A method for closed loop regeneration of components of multi-principal element alloy scrap

Abstract

This invention provides a closed-loop recycling method for multi-principal alloy scrap, comprising: Step S1, pre-treating and quantitatively analyzing the composition of the multi-principal alloy scrap to identify key element components; Step S2, calculating the theoretical mass gap of each element to be added based on the measured composition of the scrap, the target alloy design composition, and the preset scrap feeding ratio, and compensating for the theoretical mass gap according to the element category; Step S3, mixing the pre-treated scrap with the added material and then smelting to obtain a recycled ingot. The closed-loop recycling method for multi-principal alloy scrap provided by this invention can proactively address the diversity and fluctuations in scrap composition, achieving precise control of composition through a differentiated dynamic compensation mechanism, significantly improving the compositional consistency and performance reliability of the recycled ingot, and allowing for a high proportion of various scrap materials to be incorporated, providing a universal solution for the green and efficient closed-loop recycling of multi-principal alloys.

Description

Technical Field

[0001] This invention relates to the field of metal material recycling technology, specifically to a closed-loop recycling method for multi-principal alloy waste. Background Technology

[0002] Multi-principal element alloys, especially high-entropy alloys, represent a new generation of high-performance metallic materials, demonstrating enormous potential in aerospace, energy, and chemical industries due to their excellent comprehensive properties. However, their high raw material costs and complex manufacturing processes limit their large-scale application. Low-cost, high-value recycling of waste materials is key to achieving their sustainable development.

[0003] Currently, the recycling of multi-principal alloy scrap faces the following main technical challenges: First, accurate composition reproduction is difficult, and the performance of recycled materials is uncontrollable. The superior performance of multi-principal alloys is highly dependent on the precise proportions of each metal element. However, the sources of scrap are complex and diverse (including machining chips, scrapped parts, additive manufacturing waste powder, etc.), and their actual composition generally deviates significantly from the original design values. In particular: on the one hand, elements such as aluminum (Al), titanium (Ti), magnesium (Mg), and manganese (Mn) are prone to volatilization or oxidation during the smelting process, resulting in a systematically low content of these elements in the scrap; on the other hand, refractory metals such as tungsten (W), molybdenum (Mo), niobium (Nb), and tantalum (Ta) have high melting points and are prone to compositional segregation during solidification, leading to localized uneven composition in the scrap. Traditional methods such as "direct remelting" or "fixed-ratio remelting" lack differentiated compensation mechanisms for the behavior of these elements, often resulting in uncontrolled composition and severe performance degradation of the recycled ingots, failing to meet the reproduction requirements of high-performance applications.

[0004] Secondly, existing technical solutions are limited and lack universality and dynamic adjustment capabilities. Most current solutions for metal scrap recycling focus on process optimization for specific alloy grades (such as a particular high-temperature alloy) or on processing single-form scrap (such as powder). These methods heavily rely on the premise that the scrap composition is known and stable, employing fixed feed ratios and failing to proactively address the unknown composition and batch fluctuations of the scrap. For example, when the content of a refractory element in the scrap unexpectedly exceeds the standard, existing methods cannot provide a dynamic adjustment strategy, making the entire batch of scrap unusable.

[0005] Furthermore, hydrometallurgical methods are unsuitable for the high-value regeneration of multi-principal alloys. While hydrometallurgical processes (such as acid leaching-separation-purification) can separate elements into individual metals from multi-principal alloy waste, they are lengthy, consume large amounts of acids and alkalis, have high wastewater treatment costs, and impose a heavy environmental burden. More importantly, this approach completely destroys the original "pre-alloyed" microstructure of the multi-principal alloy, resulting in the loss of structural value such as high entropy effects and lattice distortions contained in the waste, making it undesirable from both an economic and resource efficiency perspective.

[0006] In conclusion, developing a universal recycling method that can proactively address the uncertainty of waste composition, does not rely on specific alloy grades, and can accurately reproduce the composition and properties of recycled materials is of vital importance for promoting the green manufacturing and large-scale application of multi-principal alloys. Summary of the Invention

[0007] The purpose of this invention is to overcome the above-mentioned technical deficiencies and propose a closed-loop recycling method for multi-principal alloy waste, which solves the technical problem that existing technologies cannot actively cope with the uncertainty of waste composition and lack a differentiated compensation mechanism, resulting in the difficulty in accurately reproducing the composition and performance of recycled ingots.

[0008] To achieve the above-mentioned technical objectives, the present invention adopts the following technical solution: This invention provides a closed-loop recycling method for multi-principal alloy waste, comprising: Step S1, Scrap Pretreatment and Composition Detection: The multi-principal element alloy scrap is pretreated, and the pretreated scrap is subjected to quantitative composition detection to identify the key element components. Step S2, Dynamic material replenishment calculation: Based on the measured composition of the scrap, the design composition of the target alloy, and the preset scrap feeding ratio, calculate the theoretical mass gap of each element that needs to be replenished, and compensate for the theoretical mass gap of each element according to the element category. Step S3, Controlled Remelting: The pretreated waste is mixed with the supplementary material calculated according to step S2 and then smelted to obtain recycled ingots.

[0009] In some embodiments, the key elemental composition includes a group of volatile and easily oxidized elements and a group of refractory and easily segregated elements; the group of volatile and easily oxidized elements includes at least one of Al, Ti, Mg, and Mn, and the group of refractory and easily segregated elements includes at least one of W, Mo, Nb, and Ta.

[0010] In some embodiments, the step of compensating for the theoretical mass gap of each element according to the element category includes: For any element in the group of volatile and easily oxidized elements, the actual amount of replenishment is obtained by adding a dynamic burn-off compensation amount based on the corresponding theoretical mass gap. For any element in the group of refractory and easily segregated elements, the actual amount to be added is determined based on the relative relationship between its measured content and the target value.

[0011] In some embodiments, the dynamic burn-off compensation amount is 5%-15% of the theoretical mass gap, and the specific value is determined based on the historical burn-off rate data or thermodynamic simulation calculation results of the corresponding element.

[0012] In some embodiments, determining the actual supplement amount based on the relative relationship between the measured content and the target value includes: If the measured content of the corresponding element is lower than the target value, the corresponding theoretical quality gap shall be made up. If the measured content of the corresponding element exceeds the target value, reduce the feeding ratio of the current batch of waste, or use the current batch of waste in combination with waste of the same series with low content.

[0013] In some embodiments, the pretreatment in step S1 includes: degreasing, washing, drying, crushing and / or densifying the waste to form raw material blocks suitable for smelting.

[0014] In some embodiments, the quantitative component detection in step S1 is performed using an X-ray fluorescence spectrometer or an inductively coupled plasma atomic emission spectrometer.

[0015] In some embodiments, the melting in step S3 is carried out in a vacuum induction melting furnace, and the ultimate vacuum degree during melting is less than or equal to 1×10⁻⁶. -2 Pa, and the melting temperature exceeds the alloy liquidus temperature by 100-200℃.

[0016] In some embodiments, step S3, after vacuum melting, further includes a step of electroslag remelting and refining the molten steel obtained from melting.

[0017] In some embodiments, the component closed-loop regeneration method further includes: Step S4, Regeneration Verification and Data Feedback: Sample and analyze the composition of the recycled ingot obtained in Step S3, and compare the measured data with the design composition of the target alloy; if the content of each major element falls within ±1.0 at.% of the target value, it is determined to be qualified recycled material; at the same time, the corresponding measured data is fed back to the material replenishment calculation model in Step S2 to optimize the compensation parameters in subsequent batch processing.

[0018] Compared with the prior art, the beneficial effects of the present invention are as follows: This invention provides a closed-loop recycling method for multi-principal alloy scrap. Through pretreatment and quantitative detection, multi-principal alloy scrap with unknown and fluctuating composition is transformed into a quantifiable known system. Then, based on the measured composition, the target design composition, and the preset feeding ratio, the theoretical mass gap of each element is calculated. The gap is dynamically compensated according to the different physicochemical behavior categories of the elements. Finally, the scrap and the added material are mixed and smelted to obtain recycled ingots.

[0019] This invention provides a closed-loop recycling method for multi-principal alloy scrap, abandoning the traditional passive processing mode of "fixed ratio" or "direct remelting" and instead establishing an active control mechanism of "first detection and classification, then compensation as needed". By applying compensation strategies matching the melting behavior characteristics of different categories of elements such as those prone to burnout and segregation, the compositional deviation of the scrap is corrected from the source, significantly improving the process adaptability to the diversity of scrap sources and compositional fluctuations. This allows the composition of the recycled ingot to stably approach the target design value, ensuring the consistency and reliability of the recycled material's performance. At the same time, it allows the incorporation of a high proportion of various forms of scrap, reducing the dependence on expensive primary raw materials and achieving efficient and precise closed-loop recycling of multi-principal alloy scrap. Attached Figure Description

[0020] Figure 1 This is a schematic flowchart of a closed-loop regeneration method for components in one embodiment of the present invention; Figure 2 This is a flowchart illustrating the regeneration verification and data feedback steps in one embodiment of the present invention. Detailed Implementation

[0021] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.

[0022] In related technologies, the recycling of multi-principal alloy waste faces the following technical challenges: First, it is difficult to accurately reproduce the composition, and the performance of recycled materials is uncontrollable; second, existing technical solutions are limited and lack universality and dynamic adjustment capabilities; in addition, hydrometallurgical methods are not suitable for the high-value recycling of multi-principal alloys.

[0023] To address the aforementioned technical problems, this invention provides a closed-loop recycling method for multi-principal alloy scrap, which significantly improves the process adaptability to the diversity of scrap sources and compositional fluctuations. This allows the composition of the recycled ingot to stably approach the target design value, ensuring the consistency and reliability of the recycled material's performance. Simultaneously, it allows for the incorporation of high proportions of various types of scrap, reducing dependence on expensive primary raw materials and achieving efficient and precise closed-loop recycling of multi-principal alloy scrap.

[0024] Please see Figure 1 , Figure 1 This is a schematic flowchart illustrating a closed-loop compositional regeneration method for multi-principal alloy waste according to an embodiment of the present invention. The closed-loop compositional regeneration method for multi-principal alloy waste includes... Step S1, Scrap Pretreatment and Composition Detection: The multi-principal element alloy scrap is pretreated, and the pretreated scrap is subjected to quantitative composition detection to identify the key element components.

[0025] Specifically, in step S1, the collected multi-principal alloy scrap is pretreated. Multi-principal alloy scrap comes from a wide range of sources, including but not limited to machining chips, forging heads, scrapped parts, and additive manufacturing waste powder. Because these scraps may have impurities such as oil, cutting fluid, and oxide scale adhering to their surfaces, and vary in shape and size, direct smelting would lead to compositional contamination and low smelting efficiency.

[0026] In some embodiments, pretreatment includes degreasing, washing, drying, crushing, and / or densifying the waste. For example, the waste is first degreased using an organic solvent or alkaline cleaning agent to remove surface oil; then it is washed multiple times with deionized water and placed in a drying oven to dry thoroughly at a predetermined temperature. For large scrap parts or irregularly shaped waste, mechanical crushing can be used to break them into smaller pieces. For thin or powdery waste, densification methods such as cold pressing or hot pressing can be used to press them into raw material blocks with a certain density and strength. After the above pretreatment, the waste is transformed into a raw material that is clean in composition, uniform in size, and suitable for subsequent smelting.

[0027] In some embodiments, after pretreatment, the pretreated waste can be quantitatively analyzed to identify key elemental components. Unlike traditional "fixed ratio" or "known composition" scenarios, this embodiment can proactively perform quantitative analysis on the actual composition of each batch of waste.

[0028] For example, quantitative component detection can be performed using X-ray fluorescence spectrometry or inductively coupled plasma atomic emission spectrometry (ICP-AES). X-ray fluorescence spectrometry offers advantages such as speed, non-destructive nature, and simultaneous multi-element analysis, making it suitable for rapid screening and quantification of waste components. Inductively coupled plasma atomic emission spectrometry offers higher sensitivity and accuracy, making it particularly suitable for the precise determination of trace or critical elements. Detection allows for the determination of the actual content of each major element in the waste, providing an accurate data basis for subsequent dynamic replenishment calculations.

[0029] It should be noted that the above-mentioned key elemental composition does not cover all elements. Based on the performance sensitivity of multi-principal alloys and the physicochemical behavior of elements during the melting process, two main groups of elements have been specifically identified: volatile and easily oxidized elements and refractory and easily segregated elements. The volatile and easily oxidized elements group includes, but is not limited to, at least one of aluminum, titanium, magnesium, and manganese. These elements have high vapor pressures or extremely strong affinity for oxygen under high-temperature melting conditions, making them highly susceptible to volatilization or burn-off, resulting in a systematically low content of these elements in the final ingot. The refractory and easily segregated elements group includes, but is not limited to, at least one of tungsten, molybdenum, niobium, and tantalum. These elements have extremely high melting points and slow diffusion rates during solidification, easily causing microscopic or macroscopic compositional segregation, leading to localized uneven composition in the waste. Therefore, targeted identification and classification of these two types of elements helps to achieve subsequent differentiated compensation.

[0030] Step S2, Dynamic Material Replenishment Calculation: Based on the measured composition of the scrap, the designed composition of the target alloy, and the preset scrap feeding ratio, calculate the theoretical mass gap of each element that needs to be replenished, and compensate for the theoretical mass gap of each element according to the element category.

[0031] Specifically, after obtaining the measured composition of the scrap, the dynamic replenishment calculation step can be initiated. This step aims to calculate the additional mass of each element required to bring the composition of the recycled ingot closer to the target alloy design composition.

[0032] In some embodiments, the theoretical mass gap of each element to be added can be calculated based on the measured composition of the scrap, the designed composition of the target alloy, and the preset scrap feeding ratio. For example, if the designed content of a certain element in the target alloy is C_target, the measured content of the same element in the scrap is C_scrap, and the planned mass ratio of scrap in this batch of smelting is R, then the theoretical mass gap of that element can be calculated using the material balance formula, which will not be elaborated here.

[0033] Furthermore, the theoretical mass gap of each element can be compensated accordingly based on the element category, which may include the following steps: For any element in the group of easily volatile and oxidizable elements, such as aluminum, titanium, magnesium, or manganese, the actual loss during the smelting process is usually greater than the theoretically calculated value. Therefore, a dynamic burn-off compensation amount needs to be added to the theoretical mass deficit to obtain the actual replenishment amount. It should be noted that this dynamic burn-off compensation amount is not a fixed value, but an adjustable parameter. For example, this dynamic burn-off compensation amount can be 5%-15% of the theoretical mass deficit of the corresponding element.

[0034] Preferably, the specific value of the dynamic burn-off compensation amount is not arbitrarily selected, but determined based on historical burn-off rate data or thermodynamic simulation results of the corresponding element. For example, a database can be established to record the actual burn-off rates of different volatile / oxidizable elements under specific melting conditions (such as temperature, vacuum, and melting time). For a new batch of melting, the system can retrieve historical burn-off rates under similar conditions from the database based on preset process parameters, or run thermodynamic software (such as FactSage or Thermo-Calc) to simulate the volatilization loss of the element under given conditions, thereby dynamically and accurately determining the corresponding dynamic burn-off compensation amount. This setting allows the feeding strategy to achieve self-learning and optimization, improving process adaptability.

[0035] For any element in the refractory and easily segregated element group, such as tungsten, molybdenum, niobium, or tantalum, these elements are not easily lost through volatilization or oxidation during smelting. However, due to the possibility of local segregation in the waste, their measured content may deviate significantly from the target value. Therefore, for these elements, the actual amount to be added can be determined based on the relative relationship between their measured content and the target value.

[0036] For example, if the measured content of a corresponding element is lower than the target value, it can be supplemented according to the theoretical mass gap of the corresponding element. However, if the measured content of a corresponding element exceeds the target value, it cannot be simply solved by "not adding more," because excessive refractory elements will also damage the alloy's properties. In this case, the following two dynamic adjustment strategies can be adopted: First, reduce the proportion of the current batch of scrap, that is, reduce the amount of scrap with excessive composition, thereby diluting the proportion of excessive elements in the total furnace charge; second, use the current batch of scrap with scrap of the same series but with low content, that is, mix it with another batch of scrap with a lower content of the same element, so that the composition of the mixed scrap meets the feeding requirements. In this way, fluctuations in scrap composition can be proactively addressed, avoiding the passive acceptance or rejection of a certain batch of scrap.

[0037] Step S3: Controlled Remelting. Specifically, after completing the dynamic feeding calculation, the controlled remelting step can be initiated. At this point, the pretreated waste material can be mixed with the feeding material calculated according to step S2, and then smelted to obtain recycled ingots.

[0038] In some embodiments, the melting process can be carried out in a vacuum induction melting furnace. The vacuum environment prevents the molten alloy from reacting with oxygen, nitrogen, and other gases in the atmosphere at high temperatures, promotes the removal of volatile impurities, and effectively inhibits further oxidation and burn-off of reactive elements such as aluminum and titanium. Preferably, the ultimate vacuum degree during melting is less than or equal to 1 × 10⁻⁶. -2 Pa. At this vacuum level, the residual gas content inside the furnace is extremely low, providing excellent protection for smelting.

[0039] For example, after evacuating to a high vacuum, a high-purity inert gas (such as argon) can be refilled as a protective atmosphere to facilitate arc ignition and molten pool stirring. To ensure that all components (especially refractory elements) are fully melted and uniformly mixed, the melting temperature can be controlled to exceed the alloy liquidus temperature by 100-200°C. At this temperature, the molten pool exhibits good fluidity, and the electromagnetic stirring effect is more significant, which is beneficial for macroscopic homogenization of the composition.

[0040] In some embodiments, to further improve the purity and internal quality of the recycled ingot, step S3 may include an electroslag remelting refining step of the molten steel obtained from vacuum melting.

[0041] Specifically, in the electroslag remelting process, the ingot obtained from vacuum induction melting is used as a consumable electrode and inserted into a slag pool composed of a specific ratio of active slag. When current passes through the slag pool, resistance heat is generated, causing the electrode tip to melt and form molten metal droplets. As the molten metal droplets pass through the slag layer, they come into full contact with the high-temperature slag system, resulting in a strong metallurgical chemical reaction, thereby effectively adsorbing, deoxidizing, desulfurizing, and removing fine non-metallic inclusions. Simultaneously, the molten metal droplets form a molten metal pool below the slag pool and solidify sequentially under the forced cooling of a water-cooled crystallizer. This significantly improves the crystal structure of the ingot, reduces component segregation, and yields a high-quality regenerated ingot with a dense structure, uniform composition, and high purity.

[0042] In some embodiments, please refer to Figure 1-2 The closed-loop recycling method for multi-principal alloy waste may further include the following steps: Step S4, Regeneration Verification and Data Feedback: Sample and analyze the composition of the recycled ingot obtained in Step S3, and compare the measured data with the design composition of the target alloy; if the content of each major element falls within ±1.0 at.% of the target value, it is determined to be qualified recycled material; at the same time, the corresponding measured data is fed back to the material replenishment calculation model in Step S2 to optimize the compensation parameters in subsequent batch processing.

[0043] For example, the recycled ingot obtained in step S3 can be sampled and its composition analyzed first. The analysis method can be consistent with that in step S1, i.e., it can also be accurately analyzed using X-ray fluorescence spectrometry or inductively coupled plasma atomic emission spectrometry. Subsequently, the measured data can be compared with the designed composition of the target alloy.

[0044] Furthermore, to quantitatively evaluate the recycling effect, the following judgment criteria can be set: if the content of each major element falls within ±1.0 at.% of the target value, it is judged as qualified recycled material. Verification has shown that recycled ingots within this deviation range have key indicators such as mechanical properties and corrosion resistance comparable to alloys prepared using virgin raw materials, fully meeting the reproduction requirements for high-performance applications.

[0045] For example, after completing the quantitative evaluation of the regeneration effect, the measured data obtained in step S4 can be used as feedback information to optimize subsequent regeneration processes. Specifically, the corresponding measured data can be fed back to the feeding calculation model in step S2, which can be set as a data-driven parameter self-tuning module. After receiving the measured composition of the regenerated ingot, the feeding calculation model can compare it with the target design composition and focus on analyzing the deviation between the actual content and the target value of easily volatile and easily oxidized element groups (such as aluminum and titanium).

[0046] For example, for a group of volatile and easily oxidized elements, the feeding calculation model can calculate the actual burn-off rate of the elements during the batch smelting process (theoretical feed amount × (1 - actual yield)) and use this actual burn-off rate as a new data point to update the historical burn-off rate database under the specific combination of smelting process parameters (such as vacuum degree, smelting temperature, and holding time).

[0047] For optimizing compensation parameters under the same process conditions in the next batch, the replenishment calculation model will dynamically determine the new dynamic burn-off compensation amount based on the updated historical database and using a preset statistical algorithm (e.g., calculating the moving weighted average of the most recent N data points, or using exponential smoothing) to make it closer to the actual process trend. For example, if the actual burn-off rate of titanium in the last three batches is 8%, 9%, and 11% of the theoretical replenishment amount, respectively, the replenishment calculation model can set its moving average to 9.3% and use it as the compensation amount for the next batch.

[0048] Furthermore, for refractory and easily segregated element groups, the feedback mechanism can be used to optimize waste sorting and proportioning strategies. Specifically, when the measured content of refractory elements (such as tungsten and molybdenum) in a batch of recycled ingots exceeds the target upper limit due to waste segregation, the replenishment calculation model will record the source and composition characteristics of that batch of waste. In the next processing of similar waste, the replenishment calculation model will prioritize suggesting a reduction in the proportion of that batch of waste, or automatically search the inventory for homologous waste with complementary components (i.e., lower content of the refractory element), and calculate the optimal proportion to prevent compositional exceedances from the source.

[0049] To verify the beneficial effects of this closed-loop regeneration method, this invention also provides an application example of the method, as follows: Taking the recycling of machining chips from a certain grade of FeCoNiCrTi high-entropy alloy as an example, the target composition (atomic percentage) of this alloy can be: Co: 20 at.%, Cr: 20 at.%, Fe: 20 at.%, Ni: 20 at.%, Ti: 20 at.%, with the balance being unavoidable impurities. The following steps can be performed sequentially for this alloy waste: Step 1: Waste pretreatment and composition analysis.

[0050] First, the scrap was degreased, cleaned, and dried. Then, it was densified into cylindrical blocks with a diameter of 50mm using a cold-pressing process. X-ray fluorescence spectrometry was used to analyze multiple samples of the pressed scrap blocks, and the average measured composition was as follows: Co: 21.5 at.%, Cr: 22.1 at.%, Fe: 22.3 at.%, Ni: 21.8 at.%, Ti: 11.2 at.%. It is evident that due to oxidation and volatilization during the early stages of service or processing, the titanium content in the scrap is significantly lower than the design value.

[0051] Step 2: Dynamic material replenishment calculation.

[0052] The feed weight ratio of this batch of scrap is set at 50%. Based on material balance, the theoretical mass shortfall of pure titanium metal required to achieve the final alloy composition is calculated. Since titanium is a volatile and easily oxidized element, further loss is expected during subsequent vacuum melting. Historical database queries show that under the same melting conditions (vacuum degree 1×10⁻⁶),... -2 At a melting temperature of 1550℃ and a holding time of 20 minutes (Pa), the average burn-off rate of titanium is 10% of the theoretical replenishment amount. Therefore, the dynamic burn-off compensation amount can be set to 10%. Ultimately, the actual replenishment amount of titanium is increased by 10% based on the theoretical gap. For matrix elements such as cobalt, chromium, iron, and nickel, their properties are relatively stable, and the theoretical gap can be directly replenished.

[0053] Step 3: Controlled remelting.

[0054] The pretreated waste blocks, along with the calculated supplementary materials (pure titanium blocks and additional pure cobalt, chromium, iron, and nickel), are loaded into the crucible of the vacuum induction melting furnace. The furnace is then evacuated to a vacuum level of 1×10⁻⁶. -2 Pa, then purged with argon to a semi-vacuum state. Electric melting was initiated, controlling the melting temperature at 1550℃ (corresponding to an alloy liquidus temperature of approximately 1420℃), and electromagnetic stirring was activated. After all the furnace charge had melted, it was refined for 15 minutes and then cast into ingots. To further improve purity, the vacuum induction melting ingot can be used as a consumable electrode for electroslag remelting to obtain the final regenerated ingot.

[0055] Step 4: Regeneration Verification and Data Feedback.

[0056] Samples were cut from the electroslag remelted ingot and subjected to precise compositional analysis using inductively coupled plasma atomic emission spectrometry (ICP-AES). The results showed that the composition of the regenerated ingot was: Co: 19.9 at.%, Cr: 20.0 at.%, Fe: 20.1 at.%, Ni: 19.9 at.%, Ti: 19.8 at.%. The content of all major elements fell within ±1.0 at.% of the target value, thus meeting the acceptable standard. The actual titanium burn-off rate during this smelting process was recorded and used to update the historical database. Since the final titanium content accurately met the target, the 10% burn-off compensation was deemed appropriate, enhancing the confidence level of the model in using this compensation value. If the titanium content were lower, the model would suggest adjusting the compensation to 11% or higher the next time the same process parameters are used.

[0057] As demonstrated by the above application examples, compared to existing technologies, this closed-loop recycling method achieves a breakthrough from "uncontrollable" to "controllable." By establishing a "detection-classification compensation" model, it actively corrects deviations in waste composition, fundamentally solving the biggest challenge in the recycling of multi-principal-element alloy waste—composition reproducibility—and ensuring the consistency of recycled material performance. Secondly, this method possesses strong universality and platform applicability, not dependent on specific alloy grades, and can be widely applied to alloy systems containing multiple principal elements, making it a universal solution. Furthermore, this method allows for the stable incorporation of high proportions of low-cost waste, significantly reducing dependence on expensive primary raw materials. Simultaneously, the all-dry process avoids the environmental pollution of hydrometallurgy, achieving green, efficient, and closed-loop resource utilization, resulting in significant economic and environmental benefits. Finally, the recycled materials prepared by this method have stable composition and performance, and can be directly applied to fields with stringent performance requirements, such as aero-engine components and biomedical implants, greatly expanding the application value of recycled materials.

[0058] The specific embodiments of the present invention described above do not constitute a limitation on the scope of protection of the present invention. Any other corresponding changes and modifications made in accordance with the technical concept of the present invention should be included within the scope of protection of the claims of the present invention.

Claims

1. A closed-loop recycling method for multi-principal-element alloy waste, characterized in that, include: Step S1, Scrap Pretreatment and Composition Detection: The multi-principal element alloy scrap is pretreated, and the pretreated scrap is subjected to quantitative composition detection to identify the key element components. Step S2, Dynamic material replenishment calculation: Based on the measured composition of the scrap, the design composition of the target alloy, and the preset scrap feeding ratio, calculate the theoretical mass gap of each element that needs to be replenished, and compensate for the theoretical mass gap of each element according to the element category. Step S3, Controlled Remelting: The pretreated waste is mixed with the supplementary material calculated according to step S2 and then smelted to obtain recycled ingots.

2. The closed-loop regeneration method for components according to claim 1, characterized in that, The key elemental composition includes a group of volatile and easily oxidized elements and a group of refractory and easily segregated elements; the group of volatile and easily oxidized elements includes at least one of Al, Ti, Mg, and Mn, and the group of refractory and easily segregated elements includes at least one of W, Mo, Nb, and Ta.

3. The closed-loop regeneration method for components according to claim 2, characterized in that, The compensation for the theoretical mass gap of each element according to its category includes: For any element in the group of volatile and easily oxidized elements, the actual amount of replenishment is obtained by adding a dynamic burn-off compensation amount based on the corresponding theoretical mass gap. For any element in the group of refractory and easily segregated elements, the actual amount to be added is determined based on the relative relationship between its measured content and the target value.

4. The closed-loop regeneration method for components according to claim 3, characterized in that, The dynamic burn-off compensation amount is 5%-15% of the theoretical mass gap, and the specific value is determined based on the historical burn-off rate data or thermodynamic simulation calculation results of the corresponding element.

5. The closed-loop regeneration method for components according to claim 3, characterized in that, The determination of the actual supplement amount based on the relative relationship between the measured content and the target value includes: If the measured content of the corresponding element is lower than the target value, the corresponding theoretical quality gap shall be made up. If the measured content of the corresponding element exceeds the target value, reduce the feeding ratio of the current batch of waste, or use the current batch of waste in combination with waste of the same series with low content.

6. The closed-loop regeneration method for components according to claim 1, characterized in that, The pretreatment in step S1 includes: degreasing, washing, drying, crushing and / or densifying the waste material to form raw material blocks suitable for smelting.

7. The closed-loop regeneration method for components according to claim 1, characterized in that, The quantitative component detection in step S1 is performed using an X-ray fluorescence spectrometer or an inductively coupled plasma atomic emission spectrometer.

8. The closed-loop regeneration method for components according to claim 1, characterized in that, The melting in the step S3 is performed in a vacuum induction melting furnace, and the limit vacuum degree during the melting is less than or equal to 1 x 10 -2 Pa, and the melting temperature exceeds the liquidus temperature of the alloy by 100-200°C.

9. The closed-loop regeneration method for components according to claim 1, characterized in that, Step S3, after vacuum melting, also includes the step of electroslag remelting and refining the molten steel obtained from melting.

10. The closed-loop regeneration method for components according to claim 1, characterized in that, Also includes: Step S4, Regeneration Verification and Data Feedback: Sample and analyze the composition of the recycled ingot obtained in Step S3, and compare the measured data with the design composition of the target alloy; if the content of each major element falls within ±1.0 at.% of the target value, it is determined to be qualified recycled material; at the same time, the corresponding measured data is fed back to the material replenishment calculation model in Step S2 to optimize the compensation parameters in subsequent batch processing.

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