process for preparing AlCoCrFeNi high-entropy alloy powder by mechanical alloying is being developed. After accurately proportioned metal powders and grinding steel balls are placed in a ball milling tank and vacuumized and filled with high-purity argon, high-energy ball milling is performed. Due to the soft texture of the aluminum component, under intense impact, the aluminum powder particles rapidly undergo plastic deformation and adhere to the steel balls and the tank wall, forming "ball wrapping" and "tank pasting" phenomena. This causes a large amount of aluminum elements to be separated from the effective mixing area, and the hard chromium and other components are also difficult to effectively interact with the grinding medium covered by aluminum, resulting in serious uneven distribution of components in the powder system. Even if the ball milling speed is increased to peel off the adhesion layer, the local high temperature and high activity surface generated by high energy input will still promote the reaction of trace nitrogen with aluminum, chromium and other components, forming a hard nitride layer on the surface of the powder. Once the hard layer completely covers the particles, it physically isolates direct contact between the particles, blocking the subsequent solid-phase atomic diffusion path.

[0032] If the above problems are not solved, the mechanical ball milling process will not effectively achieve the uniform mixing of each component and the formation of atomic-scale solid solution. The final obtained powder will be a composition segregated mixture, containing unreacted component particles, materials adhering to the equipment, and particles wrapped by hard ceramic layers that cannot be further alloyed, such powder cannot be used as a qualified precursor for preparing high-performance bulk high-entropy alloys, which will directly affect the uniformity of the microstructure and mechanical properties of the final bulk material, resulting in unstable product performance or failure to meet design requirements.

[0033] To this end, in a first aspect, see Figure 1 The present application proposes a high-entropy alloy preparation process parameter control method, comprising: In the powder system containing soft high-activity metal components, a reactive gas which reacts with the soft high-activity metal components to form a hard surface layer is quantitatively introduced to constitute a reactive initial atmosphere; In the reactive initial atmosphere, the first stage of mechanical ball milling is carried out to drive the reaction of the reactive gas with the soft high-activity metal component particles, so as to generate a hard surface layer in situ on the surface of the soft high-activity metal component particles; An online monitoring of a physical quantity associated with the consumption of the reactive gas is carried out, and the completion state of the generation of the hard surface layer is judged according to the change of the physical quantity; After judging that the generation of the hard surface layer is completed, the residual reactive gas in the reactive initial atmosphere is removed to establish an inert atmosphere environment; In the inert atmosphere environment, the second stage of mechanical ball milling is carried out to promote the formation of solid solution of each component powder in the powder system.

[0034] The soft high-activity metal component refers to a metal element that is prone to plastic deformation, adheres to the ball milling medium and the tank wall during mechanical ball milling, and has high chemical activity, and can be aluminum, magnesium, zinc or the like; a specific type and amount of gas is added to the powder system, and the reactive gas can chemically react with the soft high-activity metal component to form a compound layer with high hardness on the surface, for example, introducing nitrogen or oxygen to react with aluminum to form aluminum nitride or aluminum oxide, and building a functional hard shell on the surface of the soft component to inhibit its adhesion behavior during ball milling; the first stage of mechanical ball milling refers to the mechanical ball milling process under the initial reactive atmosphere, and the mechanical energy applied is sufficient to drive the reaction of the reactive gas with the soft high-activity metal component particles to promote the in-situ generation of the hard surface layer on the surface of the soft component particles; the hard surface layer refers to a compound layer with high hardness formed in-situ on the surface of the soft high-activity metal component particles by chemical reaction, such as a nitride layer or an oxide layer, which is used to change the surface properties of the soft component particles and reduce their adhesion tendency; during the first stage of mechanical ball milling, a physical parameter reflecting the degree of consumption of the reactive gas is measured in real time, such as the gas pressure in the ball milling tank, the concentration of the gas component, etc., to monitor the progress of the reaction of the reactive gas with the soft component in real time; determining the completion state of the hard surface layer formation refers to determining that the hard surface layer on the surface of the soft high-activity metal component particles has been formed to the expected extent according to the change trend of the online monitored physical quantity or reaching a specific threshold, accurately controlling the termination time of the first stage of ball milling, and avoiding excessive growth of the hard layer; removing the residual reactive gas in the initial reactive atmosphere refers to removing the residual reactive gas in the ball milling tank by vacuumizing, purging or replacing after determining that the hard surface layer has been formed, which is to completely terminate the continuous growth of the hard surface layer and create a non-reactive environment for the subsequent solid solution formation stage; the second stage of mechanical ball milling is carried out after the reactive gas is removed and an inert atmosphere is established, and the mechanical energy applied is intended to promote the mutual diffusion of atoms of each component in the powder system to form a uniform solid solution structure.

[0035] The core innovation of the present application is that by quantitatively introducing a reactive gas into a powder system containing a soft high-activity metal component and performing a first-stage mechanical ball milling, a hard surface layer is generated in situ on the surface of the soft component, and the completion state of the generation of the hard surface layer is determined by monitoring the consumption of the reactive gas in real time, and the residual reactive gas is removed in time, so that the originally harmful surface reaction is converted into a controllable process means, the adhesion problem of the soft component is solved, and the excessive growth of the hard layer is avoided to hinder the subsequent formation of solid solution, and finally the preparation of a uniform solid solution powder is realized. The problem of easy adhesion of the soft component and the composition segregation problem caused thereby in the process of mechanical ball milling of high-entropy alloy powder containing a soft high-activity metal component are effectively solved. At the same time, by accurately controlling the introduction and removal time of the reactive gas, the excessive growth of the hard surface layer into an obstacle to hinder the atomic diffusion and solid solution formation in the later stage is avoided, ensuring that the high-energy ball milling process can proceed smoothly and finally obtain a solid solution high-entropy alloy powder with uniform composition and ideal structure, and improving the stability and success rate of the preparation process.

[0036] The present application further proposes a step of monitoring the consumption of the reactive gas in real time and determining the completion state of the generation of the hard surface layer according to the change of the consumption, comprising: The first-stage mechanical ball milling is performed in an intermittent manner comprising a running stage and a stop stage; In the stop stage, a baseline reading of the consumption is obtained; According to the change of the baseline reading obtained in the continuous stop stage, the completion state of the generation of the hard surface layer is determined.

[0037] The first-stage mechanical ball milling performed in an intermittent manner comprising a running stage and a stop stage means that the continuous ball milling process is divided into alternating running time periods and stopping time periods, and the power supply or driving mechanism of the ball mill can be controlled to start and stop. The baseline reading of the consumption is a measurement value obtained during the stop of the ball mill for representing the consumption state of the reactive gas, which can be measured by a pressure sensor, a gas concentration sensor or other devices during the stop stage to obtain physical quantity data less affected by ball mill noise. According to the change of the baseline reading obtained in the continuous stop stage, the completion state of the generation of the hard surface layer is determined by comparing the baseline readings obtained in different stop stages and analyzing the change trend thereof with time or ball milling progress, so as to determine the change of the consumption rate of the reactive gas. The continuous baseline readings can be recorded and analyzed by a data acquisition system, for example, whether the monitoring readings tend to be stable or the change rate is reduced, and the reaction is judged to reach the preset completion standard based on more accurate data.

[0038] The first stage of mechanical milling is set as an intermittent mode including a running stage and a stop stage. In the running stage of the ball mill, the reactive gas reacts with the soft high-activity metal component particles to form a hard surface layer on the surface of the soft high-activity metal component particles. In the stop stage of the ball mill, the noise and vibration generated by mechanical operation are greatly reduced, and the reading of the consumption of the reactive gas is obtained at this time, which can more accurately reflect the true state of the reaction. By repeatedly obtaining the reference reading in the continuous stop stage and analyzing the trend of the continuous reference readings, the consumption rate of the reactive gas can be monitored. When the consumption rate of the reactive gas significantly decreases or tends to be stable, it indicates that the hard surface layer on the surface of the soft high-activity metal component particles has been basically formed. This method based on the accurate measurement in the stop stage and continuous data analysis effectively overcomes the interference of noise on the monitoring of physical quantities in the continuous milling process, and ensures the accuracy of the judgment of the completion state of the hard surface layer formation. Accurate judgment of the completion state of the hard surface layer formation enables the reactive atmosphere to be removed in time and switched to an inert atmosphere for subsequent second stage milling, avoiding the hard surface layer from growing excessively to become a diffusion barrier, thereby ensuring the quality of the solid solution of the final high-entropy alloy powder.

[0039] In some preferred embodiments, the first stage of mechanical milling can be set to run for 30 minutes and then stop for 5 minutes, and the cycle is repeated. In each 5-minute stop stage, a high-precision pressure sensor is used to measure the gas pressure in the ball mill tank, and the pressure value is the reference reading. The data acquisition system records the pressure value at the end of each stop stage. By comparing the pressure reference readings obtained in multiple consecutive stop stages, such as observing whether the pressure drop rate is lower than a certain threshold value, or whether the pressure drop values of three consecutive stop stages differ by less than a certain set value, it can be determined whether the consumption of the reactive gas (such as nitrogen) has significantly slowed down, thereby determining whether the formation of the hard surface layer (such as aluminum nitride) has been basically completed.

[0040] Through the above technical solution, the intermittent ball milling is used to monitor the physical quantity in the stop stage, which effectively avoids the noise interference generated by the operation of the ball mill, and improves the accuracy of the physical quantity reading. Based on the trend of the accurate reference readings obtained in the continuous stop stage, the completion state of the hard surface layer formation can be reliably determined. The negative effects caused by the excessive growth of the hard layer are avoided, thereby helping to obtain a high-entropy alloy powder with uniform composition and good performance.

[0041] The application further proposes a step of performing a second stage of mechanical milling in an inert atmosphere environment to promote the formation of a solid solution of each component powder in the powder system, which includes: In the inert atmosphere environment, an initial sub-stage of mechanical milling is performed, and a first mechanical energy input is applied in the initial sub-stage to start atomic diffusion between the components in the powder system; After the initial sub-stage, a subsequent sub-stage of mechanical milling is performed, which applies a second mechanical energy input that is lower than the first mechanical energy input to promote the formation of a homogeneous solid solution of the component powders that have initiated atomic diffusion while maintaining the integrity of the hard surface layer structure.

[0042] wherein the initial sub-stage of mechanical milling refers to the time period or process at the beginning of the second stage of mechanical milling for initiating atomic diffusion between the components in the powder system, which lays the foundation for the subsequent homogenization process; the first mechanical energy input refers to the level of mechanical energy applied in the initial sub-stage, which is relatively high to provide the energy required to overcome the atomic diffusion barrier, activate the components, and promote them to start diffusing with each other; the subsequent sub-stage of mechanical milling refers to the time period or process after the initial sub-stage for maintaining atomic diffusion and achieving homogenization, which ensures the continuation of atomic diffusion while avoiding excessive rupture of the hard surface layer; and the second mechanical energy input refers to the level of mechanical energy applied in the subsequent sub-stage, which is lower than the first mechanical energy input to promote the formation of a homogeneous solid solution of the component powders that have initiated atomic diffusion while maintaining the integrity of the hard surface layer structure.

[0043] The present application controls the alloying process by controlling the mechanical energy input in stages. In an inert atmosphere environment, the initial sub-stage of mechanical milling is first performed, which applies a relatively high first mechanical energy input. This relatively high energy input can activate the components in the powder system, provide the energy required to overcome the atomic diffusion barrier, and thus initiate the atomic diffusion process between the components. After the initial sub-stage, the subsequent sub-stage of mechanical milling is performed, which applies a second mechanical energy input that is lower than the first mechanical energy input. This relatively low energy input can continuously drive the initiated atomic diffusion process while maintaining the integrity of the hard surface layer structure formed in the first stage of milling. The hard surface layer can inhibit the adhesion of soft components, but too high an energy can cause it to rupture, leading to new problems. By reducing the energy input, the continuation of diffusion can be ensured while avoiding premature or excessive rupture of the hard surface layer, thereby ensuring that the component powders can form a homogeneous solid solution. This strategy of staged and differentiated energy input, combined with the first stage of in-situ generation of a hard surface layer by a reactive gas and online monitoring of the completion status, forms a process chain. The first stage solves the problem of soft component adhesion and atmosphere switching, creating suitable conditions for the second stage of solid solution formation (inert atmosphere and powders with a hard surface layer). The second stage then controls the mechanical energy input to overcome the contradiction between initiating diffusion and protecting the hard surface layer, ultimately obtaining a homogeneous solid solution powder.

[0044] By the technical solution, the atomic diffusion among the components in the powder system can be started, and meanwhile, the components whose atomic diffusion has been started can form a uniform solid solution under the premise of maintaining the integrity of the hard surface layer. Thus, the problems of difficulty in starting the diffusion by simple inert atmosphere ball milling and possible damage of the hard surface layer by high-energy ball milling are solved, and the uniformity of the finally formed solid solution is achieved.

[0045] The application further proposes that in the inert atmosphere environment, the step of performing an initial sub-stage of mechanical ball milling, which applies a first mechanical energy input to start the atomic diffusion among the components in the powder system, includes: a series of mechanical energy inputs are applied to the powder system in an incremental manner in the initial sub-stage; a physical signal associated with the cracking state of the hard surface layer is monitored during the application of the series of mechanical energy inputs; a cracking energy threshold value representing the cracking of the hard surface layer is determined based on the change of the physical signal; the first mechanical energy input is set according to the cracking energy threshold value, and the first mechanical energy input is applied to start the atomic diffusion among the components in the powder system.

[0046] Among them, the series of mechanical energy inputs applied to the powder system in an incremental manner means that the mechanical energy applied to the powder system is gradually increased, which can be achieved by gradually increasing the rotation speed of the ball mill, gradually prolonging the ball milling time, or gradually increasing the filling amount of the grinding medium, etc. The response of the powder system under different energy inputs, especially the state change of the hard surface layer, is observed. The physical signal associated with the cracking state of the hard surface layer is monitored, which means that the physical quantity reflecting whether the hard surface layer cracks or the degree of cracking is obtained. Acoustic sensors, vibration sensors, strain sensors, etc. can be used to obtain the signal, and the structural integrity of the hard surface layer can be understood in real time. The cracking energy threshold value representing the cracking of the hard surface layer is determined, which means that according to the change of the monitored physical signal, the mechanical energy input level corresponding to the start of significant cracking of the hard surface layer is identified. The change of the amplitude, frequency, energy, etc. of the signal can be analyzed to determine an energy critical point, which is used to guide the subsequent energy setting. The first mechanical energy input is set, which means that the mechanical energy input value for starting the atomic diffusion is determined. The cracking energy threshold value can be set according to the determined cracking energy threshold value, for example, a value slightly lower than the threshold value is set. The atomic diffusion is started while the integrity of the hard surface layer is maintained as much as possible.

[0047] By the technical solution, the initial sub-stage mechanical energy input is accurately controlled. The energy threshold is determined by monitoring the rupture state of the hard surface layer, and the energy input is set according to the threshold, which avoids the problem that the hard surface layer is ruptured too early due to too high energy, and avoids the problem that the atomic diffusion cannot be effectively started due to too low energy. This makes it possible to effectively protect the structural integrity of the hard surface layer while starting the atomic diffusion, better plays the role of the hard surface layer in inhibiting the adhesion of the soft component in the early stage, lays a foundation for the uniform formation of the subsequent solid solution, and improves the preparation quality of the high-entropy alloy powder.

[0048] The application further proposes that in the process of applying a series of mechanical energy inputs, the step of monitoring a physical signal associated with the rupture state of the hard surface layer includes: Under one of the series of mechanical energy inputs, the physical signal in a reference period is acquired; According to the physical signal in the reference period, a reference benchmark representing the background noise under the mechanical energy input is determined; After the reference period, the physical signal under the mechanical energy input is continuously acquired, and the continuously acquired physical signal is compared with the reference benchmark; Based on the comparison, the signal representing the rupture of the hard surface layer in the physical signal is identified.

[0049] The physical signal associated with the hard surface layer cracking state refers to a physical quantity that can reflect the change in the integrity of the hard layer structure on the surface of the powder particles during the mechanical energy input process. Acoustic emission signals, vibration signals, or impact force signals measured by force sensors can be used. The reference period refers to a time window selected before the hard surface layer has been significantly cracked for collecting physical signals to evaluate background noise after applying a mechanical energy input. The reference benchmark representing the background noise under the mechanical energy input refers to a reference value or model established based on the physical signals collected during the reference period, which is used to quantify the inherent noise characteristics under a specific mechanical energy input level. The average, median, standard deviation of the signals during the reference period, or a noise distribution model established based on statistical analysis can be used. Comparing the continuously acquired physical signals with the reference benchmark refers to comparing the physical signals collected in real time after the reference period with the pre-determined reference benchmark to determine whether the real-time signals significantly deviate from the normal background noise level. Threshold setting comparison, statistical difference test, or anomaly detection based on machine learning models can be used. Identifying the signals in the physical signals that represent the cracking of the hard surface layer refers to distinguishing and extracting those signal components with specific mode, amplitude or frequency characteristics from the continuously acquired and compared physical signals. These components indicate the cracking or damage events of the hard surface layer. Signal peak detection, specific frequency component analysis, or feature extraction based on signal processing techniques and pattern matching can be used.

[0050] The present application, by acquiring the physical signal in a reference period for each specific mechanical energy input during the application of a series of mechanical energy inputs, first captures the background noise characteristics at the specific energy input level. Since different energy inputs can produce different levels of background noise, it is necessary to establish an independent noise evaluation at each energy input. Based on the physical signal in the reference period, a reference benchmark representing the background noise at the mechanical energy input is determined, which quantifies the typical noise level at the energy input. Subsequently, after the reference period, the physical signal under the mechanical energy input is continuously acquired, and the real-time acquired signal is compared with the previously determined reference benchmark. This comparison mechanism enables the scheme to effectively distinguish between the true signal caused by the hard surface layer cracking and the inherent background noise at the energy input. Comparing the real-time signal with the specific noise benchmark at the energy input can more accurately identify those signals in the physical signal that truly represent the cracking of the hard surface layer, thereby avoiding misjudgment caused by signal fluctuations due to background noise or other non-cracking factors. In this way, the accuracy of identifying hard surface layer cracking events during the incremental energy input process is improved, thereby providing a reliable basis for subsequent accurate determination of the cracking energy threshold. This accurate cracking energy threshold determination enables the subsequent first mechanical energy input to exactly reach the energy required to start atomic diffusion, while avoiding the negative effects of excessive energy input, thereby effectively supporting the goal of starting atomic diffusion between components in the powder system in the initial sub-stage of the second stage mechanical milling.

[0051] During the application of a series of mechanical energy inputs, for each energy input level, by acquiring the physical signal in a reference period and establishing a background noise reference benchmark, and then comparing the continuously acquired physical signal with the benchmark, the background noise interference at the energy input level can be effectively filtered out, improving the ability to accurately identify signals representing the cracking of the hard surface layer from the physical signal. This accurate signal identification avoids misjudgment due to noise, ensuring the accuracy of subsequent cracking energy threshold determination, so that the first mechanical energy input set can more accurately match the energy required to start atomic diffusion, providing a guarantee for the precise regulation of high-entropy alloy preparation process.

[0052] The present application further proposes a step of determining a reference benchmark representing the background noise at the mechanical energy input based on the physical signal in the reference period, comprising: In the reference period, a plurality of signal characteristics of the physical signal measured at different time points are acquired; According to the plurality of signal characteristics, the variation law of the physical signal in the reference period is determined; The reference benchmark representing the state of the background noise at the end of the reference period is determined according to the change rule and a signal feature that is acquired last in time among the plurality of signal features.

[0053] The plurality of signal features of the physical signal refer to a plurality of quantifiable attributes or parameters exhibited by the physical signal at different time points, such as the amplitude, energy, frequency distribution, root mean square value, peak value, etc., which can be obtained by sampling and calculating the physical signal within a preset time interval by a signal acquisition device, and comprehensively describe the state of the physical signal within the reference period. The change rule of the physical signal within the reference period refers to the trend or pattern exhibited by the plurality of signal features of the physical signal over time, such as linear growth, periodic fluctuation or random distribution, etc., which can be determined by statistical analysis, curve fitting or pattern recognition, etc. on the acquired plurality of signal features, and reveals the dynamic evolution characteristics of the background noise within the reference period. The reference benchmark representing the state of the background noise at the end of the reference period refers to a value or model representing the level or characteristics of the background noise at the end of the reference period, which can be a threshold, a functional relationship or a statistical distribution parameter, and provides an accurate comparison basis for subsequent rupture signal identification.

[0054] The present application can more comprehensively understand the dynamic characteristics of the background noise by acquiring the plurality of signal features of the physical signal within the reference period and determining the change rule of the physical signal within the period based on these features. Further, in combination with the change rule and the last acquired signal feature within the reference period, the state of the background noise at the end of the reference period can be more accurately predicted or estimated, and the reference benchmark is determined accordingly. The limitations of relying only on instantaneous value or simple average value as the benchmark are avoided, and the fluctuations or trend changes of the background noise can be effectively dealt with, so that when the continuously acquired physical signal is compared with the reference benchmark, the signal truly representing the rupture of the hard surface layer can be more accurately distinguished, the interference of the background noise is reduced, and the sensitivity and accuracy of the rupture signal identification are improved.

[0055] The present application further proposes that the step of determining the change rule of the physical signal within the reference period according to the plurality of signal features comprises: performing regression analysis on the plurality of signal features; obtaining a functional relationship of the physical signal changing over time according to the result of the regression analysis; determining the change rule of the physical signal within the reference period according to the functional relationship.

[0056] The plurality of signal features refer to quantitative descriptions of the physical signal collected at different time points in the reference period, which can be the instantaneous amplitude, root mean square value, peak value, energy, frequency component, etc. of the signal, providing a data basis for subsequent analysis. Regression analysis is used to determine the strength and direction of the relationship between two or more variables, which can be linear regression, polynomial regression, nonlinear regression, etc. The mathematical model between variables is established by fitting data points to mine the internal relationship between signal features and time. The functional relationship of the physical signal changing with time refers to the mathematical expression obtained by regression analysis, which can describe how the physical signal value changes with time, which can be a linear function, a polynomial function, an exponential function, etc. The change rule of the physical signal in the reference period refers to the overall trend, fluctuation mode or periodic characteristics of the physical signal in a specific time period revealed based on the obtained functional relationship, which accurately describes the dynamic characteristics of background noise.

[0057] The present application can establish a mathematical model between signal features and time by regression analysis of the plurality of signal features obtained in the reference period, thereby obtaining the functional relationship of the physical signal changing with time. This change rule determined based on regression analysis can more accurately reflect the dynamic characteristics of background noise, overcoming the limitations of simple methods that cannot accurately capture complex signal changes. By combining this more accurate change rule with the signal feature at the end of the reference period, a reference benchmark representing the state of background noise can be more accurately determined, so that in subsequent continuous monitoring, the signal generated by the rupture of the hard surface layer can be more reliably distinguished from background noise. Through the above technical solution, by regression analysis of the plurality of signal features, an accurate function model of the physical signal changing with time can be established, thereby more accurately determining the change rule of the physical signal in the reference period. This rule determination method based on functional relationship can better reflect the real dynamics of background noise, effectively filter out the influence of random fluctuations, and make the determined reference benchmark more accurate. The accuracy of the reference benchmark is improved, which helps to more reliably distinguish the signal generated by the rupture of the hard surface layer from the background noise, thereby improving the accuracy of hard surface layer rupture signal recognition.

[0058] The present application further proposes a step of identifying the signal representing the rupture of the hard surface layer in the physical signal, comprising: Obtaining a feature representing the degree or type of rupture of the hard surface layer in the physical signal; Establishing a discrimination standard for distinguishing the harmfulness of the rupture of the hard surface layer; According to the discrimination standard, identifying the signal representing the rupture of the hard surface layer from the physical signal.

[0059] The features representing the extent or type of hard layer cracking in the physical signals refer to information extracted from the monitored physical signals that can reflect the specific attributes of the hard layer cracking events. Techniques such as signal processing and feature extraction algorithms can be used to quantitatively or categorically describe the cracking events. The discrimination criteria for distinguishing the harmfulness of hard layer cracking refer to a set of rules or a model that can be used to evaluate the potential impact of different cracking features on the subsequent alloying process. The rules or model can be established based on experimental data analysis, physical model simulation, or machine learning methods, and can associate the attributes of the cracking events with the beneficial or harmful effects on the process.

[0060] The present application extracts features representing the extent or type of hard layer cracking from the physical signals, such as signal intensity, frequency, duration, etc. These features provide more comprehensive information than simply signal amplitude. Based on these features, a discrimination criteria for distinguishing the harmfulness of hard layer cracking is established, which associates different feature combinations with different effects on the subsequent alloying process, such as promoting diffusion or hindering diffusion. This identification method is more detailed and accurate than simply judging based on signal amplitude threshold, and can distinguish between small cracks that are beneficial to alloying and excessive cracks that may hinder alloying. In this way, the cracking state of the hard layer can be more accurately mastered, providing a more reliable basis for subsequent process control.

[0061] In some preferred embodiments, the monitored physical signals are acoustic emission signals. Extracting features representing the extent or type of hard layer cracking from the physical signals can be time-frequency domain analysis of the acoustic emission signals, such as through short-time Fourier transform or wavelet analysis, to obtain the energy distribution characteristics of the signals at different time points and frequency ranges. Establishing a discrimination criteria for distinguishing the harmfulness of hard layer cracking can be through pre-conducted experiments to collect acoustic emission signal features under different ball milling conditions and their corresponding powder states, such as hard layer thickness, integrity, and agglomeration degree, and then establishing a classification model based on rules or machine learning, which can output a score or category representing the cracking harmfulness, such as slight cracking, moderate cracking, and severe cracking, according to the energy distribution characteristics of the acoustic emission signals. Identifying signals representing hard layer cracking from the physical signals according to the discrimination criteria can be inputting the features of the real-time monitored acoustic emission signals into the above discrimination model, and if the output result of the model indicates that the cracking harmfulness reaches a pre-set threshold, such as a score higher than a certain value or being classified as severe cracking, it is considered that the signals representing harmful hard layer cracking have been identified.

[0062] By the technical solution, the signal representing the rupture of the hard surface layer in the physical signal can be analyzed and recognized more finely. By obtaining the feature of the rupture degree or type and establishing the hazard discrimination standard, different rupture events of different properties can be distinguished, and the rupture signal that may have an adverse effect on the subsequent alloying process can be identified. The process control can be more targeted, and the powder agglomeration or diffusion blockage caused by excessive or improper rupture of the hard surface layer can be avoided, which is beneficial to obtain a uniform solid solution structure and ensure the quality and performance of the final high-entropy alloy powder.

[0063] The application further proposes that the step of obtaining the feature representing the rupture degree or type of the hard surface layer in the physical signal comprises: performing time-frequency domain analysis on the physical signal; obtaining the feature representing the rupture degree or type of the hard surface layer in the physical signal according to the result of the time-frequency domain analysis, the feature being the energy distribution feature of the signal at different time points and frequency ranges.

[0064] The physical signal refers to the physical signal associated with the rupture state of the hard surface layer, which can be an acoustic signal, a vibration signal, or a stress signal collected by a sensor. The time-frequency domain analysis refers to a method of decomposing and analyzing a signal in two dimensions of time and frequency, which can specifically use technologies such as short-time Fourier transform STFT, wavelet transform, and Hilbert-Huang transform HHT to reveal the energy distribution and change rule of the signal at different times and frequencies. The result of the time-frequency domain analysis refers to the representation of the signal on a two-dimensional plane of time and frequency after time-frequency domain analysis, which can specifically be in the form of a time-frequency diagram, a spectrum diagram sequence, or a time-frequency coefficient matrix. The feature representing the rupture degree or type of the hard surface layer refers to a technical index that can reflect the severity or specific form of the rupture of the hard surface layer, which can specifically be the concentration degree, change trend, peak position, or distribution mode of the signal energy in a specific time period or specific frequency range obtained by analyzing the result of the time-frequency domain analysis. The energy distribution feature of the signal at different time points and frequency ranges refers to the specific distribution of the signal energy on the time-frequency plane, which can specifically be the distribution intensity of the signal energy at different frequencies within a certain time point or time period, or the change of the signal energy at different times within a certain frequency or frequency range.

[0065] The present application can capture the transient signals generated during the rupture of the hard surface layer and the dynamic changes of different frequency components by analyzing the physical signals in the time-frequency domain. This information is difficult to obtain through simple time or frequency domain analysis. Based on this more comprehensive time-frequency domain representation, the energy distribution characteristics of the signal at different time points and frequency ranges can be extracted. These energy distribution characteristics can more accurately reflect the degree and type of rupture of the hard surface layer. For example, different degrees of rupture may be represented as energy concentration regions with different intensities or durations on the time-frequency graph, while different types of rupture may correspond to different time-frequency distribution patterns. By obtaining these more discriminative features, more reliable inputs are provided for subsequent establishment of discriminant criteria for distinguishing the severity of hard surface layer rupture, thereby enabling more accurate identification of signals representing the rupture of the hard surface layer from physical signals, overcoming the inaccuracy and limitations of relying solely on simple features for discrimination, and making the judgment of the rupture state of the hard surface layer more accurate, thereby providing a solid foundation for subsequent precise control of process parameters.

[0066] Through the above technical solutions, the physical signal can be analyzed more deeply and comprehensively to obtain the energy distribution characteristics of the signal in the time and frequency dimensions. These characteristics can more accurately reflect the subtle differences in the rupture of the hard surface layer, overcoming the limitations of relying solely on simple features for judgment. This enables more effective differentiation of different degrees and types of hard surface layer rupture, improving the accuracy of rupture state judgment and providing more reliable and refined information input for subsequent precise control of process parameters based on the rupture state.

[0067] In a second aspect, referring to Figure 2 The present application further proposes a high-entropy alloy preparation process parameter control system for executing the high-entropy alloy preparation process parameter control method. The system comprises: An atmosphere building module 210 is used to quantitatively introduce a reactive gas that reacts with the soft high-activity metal component to generate a hard surface layer in a powder system containing the soft high-activity metal component, to form a reactive initial atmosphere; A first-stage ball milling module 220 is used to perform a first-stage mechanical ball milling in the reactive initial atmosphere to drive the reaction of the reactive gas with the soft high-activity metal component particles, thereby generating a hard surface layer in situ on the surface of the soft high-activity metal component particles; A judgment module 230 is used to monitor a physical quantity associated with the consumption of the reactive gas online, and to judge the completion state of the generation of the hard surface layer according to the change of the physical quantity; an atmosphere switching module 240 for removing residual reactive gas in the reactive initial atmosphere and establishing an inert atmosphere environment after determining that the hard surface layer is generated; a second stage ball milling module 250 for performing a second stage of mechanical ball milling in the inert atmosphere environment to promote the formation of solid solution among the component powders in the powder system.

[0068] The atmosphere building module 210 refers to a device for controlling the gas composition and pressure in the ball milling environment, which can employ a gas flow controller, a vacuum pump, a gas storage tank, and corresponding valves and pipeline systems. The first stage ball milling module 220 refers to a device for applying mechanical impact energy to the powder system, which can employ a planetary ball mill, a vibration ball mill, or a high-energy stirring ball mill. The determination module 230 refers to a device for monitoring and analyzing physical quantities related to the consumption of reactive gas in real time, which can employ a pressure sensor, a gas concentration sensor, a spectrum analyzer, a data acquisition unit, and a signal processing unit. The atmosphere switching module 240 refers to a device for changing the gas composition in the ball milling environment, which can employ a vacuum pump, a gas introduction system, and control valves. The second stage ball milling module 250 refers to a device for applying mechanical impact energy to the powder system to promote the formation of solid solution, which can employ a planetary ball mill, a vibration ball mill, or a high-energy stirring ball mill.

[0069] The present application controls the introduction of reactive gas according to preset parameters through the atmosphere building module 210, ensuring the establishment of a reactive initial atmosphere. Then, the first stage ball milling module 220 performs mechanical ball milling, providing the mechanical energy required to drive the surface reaction and promoting the in-situ generation of a hard surface layer on the surface of soft component particles. In this process, the determination module 230 continuously monitors physical quantities related to the consumption of reactive gas, such as changes in gas pressure or concentration, and determines whether the surface reaction has reached completion based on the trends or reaching of specific thresholds of these physical quantities. Once the determination module 230 signals that the reaction is complete, the atmosphere switching module 240 is activated to remove the residual reactive gas in the ball milling tank and introduce inert gas to establish an inert atmosphere environment, which prevents further surface reaction and avoids the excessive growth of the hard layer into a diffusion barrier. Finally, the second stage ball milling module 250 continues mechanical ball milling in the inert atmosphere. At this time, since the soft component surface has formed a hard layer, the adhesion problem is suppressed, and the inert atmosphere ensures the purity of the powder, while the mechanical energy promotes atomic diffusion and solid solution formation among the component powders. The present application overcomes the process parameter deviation and stability problems caused by the lack of an execution system in traditional methods, ensuring the controllability and repeatability of the high-entropy alloy preparation process, thereby obtaining alloy powders with expected performance and quality.

[0070] The above merely provides an example of the present application, and is not used to limit the protection scope of the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims

1. A method for controlling process parameters in the preparation of high-entropy alloys, characterized in that, include: In a powder system containing soft metal component powder, a reactive gas that reacts with the soft metal component powder to generate a hard surface layer is introduced to form a reactive initial atmosphere. The first stage of mechanical ball milling is carried out in the reactive initial atmosphere, and the consumption of the reactive gas is monitored to determine the completion status of the hard surface layer formation. After the hard surface layer is determined to be formed, the residual reactive gas in the reactive initial atmosphere is removed to establish an inert atmosphere environment; A second stage of mechanical ball milling is performed in the inert atmosphere to promote the formation of a solid solution from the soft metal component powder.

2. The method for controlling process parameters in the preparation of high-entropy alloys according to claim 1, characterized in that, The first stage of mechanical ball milling in the reactive initial atmosphere, and monitoring the consumption of the reactive gas to determine the completion status of the hard surface layer formation, includes: The first stage of mechanical ball milling is carried out intermittently, including running and stopping phases; During the stop phase, the consumption reading is obtained; The completion status of the hard surface layer formation is determined based on the changes in the readings obtained during the continuous stop phases.

3. The method for controlling process parameters in the preparation of high-entropy alloys according to claim 1, characterized in that, The second stage of mechanical ball milling in the inert atmosphere to promote the formation of a solid solution from the soft metal component powder includes: In the inert atmosphere, an initial sub-stage of mechanical ball milling is performed, during which a first mechanical energy input is applied to induce atomic diffusion between the soft metal component powders. After the initial sub-stage, a subsequent sub-stage of mechanical ball milling is performed, in which a second mechanical energy input is applied, which is lower than the first mechanical energy input, so as to form a uniform solid solution of the soft metal component powder while maintaining the integrity of the hard surface structure.

4. The method for controlling process parameters in the preparation of high-entropy alloys according to claim 3, characterized in that, The initial sub-stage of mechanical ball milling, performed in the inert atmosphere environment, wherein a first mechanical energy input is applied in the initial sub-stage to induce atomic diffusion between the soft metal component powders, comprises: During the initial sub-stage, a series of mechanical energy inputs are applied in an incremental manner, and physical signals associated with the fracture state of the hard surface are monitored. Based on the changes in the physical signal, the fracture energy threshold for the hard surface layer to fracture is determined. Based on the fracture energy threshold, the first mechanical energy input is set and applied to enable atomic diffusion between the soft metal component powders.

5. The method for controlling process parameters in the preparation of high-entropy alloys according to claim 4, characterized in that, The process of applying a series of mechanical energy inputs in an incremental manner during the initial sub-stage and monitoring physical signals associated with the fracture state of the hard surface layer includes: Under one of the series of mechanical energy inputs, the physical signal is acquired within a reference time period; Based on the physical signal within the reference time period, a background noise reference is determined for the mechanical energy input. After the reference period, under the mechanical energy input, the physical signal is continuously acquired and compared with the background noise benchmark to identify the signal features in the physical signal that characterize the cracking of the hard surface layer.

6. The method for controlling process parameters in the preparation of high-entropy alloys according to claim 5, characterized in that, The step of determining the background noise reference under the mechanical energy input based on the physical signal within the reference time period includes: Within the reference time period, multiple signal characteristics of the physical signal measured at different time points are acquired; Based on the multiple signal characteristics, the variation pattern of the physical signal within the reference time period is determined, and the background noise reference under the mechanical energy input is determined accordingly.

7. The method for controlling process parameters in the preparation of high-entropy alloys according to claim 6, characterized in that, The step of determining the variation pattern of the physical signal within the reference time period based on the multiple signal characteristics includes: Regression analysis was performed on the multiple signal features; Based on the results of the regression analysis, the functional relationship between the physical signal and time is obtained; Based on the aforementioned functional relationship, the variation pattern of the physical signal within the reference time period is determined.

8. The method for controlling process parameters in the preparation of high-entropy alloys according to claim 5, characterized in that, The signal features in the physical signal that characterize the cracking of the hard surface layer include: To obtain features from the physical signal that characterize the degree or type of fracture in the hard surface layer; Establish criteria for distinguishing the hazards of cracks in the hard surface layer; Based on the discrimination criteria, signal features characterizing the cracking of the hard surface layer are identified from the physical signals.

9. The method for controlling process parameters in the preparation of high-entropy alloys according to claim 8, characterized in that, The features acquired from the physical signal that characterize the degree or type of fracture in the hard surface layer include: Perform time-frequency domain analysis on the physical signal; Based on the results of the time-frequency domain analysis, the features characterizing the degree or type of fracture of the hard surface layer in the physical signal are obtained, and the features are the energy distribution characteristics of the signal at different time points and frequency ranges.

10. A high-entropy alloy preparation process parameter control system, used to execute the high-entropy alloy preparation process parameter control method as described in claim 1, characterized in that, The system includes: An atmosphere construction module is used to introduce a reactive gas into a powder system containing soft metal component powder to react with the soft metal component powder to generate a hard surface layer, thereby forming a reactive initial atmosphere. The first-stage ball milling module is used to perform the first stage of mechanical ball milling in the reactive initial atmosphere; The judgment module is used to monitor the consumption of the reactive gas in order to determine the completion status of the hard surface layer formation. An atmosphere switching module is used to remove the residual reactive gas in the reactive initial atmosphere after determining that the hard surface layer has been generated, so as to establish an inert atmosphere environment. The second-stage ball milling module is used to perform a second stage of mechanical ball milling in the inert atmosphere to promote the formation of a solid solution from the soft metal component powder.

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