Cleaning agents and methods of making same, methods of removing swarf from a nickel-based alloy 690 sample, and methods of determining damage to a nickel-based alloy 690 sample after removal of swarf

By using a cleaning agent composed of disodium ethylenediaminetetraacetate, citric acid, and a reducing agent, and adjusting the pH to 3, the iron-chromium-nickel spinel oxide was destroyed and chelated, thus solving the problem of difficult removal of wear debris from the surface of nickel-based alloy 690 samples and ensuring the accuracy of experimental data.

CN123043536APending Publication Date: 2026-11-06CHINA INSTITUTE OF ATOMIC ENERGY
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Patent Information

Application Number
CN202611247720.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-08-17
Publication Date
2026-11-06

AI Technical Summary

Technical Problem

Existing technologies are insufficient to effectively remove wear debris, especially iron-chromium-nickel spinel oxide debris, from the surface of nickel-based alloy 690 samples. Furthermore, conventional methods can easily damage the alloy matrix, affecting the accuracy of fretting corrosion experiments.

Method used

The cleaning agent consists of disodium ethylenediaminetetraacetate, citric acid, a reducing agent (such as hydrazine), and deionized water. By adjusting the pH value to 3, the citric acid ionizes and breaks the bonds of iron-chromium-nickel spinel oxides. The reducing agent then reduces these oxides to soluble ions, which chelate to form stable chelates. This achieves efficient removal of wear debris and protects the alloy matrix.

Benefits of technology

Without damaging the nickel-based alloy 690 sample, efficient removal of wear debris was achieved, ensuring the accuracy of the measurement of wear volume and maximum wear depth in the fretting wear experiment and ensuring the reliability of the experimental data.

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Abstract

The embodiment of the present application relates to the field of cleaning metal materials with solution, and particularly relates to a cleaning agent and a preparation method thereof, a method for removing swarf on the surface of a nickel-based alloy 690 sample, and a method for determining damage of the nickel-based alloy 690 sample after the swarf is removed. The cleaning agent is suitable for removing swarf on the surface of the nickel-based alloy 690 sample, and comprises the following components: ethylenediaminetetraacetic acid disodium salt (EDTA), citric acid (C6H5O7), a reducing agent, an alkalizing agent, and deionized water; wherein the mass fraction of each component and the pH value of the cleaning agent are set so that the cleaning agent can remove swarf including iron-chromium-nickel spinel oxide (FeCrNi2O4). The cleaning agent uses the above components, and the mass fraction of each component and the pH value of the cleaning agent are reasonably set, so that efficient removal of the swarf is realized while the sample is not damaged, thereby eliminating the interference of the swarf on the measurement accuracy of the fretting corrosion volume and the maximum fretting corrosion depth in the fretting corrosion experiment, and ensuring that the experimental data is accurate and reliable.
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Description

Technical Field

[0001] The embodiments of this application relate to the field of cleaning metallic materials with solutions, specifically to a cleaning agent and its preparation method, a method for removing wear debris from the surface of a nickel-based alloy 690 sample, and a method for determining the damage to the nickel-based alloy 690 sample after removing wear debris. Background Technology

[0002] The statements herein are provided only as background information in connection with this application and do not necessarily constitute prior art.

[0003] In pressurized water reactors, the heat transfer tubes of the steam generator experience fretting erosion against the vibration damping strips, leading to thinning or even perforation of the tubes. Therefore, fretting erosion experiments are necessary on samples of the heat transfer tubes and vibration damping strips. The fretting erosion resistance of the heat transfer tubes is evaluated by measuring the erosion volume and maximum erosion depth. The heat transfer tubes are typically made of nickel-based alloy 690, while the vibration damping strips are typically made of 405 steel.

[0004] In fretting erosion experiments, the surface of nickel-based alloy 690 samples is covered with wear debris of a special composition formed under high-temperature, high-pressure, and high-frequency friction and wear conditions. This debris must be removed before the erosion volume and maximum erosion depth of the nickel-based alloy 690 samples can be measured. However, in practice, removing the wear debris is extremely difficult. Summary of the Invention

[0005] A brief overview of this application is provided below to offer a basic understanding of certain aspects thereof. It should be understood that this overview is not an exhaustive summary of the application. It is not intended to identify key or essential parts of the application, nor is it intended to limit its scope. Its purpose is merely to present certain concepts in a simplified form as a prelude to the more detailed description that follows.

[0006] In a first aspect, embodiments of this application provide a cleaning agent suitable for removing wear debris from the surface of a nickel-based alloy 690 sample. The cleaning agent comprises the following components: disodium ethylenediaminetetraacetate (EDTA) ), citric acid ( ), reducing agent, alkalizing agent, and deionized water; wherein, the mass fraction of each component and the pH value of the cleaning agent are set so that the cleaning agent can remove components including iron-chromium-nickel spinel oxide ( ( ) grinding debris.

[0007] The cleaning agent of this application, by employing the above-mentioned components and reasonably setting the mass fraction of each component and adjusting the pH value of the cleaning agent with an alkalizing agent, can achieve efficient removal of wear debris while ensuring that the nickel-based alloy 690 sample is not damaged. Thus, in the fretting corrosion experiment, it can eliminate the interference of wear debris on the accuracy of the measurement of fretting corrosion volume and maximum corrosion depth, and ensure that the experimental data are accurate and reliable.

[0008] Secondly, embodiments of this application also provide a method for preparing a cleaning agent suitable for removing wear debris from the surface of a nickel-based alloy 690 sample, comprising the following steps: S10: preparing disodium ethylenediaminetetraacetate (EDTA) ), citric acid ( ), hydrazine ( S20: Add ammonia water to the mixed solution obtained in step S10. Stir and adjust the pH of the mixed solution to 3 to obtain the cleaning agent.

[0009] The cleaning agent prepared by the preparation method of the embodiments of this application can achieve efficient removal of wear debris while ensuring that the nickel-based alloy 690 sample is not damaged. In this way, in the fretting corrosion experiment, the interference of wear debris on the accuracy of the measurement of fretting corrosion volume and maximum corrosion depth can be eliminated, ensuring that the experimental data are accurate and reliable.

[0010] Thirdly, embodiments of this application also provide a method for removing wear debris from the surface of a nickel-based alloy 690 sample, wherein the method uses a cleaning agent provided in any embodiment of the first aspect of this application to clean the nickel-based alloy 690 sample.

[0011] Fourthly, embodiments of this application also provide a method for determining the damage to a nickel-based alloy 690 sample after removing wear debris, comprising: S10: Select a nickel-based alloy 690 sample and determine the weight of the nickel-based alloy 690 sample; S20: A fretting abrasion test was conducted on a nickel-based alloy 690 sample and a vibration damping strip 405 steel to obtain a nickel-based alloy 690 sample with wear debris on the surface. S30: Place the cleaning agent provided in any embodiment of the first aspect of this application into a container and seal the container; S40: Heat the cleaning agent in the container to a predetermined temperature in a water bath; S50: Open the container, immerse the nickel-based alloy 690 sample with abrasive particles on the surface in the cleaning agent in the container, and then seal the container. S60: Open the container at predetermined intervals, take out the nickel-based alloy 690 sample, treat the surface of the nickel-based alloy 690 sample so that the reactants generated after the grinding debris reacts with the cleaning agent are removed from the nickel-based alloy 690 sample, put the nickel-based alloy 690 sample back into the container and seal the container, repeat the predetermined number of times, take out the nickel-based alloy 690 sample, and obtain the nickel-based alloy 690 sample after cleaning. S70; Determine the weight of the nickel-based alloy 690 sample after cleaning; S80: Compare the weight of the nickel-based alloy 690 sample without fretting abrasion test in step S10 with the weight of the nickel-based alloy 690 sample after cleaning as determined in step S70, to determine the damage of the nickel-based alloy 690 sample after removing abrasive debris. Attached Figure Description

[0012] Other objects and advantages of this application will become apparent from the following description of embodiments of this application with reference to the accompanying drawings, and will help to provide a comprehensive understanding of this application.

[0013] Figure 1 A sample of nickel-based alloy 690 to be cleaned is shown; Figure 2 The image shows a nickel-based alloy 690 sample after cleaning with the cleaning agent according to an embodiment of this application; Figure 3 The weight of the nickel-based alloy 690 sample without fretting abrasion testing is shown. Figure 4 The weight of a nickel-based alloy 690 sample after cleaning using an embodiment of this application is shown.

[0014] It should be noted that the accompanying drawings are not necessarily drawn to scale, but are shown only in a schematic manner without affecting the reader's understanding. Detailed Implementation

[0015] Exemplary embodiments of this application will be described below with reference to the accompanying drawings. For clarity and brevity, not all features of actual implementations are described in the specification. However, it should be understood that many implementation-specific decisions must be made in the development of any such actual embodiment to achieve the developer's specific goals, such as complying with constraints related to the system and business, and these constraints may vary depending on the implementation. Furthermore, it should be understood that while development work can be very complex and time-consuming, such development work is merely a routine task for those skilled in the art who benefit from the content of this application.

[0016] It should also be noted that, in order to avoid obscuring this application with unnecessary details, only the equipment structure and / or processing steps closely related to the solution according to this application are shown in the accompanying drawings, while other details that are not closely related to this application are omitted.

[0017] Because the fretting abrasion experiment is carried out in a high temperature and high pressure environment, it is accompanied by complex changes such as oxidation and plastic deformation. As a result, the abrasion debris will adhere tightly to the surface of the nickel-based alloy 690 sample. The main component of the abrasion debris is iron-chromium-nickel spinel oxide, which has strong bonding force and is difficult to dissolve. Conventional methods are difficult to completely remove the abrasion debris and cannot guarantee that the nickel-based alloy 690 matrix will not be damaged.

[0018] Embodiments of this application provide a cleaning agent suitable for removing wear debris from the surface of a nickel-based alloy 690 sample. The cleaning agent comprises the following components: disodium ethylenediaminetetraacetate (EDTA) ), citric acid ( ), reducing agent, alkalizing agent, and deionized water; wherein, the mass fraction of each component and the pH value of the cleaning agent are set so that the cleaning agent can remove components including iron-chromium-nickel spinel oxide ( ( ) grinding debris.

[0019] In the cleaning agent provided in this application embodiment, deionized water, as a high-purity mass transfer medium, can dissolve all solid components and carry ion migration; citric acid ionizes in deionized water... Its ionization It will first react with the lattice oxygen on the surface of the iron-chromium-nickel spinel oxide ( This process combines with other materials to break the Ni-O and Fe-O bonds in the iron-chromium-nickel spinel oxide, causing the surface oxide to loosen and hydrate, releasing [resources / materials]. and The reducing agent can neutralize the released insoluble substances. Restore to ,because The radius of the ion is greater than Iron-chromium-nickel spinel oxide Dislocation stress is generated within the crystal lattice, forcing adjacent bond lengths to distort, causing the spinel structure to transform from a compact state to a disordered state. Under the alternating action of citric acid and reducing agents, the complete unit cell of iron-chromium-nickel spinel oxide can directly disintegrate into a loose amorphous hydroxide layer on the solid surface, thus making it highly susceptible to… Chelation removal.

[0020] Specifically, Capable of providing strong coordination ability Anions that can react with iron-chromium-nickel spinel oxides to release... and the result of restoration They combine to form extremely stable water-soluble octahedral chelates, such as Fe-EDTA and Ni-EDTA, thereby significantly reducing the concentration of free metal ions in the solution, disrupting the solid-liquid interface dissolution equilibrium, and promoting the continuous dissolution of grinding debris. Furthermore, because the reducing agent will... Restore to , Further with It combines to form Ni-EDTA, thereby preventing Oxidation damages the passivation film on the surface of nickel-based alloy 690, thereby damaging the metal substrate and preventing... Hydrolysis to The colloid adheres to the alloy surface, thereby slowing down the reaction rate and causing secondary contamination of the wear marks on the alloy.

[0021] and, It can also work synergistically with citric acid to achieve continuous and efficient removal of wear debris and non-destructive protection of nickel-based alloy 690: on the one hand, It can also adsorb and form a physical barrier film on the surface of nickel-based alloy 690 to block the free citric acid. It isolates the alloy matrix from the substrate to prevent corrosion; on the other hand, the stability of chelated Ni-EDTA is relatively weaker than that of Fe-EDTA, and it may decompose again. and Furthermore, the hydroxyl and carboxyl groups of citric acid can also react with... They combine to form a five-membered ring chelate, thereby supplementing right Insufficient complexation.

[0022] Therefore, the cleaning agent of the embodiments of this application, by adopting the above-mentioned components, reasonably setting the mass fraction of each component, and adjusting the pH value of the cleaning agent with an alkalizing agent, can achieve efficient removal of wear debris while ensuring that the nickel-based alloy 690 sample is not damaged. Thus, in the fretting corrosion experiment, it can eliminate the interference of wear debris on the accuracy of the measurement of fretting corrosion volume and maximum corrosion depth, and ensure that the experimental data are accurate and reliable.

[0023] In some embodiments, the reducing agent is hydrazine ( ).

[0024] In such an embodiment, hydrazine, as a reducing agent, can not only release the iron-chromium-nickel spinel oxide... Restore to Destroys iron-chromium-nickel spinel oxide The rigid lattice framework causes structural instability and accelerated dissolution. It can also react with dissolved oxygen in deionized water to generate nitrogen and water, consuming dissolved oxygen that is corrosive to nickel-based alloy 690. This effectively inhibits the corrosion of nickel-based alloy 690 samples by dissolved oxygen and provides passivation protection to the matrix of nickel-based alloy 690 samples, thereby further achieving non-destructive cleaning.

[0025] In some embodiments, the alkalizing agent is ammonia ( ).

[0026] In such an embodiment, since ammonia can be generated , and free It forms a weak acid-weak base buffer pair, thereby stabilizing the pH fluctuations of the cleaning agent during the cleaning process of the alloy.

[0027] The inventors of this application have also discovered that when the pH value of the solution is less than 2, and Improved integration capabilities and The chelating ability decreases; when the pH of the solution is greater than 4, It will begin to hydrolyze into Colloid; and when the pH of the solution is 3, and citric acid and The overall chelating ability is in the cross-peak region, and at the same time, when the pH value of the solution is 3, it can also avoid damaging the matrix of the nickel-based alloy 690 sample.

[0028] Therefore, in some embodiments, the cleaning agent is set to a pH of 3.

[0029] In some embodiments, the cleaning agent is set to a pH of 3 by adding disodium ethylenediaminetetraacetate (EDTA) to the solution. ), citric acid ( Add ammonia to a mixed solution of reducing agent and deionized water. Adjust the pH of the mixed solution to 3 to obtain the cleaning agent.

[0030] In such an embodiment, disodium ethylenediaminetetraacetate (EDTA) is first prepared. ), citric acid ( A mixture of a reducing agent and deionized water is prepared, and then ammonia is added to adjust the pH value, so that the amount of ammonia to be added can be determined based on the pH value of the mixed solution.

[0031] In some embodiments, disodium ethylenediaminetetraacetate (EDTA) ) and citric acid ( The mass fraction ratio of ) is 10:1.

[0032] In such an embodiment, When mixed with citric acid at a mass ratio of 10:1, it provides a better synergistic effect for achieving continuous and efficient removal of wear debris and non-destructive protection of nickel-based alloy 690 samples. A trace amount of citric acid can provide adequate... To loosen the surface of the wear debris and release and At the same time, it does not cause corrosive damage to the alloy matrix; while high concentrations of It can act as the main chelating agent, continuously capturing released metal ions with its strong complexing ability, reducing the ion concentration at the solid-liquid interface, and thus continuously promoting the dissolution of wear debris; and, sufficient amount It can also adsorb and form a physical barrier film on the alloy surface to isolate the ionization of citric acid. Completely solve Corrosion issues with the alloy matrix.

[0033] The inventors of this application discovered that, in disodium ethylenediaminetetraacetate (EDTA) ), citric acid ( In a mixed solution of reducing agent and deionized water, When the mass fraction is above 1.5%, it ensures that all metal ions released from the wear debris can be complexed, and the wear debris can be completely dissolved; while when When the mass fraction exceeds 2%, excessive They will compete to adsorb onto the surface of the alloy sample, hindering the dissolution of the iron-chromium-nickel spinel oxide surface layer by citric acid. Furthermore, the solution viscosity is also high at this point, reducing the diffusion efficiency of ions in the solution. A citric acid mass fraction above 0.15% ensures sufficient ionization. It can dissolve the surface layer of iron-chromium-nickel spinel oxide and also... right The insufficient complexation needs to be supplemented; however, when the mass fraction of citric acid exceeds 0.2%, on the one hand, the excess citrate ions and... Forming a competitive coordination relationship, in It can also connect and At that time, the robbery should have been carried out by the authorities. Metal ions that complex to form stable chelates, especially This process generates unstable citric acid metal complexes, which are likely to hydrolyze and reprecipitate, potentially adhering to the surface of the wear tracks and affecting the measurement of wear volume and maximum wear depth. Furthermore, excessively high citric acid concentrations can corrode the alloy sample matrix. Based on redox equivalents, the mass fraction of hydrazine must be at least 0.2% to effectively remove the iron-chromium-nickel spinel oxide layer from the surface. All converted to If the concentration is less than 0.2%, reduction failure is likely to occur. However, when the mass fraction of hydrazine exceeds 0.3%, the large amount of hydrazine reacts with dissolved oxygen in the solution and decomposes to release nitrogen gas too quickly, which can easily cause bubbles and localized boiling. Furthermore, hydrazine has a certain degree of toxicity, and a mass fraction exceeding 0.3% may pose a safety risk.

[0034] Therefore, in some embodiments, in the disodium ethylenediaminetetraacetic acid (EDTA) salt ( ), citric acid ( In a mixed solution of ethylenediaminetetraacetic acid disodium salt (), reducing agent, and deionized water, the mass fraction of each component is as follows: The content is 1.5-2%, citric acid ( The concentration of hydrazine (Hydrazine) is 0.15-0.2%. The content of the component is 0.2-0.3%, and the remaining component is deionized water.

[0035] In such an embodiment, in disodium ethylenediaminetetraacetate (EDTA) ), citric acid ( In a mixed solution of reducing agent and deionized water, When the mass fraction is 1.5-2%, it can ensure that the grinding debris is fully dissolved and prevent [further damage]. Excessive adsorption of citric acid onto the surface of the alloy sample can prevent citric acid from dissolving the wear debris surface layer, while also avoiding excessively high solution viscosity that would reduce mass transfer and diffusion efficiency. A citric acid mass fraction of 0.15-0.2% ensures sufficient dissolution of the wear debris surface layer while preventing excessive citric acid from reacting with the wear debris. snatch and , in order to These components work together to achieve continuous and efficient removal of wear debris while providing non-destructive protection for nickel-based alloy 690. A hydrazine mass fraction of 0.2-0.3% ensures... All converted to This also avoids causing safety risks.

[0036] See Figure 1 and Figure 2 , Figure 1 A sample of nickel-based alloy 690 to be cleaned is shown. Figure 2 The figure shows a nickel-based alloy 690 sample after cleaning with the cleaning agent of the present application embodiment. As shown, after cleaning with the cleaning agent of the present application embodiment, the wear debris attached to the surface of the nickel-based alloy 690 sample can be completely removed, and no obvious damage is observed to the alloy substrate.

[0037] Embodiments of this application also provide a method for preparing a cleaning agent suitable for removing wear debris from the surface of a nickel-based alloy 690 sample, comprising the following steps: S10: preparing disodium ethylenediaminetetraacetate (EDTA) ), citric acid ( ), hydrazine ( S20: Add ammonia water to the mixed solution obtained in step S10. Stir and adjust the pH of the mixed solution to 3 to obtain the cleaning agent.

[0038] In the cleaning agent prepared by the method of the embodiments of this application, deionized water, as a high-purity mass transfer medium, can dissolve all solid components and carry ion migration; citric acid ionizes in deionized water. Its ionization It will first react with the lattice oxygen on the surface of the iron-chromium-nickel spinel oxide ( This process combines with other materials to break the Ni-O and Fe-O bonds in the iron-chromium-nickel spinel oxide, causing the surface oxide to loosen and hydrate, releasing [resources / materials]. and The reducing agent can neutralize the released insoluble substances. Restore to ,because The radius of the ion is greater than Iron-chromium-nickel spinel oxide Dislocation stress is generated within the crystal lattice, forcing adjacent bond lengths to distort, causing the spinel structure to transform from a compact state to a disordered state. Under the alternating action of citric acid and reducing agents, the complete unit cell of iron-chromium-nickel spinel oxide can directly disintegrate into a loose amorphous hydroxide layer on the solid surface, thus making it highly susceptible to… Chelation removal.

[0039] Specifically, Capable of providing strong coordination ability Anions that can react with iron-chromium-nickel spinel oxides to release... and the result of restoration They combine to form extremely stable water-soluble octahedral chelates, such as Fe-EDTA and Ni-EDTA, thereby significantly reducing the concentration of free metal ions in the solution, disrupting the solid-liquid interface dissolution equilibrium, and promoting the continuous dissolution of grinding debris. Furthermore, because the reducing agent will... Restore to , Further with It combines to form Ni-EDTA, thereby preventing Oxidation damages the passivation film on the surface of nickel-based alloy 690, thereby damaging the metal substrate and preventing... Hydrolysis to The colloid adheres to the alloy surface, thereby slowing down the reaction rate and causing secondary contamination of the wear marks on the alloy.

[0040] and, It can also work synergistically with citric acid to achieve continuous and efficient removal of wear debris and non-destructive protection of nickel-based alloy 690: on the one hand, It can also adsorb and form a physical barrier film on the surface of nickel-based alloy 690 to block the free citric acid. It isolates the alloy matrix from the substrate to prevent corrosion; on the other hand, the stability of chelated Ni-EDTA is relatively weaker than that of Fe-EDTA, and it may decompose again. and Furthermore, the hydroxyl and carboxyl groups of citric acid can also react with... They combine to form a five-membered ring chelate, thereby supplementing right Insufficient complexation.

[0041] And when the pH of the solution is 3, and citric acid and The overall chelating ability is in the cross-peak region, and at the same time, when the pH value of the solution is 3, it can also avoid damaging the matrix of the nickel-based alloy 690 sample.

[0042] Therefore, the cleaning agent prepared by the preparation method of the embodiments of this application can achieve efficient removal of wear debris while ensuring that the nickel-based alloy 690 sample is not damaged. Thus, in the fretting corrosion experiment, the interference of wear debris on the accuracy of the measurement of fretting corrosion volume and maximum corrosion depth can be eliminated, ensuring that the experimental data are accurate and reliable.

[0043] In some embodiments, in step S10, the mass fraction of each component in the mixed solution is: disodium ethylenediaminetetraacetate (EDTA) The content is 1.5-2%, citric acid ( The concentration of hydrazine (Hydrazine) is 0.15-0.2%. The content of the component is 0.2-0.3%, and the remaining component is deionized water.

[0044] In such an embodiment, in the mixed solution, When the mass fraction is 1.5-2%, it can ensure that the grinding debris is fully dissolved and prevent [further damage]. Excessive adsorption of citric acid onto the surface of the alloy sample can prevent citric acid from dissolving the wear debris surface layer, while also avoiding excessively high solution viscosity that would reduce mass transfer and diffusion efficiency. A citric acid mass fraction of 0.15-0.2% ensures sufficient dissolution of the wear debris surface layer while preventing excessive citric acid from reacting with the wear debris. snatch and , in order to These components work together to achieve continuous and efficient removal of wear debris while providing non-destructive protection for nickel-based alloy 690. A hydrazine mass fraction of 0.2-0.3% ensures... All converted to This also avoids causing safety risks.

[0045] In some embodiments, disodium ethylenediaminetetraacetate (EDTA) ), citric acid ( ), hydrazine ( ), deionized water and ammonia water ( All chemical reagents used are analytical grade.

[0046] Embodiments of this application also provide a method for removing wear debris from the surface of a nickel-based alloy 690 sample, wherein the method uses a cleaning agent provided in any embodiment of this application to clean the nickel-based alloy 690 sample.

[0047] The method of the embodiments of this application, by using the cleaning agent provided in any embodiment of this application to clean the nickel-based alloy 690 sample, can achieve efficient removal of wear debris while ensuring that the nickel-based alloy 690 sample is not damaged. Thus, in the fretting corrosion experiment, the interference of wear debris on the accuracy of the measurement of fretting corrosion volume and maximum corrosion depth can be eliminated, ensuring that the experimental data are accurate and reliable.

[0048] In some embodiments, the method specifically includes the following steps: S10: placing the cleaning agent in a container and sealing the container; S20: heating the cleaning agent in the container to a predetermined temperature in a water bath; S30: opening the container, immersing the nickel-based alloy 690 sample to be cleaned in the cleaning agent in the container, and sealing the container; S40: opening the container at predetermined intervals, taking out the nickel-based alloy 690 sample, treating the surface of the nickel-based alloy 690 sample so that the reactants generated after the abrasive particles react with the cleaning agent are removed from the nickel-based alloy 690 sample, putting the nickel-based alloy 690 sample back into the container and sealing the container, repeating the process a predetermined number of times, and then taking out the nickel-based alloy 690 sample to obtain the cleaned nickel-based alloy 690 sample.

[0049] In this embodiment, during the cleaning process, the container is sealed after the cleaning agent is placed inside to prevent carbon dioxide from entering and affecting the pH value of the cleaning agent. During the reaction, the nickel-based alloy 690 sample is removed at predetermined intervals and its surface is treated to remove the reactants from the sample, which helps to expose unreacted wear debris on the sample to react with the cleaning agent.

[0050] In some embodiments, treating the surface of the nickel-based alloy 690 sample so that the reactants generated after the grinding debris reacts with the cleaning agent are removed from the nickel-based alloy 690 sample specifically involves lightly brushing the surface of the nickel-based alloy 690 sample so that the reactants generated after the grinding debris reacts with the cleaning agent are removed from the nickel-based alloy 690 sample.

[0051] In some embodiments, the predetermined temperature is 90°C, the predetermined time is 20 minutes, and the predetermined number of times is 5. In such embodiments, the nickel-based alloy 690 sample and the cleaning agent can react at the temperature required for the reaction. The sample is removed and the surface of the nickel-based alloy 690 sample is treated every 20 minutes to allow the reactants generated from the reaction of the wear debris and the cleaning agent to detach from the nickel-based alloy 690 sample. This process is repeated 5 times, and after soaking for approximately 100 minutes, sufficient removal of wear debris from the sample surface is achieved.

[0052] Embodiments of this application also provide a method for determining the damage to a nickel-based alloy 690 sample after removing grinding debris, comprising: S10: Select a nickel-based alloy 690 sample and determine the weight of the nickel-based alloy 690 sample; S20: A fretting abrasion test was conducted on a nickel-based alloy 690 sample and a vibration damping strip 405 steel to obtain a nickel-based alloy 690 sample with wear debris on the surface. S30: Place the cleaning agent provided in any embodiment of this application into a container and seal the container; S40: Heat the cleaning agent in the container to a predetermined temperature in a water bath; S50: Open the container, immerse the nickel-based alloy 690 sample with abrasive particles on the surface in the cleaning agent in the container, and then seal the container. S60: Open the container at predetermined intervals, take out the nickel-based alloy 690 sample, treat the surface of the nickel-based alloy 690 sample so that the reactants generated after the grinding debris reacts with the cleaning agent are removed from the nickel-based alloy 690 sample, put the nickel-based alloy 690 sample back into the container and seal the container, repeat the predetermined number of times, take out the nickel-based alloy 690 sample, and obtain the nickel-based alloy 690 sample after cleaning. S70; Determine the weight of the nickel-based alloy 690 sample after cleaning; S80: Compare the weight of the nickel-based alloy 690 sample without fretting abrasion test in step S10 with the weight of the nickel-based alloy 690 sample after cleaning as determined in step S70, to determine the damage of the nickel-based alloy 690 sample after removing abrasive debris.

[0053] The method of this application embodiment, by comparing the weight of the nickel-based alloy 690 sample before the fretting abrasion test with its weight after the fretting abrasion test and the removal of surface wear debris, can directly determine the damage to the nickel-based alloy 690 sample after cleaning it with the cleaning agent of this application. This verifies that the cleaning agent of this application can remove wear debris from the alloy surface without damaging the nickel-based alloy 690 substrate.

[0054] See Figure 3 and Figure 4 , Figure 3 The weight of a nickel-based alloy 690 sample without fretting abrasion testing is shown. Figure 4 The figure shows the weight of a nickel-based alloy 690 sample after cleaning with the cleaning agent of this application. As shown in the figure, the weight of the nickel-based alloy 690 sample without fretting abrasion test is 7.45007 g, and the weight of the nickel-based alloy 690 sample after cleaning is 7.45000 g. The weight loss of the nickel-based alloy 690 sample after cleaning with the cleaning agent of this application is only 0.07 mg, which should be due to the balance error. This proves that the matrix of the nickel-based alloy 690 sample was not damaged after cleaning with the cleaning agent of this application.

[0055] Regarding the embodiments of this application, it should also be noted that, without conflict, the embodiments of this application and the features in the embodiments can be combined with each other to obtain new embodiments.

[0056] The above description is merely a specific embodiment of this application, but the scope of protection of this application is not limited thereto. The scope of protection of this application shall be determined by the scope of the claims.

Claims

1. A cleaning agent suitable for removing wear debris from the surface of a nickel-based alloy 690 sample, characterized in that, The cleaning agent includes the following components: disodium ethylenediaminetetraacetate (EDTA-1,5-diaminetetraacetate) ), citric acid ( ), reducing agent, alkalizing agent, and deionized water; The mass fraction of each component and the pH value of the cleaning agent are set such that the cleaning agent can remove components including iron-chromium-nickel spinel oxide (…). ( ) grinding debris.

2. The cleaning agent according to claim 1, characterized in that, The reducing agent is hydrazine ( ).

3. The cleaning agent according to claim 2, characterized in that, The alkalizing agent is ammonia water ( ).

4. The cleaning agent according to claim 3, characterized in that, The cleaning agent is set to a pH of 3.

5. The cleaning agent according to claim 4, characterized in that, The cleaning agent is set to pH 3 by the following method: by adding the disodium ethylenediaminetetraacetate (EDTA) salt ( ), the citric acid ( Ammonia water is added to the mixed solution of the reducing agent and the deionized water. The pH of the mixed solution is adjusted to 3 to obtain the cleaning agent.

6. The cleaning agent according to claim 5, characterized in that, The disodium ethylenediaminetetraacetate ( ) and the citric acid ( The mass fraction ratio of ) is 10:

1.

7. The cleaning agent according to claim 6, characterized in that, The disodium ethylenediaminetetraacetate (EDTA) ), the citric acid ( The mass fraction of each component in the mixed solution of the reducing agent and the deionized water is as follows: the disodium ethylenediaminetetraacetate (EDTA) The content is 1.5-2%, and the citric acid ( The concentration of hydrazine ( ) is 0.15-0.2%. The content of the component is 0.2-0.3%, and the remaining component is the deionized water.

8. A method for preparing a cleaning agent suitable for removing wear debris from the surface of a nickel-based alloy 690 sample, characterized in that, It includes the following steps: S10: Preparation of disodium ethylenediaminetetraacetate ( ), citric acid ( ), hydrazine ( A mixed solution of deionized water; S20: Add ammonia water to the mixed solution obtained in step S10. Stir and adjust the pH of the mixture to 3 to obtain the cleaning agent.

9. The method according to claim 8, characterized in that, In step S10, In the mixed solution, the mass fraction of each component is: the disodium ethylenediaminetetraacetate (EDTA) ( The content is 1.5-2%, and the citric acid ( The concentration of hydrazine ( ) is 0.15-0.2%. The content of the component is 0.2-0.3%, and the remaining component is the deionized water.

10. A method for removing wear debris from the surface of a nickel-based alloy 690 sample, characterized in that, The method uses the cleaning agent as described in any one of claims 1-7 to clean the nickel-based alloy 690 sample.

11. The method according to claim 10, characterized in that, The method specifically includes the following steps: S10: Place the cleaning agent in a container and seal the container; S20: Heat the cleaning agent in the container to a predetermined temperature in a water bath; S30: Open the container, immerse the nickel-based alloy 690 sample to be cleaned in the cleaning agent in the container, and then seal the container; S40: Open the container at predetermined intervals, take out the nickel-based alloy 690 sample, treat the surface of the nickel-based alloy 690 sample so that the reactants generated after the abrasive and the cleaning agent react with each other are removed from the nickel-based alloy 690 sample, put the nickel-based alloy 690 sample back into the container and seal the container, repeat the process a predetermined number of times, take out the nickel-based alloy 690 sample, and obtain the cleaned nickel-based alloy 690 sample.

12. A method for determining the damage to a nickel-based alloy 690 sample after removing grinding debris, characterized in that, It includes: S10: Select a nickel-based alloy 690 sample and determine the weight of the nickel-based alloy 690 sample; S20: The nickel-based alloy 690 sample was subjected to a fretting abrasion test with the vibration damping strip 405 steel to obtain a nickel-based alloy 690 sample with wear debris on the surface. S30: Place the cleaning agent as described in any one of claims 1-7 into a container and seal the container; S40: Heat the cleaning agent in the container to a predetermined temperature in a water bath; S50: Open the container, immerse the nickel-based alloy 690 sample with abrasive particles on its surface in the cleaning agent in the container, and then seal the container. S60: Open the container at predetermined intervals, take out the nickel-based alloy 690 sample, treat the surface of the nickel-based alloy 690 sample so that the reactants generated after the abrasive and the cleaning agent react with each other are removed from the nickel-based alloy 690 sample, put the nickel-based alloy 690 sample back into the container and seal the container, repeat the process a predetermined number of times, take out the nickel-based alloy 690 sample, and obtain the cleaned nickel-based alloy 690 sample; S70; Determine the weight of the nickel-based alloy 690 sample after cleaning; S80: Compare the weight of the nickel-based alloy 690 sample without fretting abrasion test in step S10 with the weight of the nickel-based alloy 690 sample after cleaning as determined in step S70, to determine the damage to the nickel-based alloy 690 sample after removing abrasive debris.