Multi-dimensional removal method for hydrogen damage of nickel-based superalloy

Abstract

The invention discloses a multi-dimensional removal method for hydrogen damage of a nickel-based superalloy. The multi-dimensional removal method comprises the following steps: carrying out a creep test on a nickel-based superalloy sample according to design requirements; a nickel-based high-temperature alloy sample is put into an acetone solution to be cleaned; the nickel-based high-temperature alloy sample is subjected to ultrasonic cleaning; the nickel-based superalloy sample is put into an electrolyte to be subjected to electrolytic treatment, so that the hydrogen damage defect on the surface of the nickel-based superalloy sample is removed; taking out a test block from the surface of the nickel-based superalloy sample, grinding the test block, putting the test block into a thermal desorption instrument, and carrying out a thermal desorption test to obtain a curve of the thermal desorption rate of the nickel-based superalloy test block along with the temperature change; and the nickel-based superalloy sample is put into a vacuum heat treatment furnace to be subjected to cyclic heating treatment, so that the average hydrogen concentration of the nickel-based superalloy sample is reduced. According to the method, the internal hydrogen damage defect and the surface hydrogen damage defect caused by service of the nickel-based superalloy in the hydrogen-rich environment can be removed at the same time, and therefore the mechanical property of the nickel-based superalloy is recovered.

Description

Technical Field

[0001] The present invention belongs to the technical field of dehydrogenation of nickel-based high-temperature alloys, and in particular relates to a multi-dimensional method for removing hydrogen damage from nickel-based high-temperature alloys. Background Art

[0002] At present, the carbon emissions of the global aviation transport industry account for about 2-3% of the total global carbon emissions each year. New clean energy aviation engines such as hydrogen-powered aviation engines have attracted widespread attention from countries around the world, and countries are stepping up the development of hydrogen-powered aviation engines. However, the use of current aviation engine structures and nickel-based high-temperature alloy materials will cause hydrogen damage to the hot end components of aviation engines after long-term service in a hydrogen environment, thereby reducing the structural stability of the alloy and deteriorating the performance of the alloy. Therefore, it is urgent to develop a multi-dimensional removal method for hydrogen damage in nickel-based high-temperature alloys, so as to efficiently, quickly and thoroughly remove hydrogen damage in nickel-based high-temperature alloys, including reducing the hydrogen content in the alloy and removing defects caused by hydrogen damage.

[0003] In hydrogen-powered aircraft engines, hydrogen enters the combustion chamber after gasification for combustion and drives the turbine to do work. Therefore, the parts in hydrogen-powered aircraft engines that are susceptible to hydrogen damage are nickel-based superalloys in the combustion chamber and turbine. The main components of nickel-based superalloys are γ matrix phase and γ′ strengthening phase, which play the role of solid solution strengthening and precipitation strengthening respectively, and polycrystalline alloys also contain a large number of grain boundaries. Current research shows that after hydrogen enters nickel-based superalloys, it will be enriched in grain boundaries, γ / γ′ phase boundaries, vacancies, dislocation cores and other locations, resulting in a significant increase in the local plasticity of the alloy, reducing the metal bond strength of the alloy, and promoting the aggregation of vacancies to form holes during the service of the alloy. Hydrogen promotes dislocation movement and accumulation, resulting in local stress concentration. The hydrostatic stress increases significantly, which promotes the further diffusion of hydrogen into the stress concentration area, leading to the initiation of microcracks and the generation of a large number of microvoids near the crack tip, further aggravating the degree of stress concentration at the crack tip and promoting the rapid expansion of microcracks, ultimately leading to a significant decrease in the plasticity of the nickel-based high-temperature alloy, which damages the service safety of the nickel-based high-temperature alloy in hydrogen-powered aviation engines.

[0004] The invention patent with application publication number CN102912098A discloses a method for vacuum dehydrogenation of titanium alloy blades, comprising the following steps: cleaning the blades with excessive hydrogen content with acetone; placing the blades in a metal mold vacuum furnace so that the distance between the thermocouple and the blades is 0-10 mm; evacuating the vacuum furnace to a pressure of 6.65×10 -3Pa, raise the temperature of the vacuum furnace to 500-530℃, and keep the temperature to 500-530℃ for 3-8 hours. After the insulation, the blade is cooled to 300℃ with the vacuum furnace, filled with argon gas, and cooled to 80℃ by a fan. The blade is then air-cooled and removed from the furnace to obtain a dehydrogenated blade. This technical solution is mainly designed for titanium alloy blades to remove the hydrogen content inside the blades, but it does not process the hydrogen damage defects on the surface and near the surface of the titanium alloy, such as stress layers, microcracks and micropores. These defects are caused by the alloy serving in a hydrogen environment and play a key role in promoting hydrogen-induced fracture of the alloy. Therefore, these hydrogen-induced defects need to be removed synchronously. Summary of the invention

[0005] In order to solve the problems existing in the prior art, the present invention provides a multi-dimensional removal method for hydrogen damage of a nickel-based high-temperature alloy, and the multi-dimensional removal method comprises the following steps in order:

[0006] Step 1: Prepare several nickel-based high-temperature alloy specimens according to the design requirements, and conduct creep tests on the nickel-based high-temperature alloy specimens. When the creep test is carried out for a certain period of time, the creep test is interrupted, and hydrogen damage occurs in the nickel-based high-temperature alloy specimens at this time;

[0007] Step 2: Put the nickel-based high-temperature alloy sample with hydrogen damage into acetone, and use a brush to scrub the organic and inorganic stains on the surface of the nickel-based high-temperature alloy sample until there is no obvious residue peeling off the surface of the nickel-based high-temperature alloy sample, and then rinse the nickel-based high-temperature alloy sample with clean water and anhydrous ethanol in turn, and dry it naturally;

[0008] Step 3: Place the rinsed nickel-based high-temperature alloy sample in anhydrous ethanol and use an ultrasonic cleaning machine to perform ultrasonic cleaning to further remove the residue on the surface of the nickel-based high-temperature alloy sample, then rinse the nickel-based high-temperature alloy sample with anhydrous ethanol and dry it naturally;

[0009] Step 4: Place the rinsed nickel-based high-temperature alloy sample in an electrolyte for electrolytic treatment. After the electrolytic treatment is completed, hydrogen damage defects on the surface of the nickel-based high-temperature alloy sample, including stress layer, microcracks, and micropores, can be removed;

[0010] Step 5: randomly select a nickel-based high-temperature alloy sample from a plurality of nickel-based high-temperature alloy samples after electrolysis, take out a nickel-based high-temperature alloy test block from the surface of the nickel-based high-temperature alloy sample, and use sandpaper to polish its surface flat, then put the polished nickel-based high-temperature alloy test block into a thermal desorption instrument, and perform a thermal desorption test according to the design requirements. After the thermal desorption test is completed, a curve of the thermal desorption rate of the nickel-based high-temperature alloy test block changing with temperature can be obtained;

[0011] Step 6: Place the remaining nickel-based high-temperature alloy sample after electrolysis into a vacuum heat treatment furnace for cyclic heating treatment. After the cyclic heating treatment is completed, the average hydrogen concentration of the nickel-based high-temperature alloy sample can be reduced.

[0012] Preferably, in step one, the test section of the nickel-based high-temperature alloy sample is in the shape of a flat plate, with a length of 25 mm, a width of 5 mm, and a height of 1.5 mm; the test conditions of the creep test are as follows: 90% oxygen and 10% hydrogen in the test environment, a test temperature of 850°C, an applied stress of 360 MPa, and a test time of 100 h; the nickel-based high-temperature alloy sample produces hydrogen damage, including the generation of hydrogen or an increase in the hydrogen content inside the nickel-based high-temperature alloy sample, and hydrogen damage defects on the surface or near the surface of the nickel-based high-temperature alloy sample.

[0013] In any of the above schemes, preferably, in step 2, the nickel-based high-temperature alloy sample is rinsed with clean water for 1-2 minutes.

[0014] In any of the above schemes, preferably, in step three, an ultrasonic cleaning machine is used to clean the nickel-based high-temperature alloy sample, and the ultrasonic cleaning time is 5-10 minutes.

[0015] In any of the above schemes, it is preferred that in step four, the conditions for the electrolysis treatment are: the nickel-based high-temperature alloy sample is used as the anode, the platinum electrode is used as the cathode, the electrolyte contains 20% sulfuric acid and 80% methanol, the voltage intensity is 3-8V, and the electrolysis time is 2-3 times the time from the start of electrolysis to the emergence of all bubbles on the surface of the nickel-based high-temperature alloy sample.

[0016] In any of the above schemes, preferably, in step five, the length of the nickel-based high-temperature alloy test block is 10 mm, the width is 5 mm, and the height is 1 mm; and the surface of the nickel-based high-temperature alloy test block is polished to 800# sandpaper.

[0017] In any of the above schemes, preferably, in step five, the process system of the thermal desorption test is as follows: placing the nickel-based high-temperature alloy test block in a thermal desorption instrument, heating the temperature from room temperature to 200°C at a heating rate of 5-10°C / min, and keeping it warm for 5-15min; continuing to heat the temperature from 200°C to 500°C at a heating rate of 10-15°C / min, and keeping it warm for 5-15min; continuing to heat the temperature from 500°C to 850°C at a heating rate of 8-12°C / min, and keeping it warm for 10-15min; during the entire thermal desorption test of the nickel-based high-temperature alloy test block, the change of the thermal desorption rate with temperature is observed in real time.

[0018] In any of the above schemes, preferably, in step six, the cyclic heating treatment comprises the following steps in chronological order:

[0019] Step (1): placing a nickel-based high-temperature alloy sample into a vacuum heat treatment furnace and evacuating the furnace to a vacuum degree of no more than 1 Pa;

[0020] Step (2): Heat the temperature from room temperature to Keep warm for 5-10 minutes; continue heating at a rate of 10-20℃ / min. Rise to Keep warm for 5-10 minutes; continue heating at a rate of 10-20℃ / min. Heat to T1, keep warm for 5-10 minutes; continue to cool from T1 to T2 at a cooling rate of 20-30°C / min, keep warm for 5-10 minutes; step (3): repeat step (2) three to five times, after the cycle heating treatment is completed, fill the vacuum heat treatment furnace with argon gas for cooling;

[0021] Wherein, T1 is the temperature corresponding to the highest hydrogen desorption peak in the thermal desorption test, °C; T2 is the temperature corresponding to the lowest hydrogen desorption peak in the thermal desorption test, °C.

[0022] The ultrasonic cleaning machine, direct current power supply for electrolysis, thermal desorber and vacuum heat treatment furnace used in the present invention can select existing equipment according to actual conditions, and no special requirements are made on the equipment model.

[0023] The multi-dimensional removal method of hydrogen damage to nickel-based high-temperature alloys of the present invention has the following beneficial effects:

[0024] (1) The present invention can simultaneously remove internal hydrogen and surface hydrogen damage defects caused by the nickel-based high-temperature alloy serving in a hydrogen-rich environment, thereby restoring the mechanical properties of the nickel-based high-temperature alloy.

[0025] (2) The present invention adopts an electrolytic treatment method to remove defects on the surface and near the surface of nickel-based high-temperature alloys, eliminate stress layers and microcracks caused by hydrogen entering the alloy when the alloy is serving in a hydrogen environment, and significantly reduce the content of hydrogen-induced micropores near the surface of the alloy, thereby suppressing the influence of hydrogen-induced damage at the micro and meso scales.

[0026] (3) The present invention adds a thermal desorption method to determine the hydrogen desorption temperature of the nickel-based high-temperature alloy before the cyclic heating treatment, and can dehydrogenate the alloy at the lowest possible temperature, thereby ensuring that the hydrogen concentration inside and on the surface of the alloy is reduced without damaging the alloy microstructure, and reducing the enrichment concentration of hydrogen in the alloy matrix and various hydrogen trap positions, thereby reducing the risk of alloy hydrogen damage at the microscopic scale. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 A flowchart of a preferred embodiment of a multi-dimensional method for removing hydrogen damage to a nickel-based high-temperature alloy according to the present invention;

[0028] Figure 2 for Figure 1 Thermal desorption curve of the nickel-based high-temperature alloy test block in the embodiment shown;

[0029] Figure 3 for Figure 1 Room temperature tensile curves of the nickel-based superalloy specimens with and without hydrogen damage removal in the illustrated embodiment;

[0030] Figure 4 for Figure 1 Creep curves of nickel-based high-temperature alloy specimens with and without hydrogen damage removed in the illustrated embodiment;

[0031] Figure 5 for Figure 1 Surface morphology photos of the nickel-based high-temperature alloy samples with and without hydrogen damage removed in the illustrated embodiment, wherein: (a) shows hydrogen damage not removed, (b) shows hydrogen damage removed;

[0032] Figure 6 A thermal desorption curve of a nickel-based high-temperature alloy test block in another preferred embodiment of the multi-dimensional removal method for hydrogen damage to a nickel-based high-temperature alloy according to the present invention;

[0033] Figure 7 for Figure 6 Room temperature tensile curves of the nickel-based superalloy specimens with and without hydrogen damage removal in the illustrated embodiment;

[0034] Figure 8 for Figure 6 Creep curves of nickel-based high-temperature alloy specimens with and without hydrogen damage removed in the illustrated embodiment;

[0035] Fig. 9 for Figure 6 Surface morphology photos of the nickel-based high-temperature alloy samples with and without hydrogen damage removed in the illustrated embodiment, wherein: (a) shows hydrogen damage not removed, (b) shows hydrogen damage removed;

[0036] Fig.10 A thermal desorption curve of a nickel-based high-temperature alloy test block in another preferred embodiment of the multi-dimensional removal method for hydrogen damage to a nickel-based high-temperature alloy according to the present invention;

[0037] Fig.11 for Fig.10 Room temperature tensile curves of the nickel-based superalloy specimens with and without hydrogen damage removal in the illustrated embodiment;

[0038] Fig.12 for Fig.11 Creep curves of nickel-based high-temperature alloy specimens with and without hydrogen damage removed in the illustrated embodiment;

[0039] Fig.13 for Fig.12The surface morphology photos of the nickel-based high-temperature alloy samples with and without hydrogen damage removed in the shown embodiment, wherein: (a) is without hydrogen damage removal, and (b) is with hydrogen damage removal. DETAILED DESCRIPTION

[0040] In order to further understand the content of the present invention, the present invention will be described in detail below in conjunction with specific embodiments.

[0041] Embodiment 1:

[0042] like Figure 1 As shown, according to a preferred embodiment of the multi-dimensional removal method of hydrogen damage to nickel-based high-temperature alloys of the present invention, the multi-dimensional removal method comprises the following steps in chronological order:

[0043] Step 1: Prepare several nickel-based high-temperature alloy specimens according to the design requirements, and conduct creep tests on the nickel-based high-temperature alloy specimens. When the creep test is carried out for a certain period of time, the creep test is interrupted, and hydrogen damage occurs in the nickel-based high-temperature alloy specimens at this time;

[0044] Step 2: Put the nickel-based high-temperature alloy sample with hydrogen damage into acetone, and use a brush to scrub the organic and inorganic stains on the surface of the nickel-based high-temperature alloy sample until there is no obvious residue peeling off the surface of the nickel-based high-temperature alloy sample, and then rinse the nickel-based high-temperature alloy sample with clean water and anhydrous ethanol in turn, and dry it naturally;

[0045] Step 3: Place the rinsed nickel-based high-temperature alloy sample in anhydrous ethanol and use an ultrasonic cleaning machine to perform ultrasonic cleaning to further remove the residue on the surface of the nickel-based high-temperature alloy sample, then rinse the nickel-based high-temperature alloy sample with anhydrous ethanol and dry it naturally;

[0046] Step 4: Place the rinsed nickel-based high-temperature alloy sample in an electrolyte for electrolytic treatment. After the electrolytic treatment is completed, hydrogen damage defects on the surface of the nickel-based high-temperature alloy sample, including stress layer, microcracks, and micropores, can be removed;

[0047] Step 5: randomly select a nickel-based high-temperature alloy sample from a plurality of nickel-based high-temperature alloy samples after electrolysis, take out a nickel-based high-temperature alloy test block from the surface of the nickel-based high-temperature alloy sample, and use sandpaper to polish its surface flat, then put the polished nickel-based high-temperature alloy test block into a thermal desorption instrument, and perform a thermal desorption test according to the design requirements. After the thermal desorption test is completed, a curve of the thermal desorption rate of the nickel-based high-temperature alloy test block changing with temperature can be obtained;

[0048] Step 6: Place the remaining nickel-based high-temperature alloy sample after electrolysis into a vacuum heat treatment furnace for cyclic heating treatment. After the cyclic heating treatment is completed, the average hydrogen concentration of the nickel-based high-temperature alloy sample can be reduced.

[0049] In step one, the grade of the nickel-based high-temperature alloy is DZ125; the test section of the nickel-based high-temperature alloy sample is in the shape of a flat plate, with a length of 25 mm, a width of 5 mm, and a height of 1.5 mm; the test conditions of the creep test are as follows: 90% oxygen and 10% hydrogen in the test environment, a test temperature of 850°C, an applied stress of 360 MPa, and a test time of 100 h; the nickel-based high-temperature alloy sample produces hydrogen damage, including the generation of hydrogen or an increase in hydrogen content inside the nickel-based high-temperature alloy sample, and hydrogen damage defects on the surface or near the surface of the nickel-based high-temperature alloy sample.

[0050] In step 2, the nickel-based high-temperature alloy sample is rinsed with clean water for 1 min.

[0051] In step three, an ultrasonic cleaning machine is used to clean the nickel-based high-temperature alloy sample, and the ultrasonic cleaning time is 5 minutes.

[0052] In step 4, the conditions for the electrolysis treatment are: the nickel-based high-temperature alloy sample is used as the anode, the platinum electrode is used as the cathode, the electrolyte contains 20% sulfuric acid and 80% methanol, the voltage intensity is 3V, and the electrolysis time is twice the time from the start of electrolysis to the emergence of all bubbles on the surface of the nickel-based high-temperature alloy sample.

[0053] In step five, the length of the nickel-based high-temperature alloy test block is 10 mm, the width is 5 mm, and the height is 1 mm; the surface of the nickel-based high-temperature alloy test block is polished to 800# sandpaper. The process system of the thermal desorption test is as follows: place the nickel-based high-temperature alloy test block in a thermal desorption instrument, heat the temperature from room temperature to 200°C at a heating rate of 5°C / min, and keep warm for 5 minutes; continue to heat the temperature from 200°C to 500°C at a heating rate of 10°C / min, and keep warm for 5 minutes; continue to heat the temperature from 500°C to 850°C at a heating rate of 8°C / min, and keep warm for 10 minutes; during the entire thermal desorption test of the nickel-based high-temperature alloy test block, observe the change of thermal desorption rate with temperature in real time. The thermal desorption curve of the nickel-based high-temperature alloy test block is as shown in the figure. Figure 2 shown.

[0054] In step six, the cyclic heating treatment includes the following steps in order:

[0055] Step (1): placing a nickel-based high-temperature alloy sample into a vacuum heat treatment furnace and evacuating the furnace to a vacuum degree of no more than 1 Pa;

[0056] Step (2): Heating from room temperature to That is, heat from room temperature to 356.5℃, keep warm for 5 minutes, and continue to heat at a rate of 10℃ / min. Rise to That is, from 356.5℃ to 475.3℃, keep warm for 5min; continue to increase the temperature at a rate of 10℃ / min from Raise to T1, that is, from 475.3℃ to 615℃, keep warm for 5 minutes; continue to cool down from T1 to T2 at a cooling rate of 20℃ / min, that is, from 615℃ to 98℃, keep warm for 5 minutes. Among them, T1 is the temperature corresponding to the highest hydrogen desorption peak in the thermal desorption test, 615℃; T2 is the temperature corresponding to the lowest hydrogen desorption peak in the thermal desorption test, 98℃.

[0057] Step (3): Repeat step (2) three to five times. After the cyclic heating treatment is completed, fill the vacuum heat treatment furnace with argon gas for cooling.

[0058] In this embodiment, the nickel-based high-temperature alloy samples with and without hydrogen damage removal were subjected to room temperature tensile tests at a strain rate of 1×10 -4 s -1 The room temperature tensile curve is as follows: Figure 3 As shown in the figure, it can be seen that the total tensile strain of the nickel-based superalloy sample with hydrogen damage removed is higher than that of the sample without hydrogen damage removed, which shows that the method of removing hydrogen damage in this embodiment can significantly improve the plasticity of the nickel-based superalloy. At the same time, creep tests were performed on nickel-based superalloy samples with and without hydrogen damage removed. The test curves are shown in Figure 4 As shown in the figure, it can be seen that the life of the nickel-based superalloy sample with hydrogen damage removed is longer. The surface morphology photos of the nickel-based superalloy with and without hydrogen damage removed are shown in Figure 5 As shown, (a) is the hydrogen damage not removed, (b) is the hydrogen damage removed. It can be seen from the figure that the surface of the nickel-based high-temperature alloy with hydrogen damage removed has no defects such as stress layer, microcracks, and micropores.

[0059] The ultrasonic cleaning machine, DC power supply for electrolysis, thermal desorber and vacuum heat treatment furnace used in this embodiment can be selected from existing equipment according to actual conditions, and no special requirements are made on the equipment model. The multi-dimensional removal method of hydrogen damage to nickel-based high-temperature alloys in this embodiment has the following beneficial effects: (1) It can simultaneously remove the internal hydrogen and surface hydrogen damage defects caused by the nickel-based high-temperature alloy serving in a hydrogen-rich environment, thereby restoring the mechanical properties of the nickel-based high-temperature alloy. (2) The electrolytic treatment method can remove the surface and near-surface defects of the nickel-based high-temperature alloy, remove the stress layer and microcracks generated by hydrogen entering the alloy when the alloy serves in a hydrogen environment, and significantly reduce the content of hydrogen-induced micropores near the surface of the alloy, thereby inhibiting the influence of hydrogen-induced damage at the micro and meso scales. (3) Before the cyclic heating treatment, the thermal desorption method is added to determine the hydrogen desorption temperature of the nickel-based high-temperature alloy, so that the alloy can be dehydrogenated at the lowest possible temperature, ensuring that the hydrogen concentration inside and on the surface of the alloy is reduced without damaging the alloy microstructure, and reducing the enrichment concentration of hydrogen in the alloy matrix and each hydrogen trap position, thereby reducing the risk of hydrogen damage to the alloy at the micro scale.

[0060] Embodiment 2:

[0061] According to another preferred embodiment of the multi-dimensional removal method of hydrogen damage to nickel-based high-temperature alloys of the present invention, its process flow, equipment used, technical principles, beneficial effects, etc. are basically the same as those of the first embodiment, except that:

[0062] In step one, the test section of the nickel-based high-temperature alloy sample is in the shape of a flat plate, with a length of 25 mm, a width of 5 mm, and a height of 1.5 mm; the test conditions of the creep test are as follows: 90% oxygen and 10% hydrogen in the test environment, a test temperature of 850°C, an applied stress of 360 MPa, and a test time of 100 h; the nickel-based high-temperature alloy sample produces hydrogen damage, including the generation of hydrogen or an increase in the hydrogen content inside the nickel-based high-temperature alloy sample, and hydrogen damage defects on the surface or near the surface of the nickel-based high-temperature alloy sample.

[0063] In step 2, the nickel-based high-temperature alloy sample is rinsed with clean water for 2 minutes.

[0064] In step three, an ultrasonic cleaning machine is used to clean the nickel-based high-temperature alloy sample, and the ultrasonic cleaning time is 10 minutes.

[0065] In step 4, the conditions for the electrolysis treatment are: the nickel-based high-temperature alloy sample is used as the anode, the platinum electrode is used as the cathode, the electrolyte contains 20% sulfuric acid and 80% methanol, the voltage intensity is 8V, and the electrolysis time is 3 times the time from the start of electrolysis to the emergence of all bubbles on the surface of the nickel-based high-temperature alloy sample.

[0066] In step five, the length of the nickel-based high-temperature alloy test block is 10 mm, the width is 5 mm, and the height is 1 mm; the surface of the nickel-based high-temperature alloy test block is polished to 800# sandpaper. The process system of the thermal desorption test is as follows: place the nickel-based high-temperature alloy test block in a thermal desorption instrument, heat the temperature from room temperature to 200°C at a heating rate of 10°C / min, and keep warm for 15 minutes; continue to heat the temperature from 200°C to 500°C at a heating rate of 15°C / min, and keep warm for 15 minutes; continue to heat the temperature from 500°C to 850°C at a heating rate of 12°C / min, and keep warm for 15 minutes; during the entire thermal desorption test of the nickel-based high-temperature alloy test block, observe the change of thermal desorption rate with temperature in real time. The thermal desorption curve of the nickel-based high-temperature alloy test block is as shown in the figure. Figure 6 shown.

[0067] In step six, the cyclic heating treatment includes the following steps in order:

[0068] Step (1): placing a nickel-based high-temperature alloy sample into a vacuum heat treatment furnace and evacuating the furnace to a vacuum degree of no more than 1 Pa;

[0069] Step (2): Heating from room temperature to That is, heat from room temperature to 375.5℃, keep warm for 10 minutes, and continue to heat at a rate of 20℃ / min. Rise to That is, from 375.5℃ to 500.7℃, keep warm for 10min; continue to increase the temperature at a rate of 20℃ / min from Raise to T1, that is, from 500.7℃ to 655℃, keep warm for 10min; continue to cool down from T1 to T2 at a cooling rate of 30℃ / min, that is, from 655℃ to 96℃, keep warm for 10min. Among them, T1 is the temperature corresponding to the highest hydrogen desorption peak in the thermal desorption test, 655℃; T2 is the temperature corresponding to the lowest hydrogen desorption peak in the thermal desorption test, 96℃.

[0070] Step (3): Repeat step (2) three to five times. After the cyclic heating treatment is completed, fill the vacuum heat treatment furnace with argon gas for cooling.

[0071] In this embodiment, the nickel-based high-temperature alloy samples with and without hydrogen damage removal were subjected to room temperature tensile tests at a strain rate of 1×10 -4 s -1 The room temperature tensile curve is as follows: Figure 7 As shown in the figure, it can be seen that the total tensile strain of the nickel-based superalloy sample with hydrogen damage removed is higher than that of the sample without hydrogen damage removed, which shows that the method of removing hydrogen damage in this embodiment can significantly improve the plasticity of the nickel-based superalloy. At the same time, creep tests were performed on nickel-based superalloy samples with and without hydrogen damage removed. The test curves are shown in Figure 8As shown in the figure, it can be seen that the life of the nickel-based superalloy sample with hydrogen damage removed is longer. The surface morphology photos of the nickel-based superalloy with and without hydrogen damage removed are shown in Fig. 9 As shown, (a) is the hydrogen damage not removed, (b) is the hydrogen damage removed. It can be seen from the figure that the surface of the nickel-based high-temperature alloy with hydrogen damage removed has no defects such as stress layer, microcracks, and micropores.

[0072] Embodiment three:

[0073] According to another preferred embodiment of the multi-dimensional removal method of hydrogen damage to nickel-based high-temperature alloys of the present invention, its process flow, equipment used, technical principles, beneficial effects, etc. are basically the same as those of the first embodiment, except that:

[0074] In step one, the test section of the nickel-based high-temperature alloy sample is in the shape of a flat plate, with a length of 25 mm, a width of 5 mm, and a height of 1.5 mm; the test conditions of the creep test are as follows: 90% oxygen and 10% hydrogen in the test environment, a test temperature of 850°C, an applied stress of 360 MPa, and a test time of 100 h; the nickel-based high-temperature alloy sample produces hydrogen damage, including the generation of hydrogen or an increase in the hydrogen content inside the nickel-based high-temperature alloy sample, and hydrogen damage defects on the surface or near the surface of the nickel-based high-temperature alloy sample.

[0075] In step 2, the nickel-based high-temperature alloy sample is rinsed with clean water for 1.5 minutes.

[0076] In step three, an ultrasonic cleaning machine is used to clean the nickel-based high-temperature alloy sample, and the ultrasonic cleaning time is 8 minutes.

[0077] In step 4, the conditions for the electrolysis treatment are: the nickel-based high-temperature alloy sample is used as the anode, the platinum electrode is used as the cathode, the electrolyte contains 20% sulfuric acid and 80% methanol, the voltage intensity is 5V, and the electrolysis time is 2.5 times the time from the start of electrolysis to the emergence of all bubbles on the surface of the nickel-based high-temperature alloy sample.

[0078] In step five, the length of the nickel-based high-temperature alloy test block is 10 mm, the width is 5 mm, and the height is 1 mm; the surface of the nickel-based high-temperature alloy test block is polished to 800# sandpaper. The process system of the thermal desorption test is as follows: place the nickel-based high-temperature alloy test block in a thermal desorption instrument, heat the temperature from room temperature to 200°C at a heating rate of 8°C / min, and keep warm for 10 minutes; continue to heat the temperature from 200°C to 500°C at a heating rate of 12°C / min, and keep warm for 10 minutes; continue to heat the temperature from 500°C to 850°C at a heating rate of 10°C / min, and keep warm for 12 minutes; during the entire thermal desorption test of the nickel-based high-temperature alloy test block, observe the change of the thermal desorption rate with temperature in real time. The thermal desorption curve of the nickel-based high-temperature alloy test block is as shown in the figure. Fig.10 shown.

[0079] In step six, the cyclic heating treatment includes the following steps in order:

[0080] Step (1): placing a nickel-based high-temperature alloy sample into a vacuum heat treatment furnace and evacuating the furnace to a vacuum degree of no more than 1 Pa;

[0081] Step (2): Heating from room temperature to That is, from room temperature to 421.5℃, keep warm for 8min; continue to increase the temperature at a rate of 15℃ / min from Rise to That is, from 421.5℃ to 562℃, keep warm for 8min; continue to increase the temperature at a rate of 15℃ / min from Raise to T1, that is, from 562℃ to 684℃, keep warm for 8min; continue to cool down from T1 to T2 at a cooling rate of 25℃ / min, that is, from 684℃ to 159℃, keep warm for 8min. Among them, T1 is the temperature corresponding to the highest hydrogen desorption peak in the thermal desorption test, 684℃; T2 is the temperature corresponding to the lowest hydrogen desorption peak in the thermal desorption test, 159℃.

[0082] Step (3): Repeat step (2) three to five times. After the cyclic heating treatment is completed, fill the vacuum heat treatment furnace with argon gas for cooling.

[0083] In this embodiment, the nickel-based high-temperature alloy samples with and without hydrogen damage removal were subjected to room temperature tensile tests at a strain rate of 1×10 -4 s -1 The room temperature tensile curve is as follows: Fig.11 As shown in the figure, it can be seen that the total tensile strain of the nickel-based superalloy sample with hydrogen damage removed is higher than that of the sample without hydrogen damage removed, which shows that the method of removing hydrogen damage in this embodiment can significantly improve the plasticity of the nickel-based superalloy. At the same time, creep tests were performed on nickel-based superalloy samples with and without hydrogen damage removed. The test curves are shown in Fig.12 As shown in the figure, it can be seen that the life of the nickel-based superalloy sample with hydrogen damage removed is longer. The surface morphology photos of the nickel-based superalloy with and without hydrogen damage removed are shown in Fig.13 As shown, (a) is the hydrogen damage not removed, (b) is the hydrogen damage removed. It can be seen from the figure that the surface of the nickel-based high-temperature alloy with hydrogen damage removed has no defects such as stress layer, microcracks, and micropores.

[0084] Special note: The technical solution of the present invention involves many parameters, and the synergistic effects between the various parameters need to be comprehensively considered to obtain the beneficial effects and significant progress of the present invention. Moreover, the value ranges of the various parameters in the technical solution are obtained after a large number of experiments. For each parameter and the combination of each parameter, the inventor has recorded a large amount of experimental data. Due to space limitations, the specific experimental data will not be disclosed here.

[0085] It is not difficult for those skilled in the art to understand that the multi-dimensional removal method of hydrogen damage to nickel-based high-temperature alloys of the present invention includes any combination of the invention content and specific implementation methods of the above-mentioned invention specification and the various parts shown in the drawings. Due to the limited space and to make the specification concise, the various schemes composed of these combinations are not described one by one. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection scope of the present invention.

Claims

1. A multi-dimensional method for removing hydrogen damage from a nickel-based high-temperature alloy, characterized in that: The multi-dimensional removal method comprises the following steps in order: Step 1: Prepare several nickel-based high-temperature alloy specimens according to the design requirements, and conduct creep tests on the nickel-based high-temperature alloy specimens. When the creep test is carried out for a certain period of time, the creep test is interrupted, and hydrogen damage occurs in the nickel-based high-temperature alloy specimens at this time; Step 2: Put the nickel-based high-temperature alloy sample with hydrogen damage into acetone, and use a brush to scrub the organic and inorganic stains on the surface of the nickel-based high-temperature alloy sample until there is no obvious residue peeling off the surface of the nickel-based high-temperature alloy sample, and then rinse the nickel-based high-temperature alloy sample with clean water and anhydrous ethanol in turn, and dry it naturally; Step 3: Place the rinsed nickel-based high-temperature alloy sample in anhydrous ethanol and use an ultrasonic cleaning machine to perform ultrasonic cleaning to further remove the residue on the surface of the nickel-based high-temperature alloy sample, then rinse the nickel-based high-temperature alloy sample with anhydrous ethanol and dry it naturally; Step 4: Place the rinsed nickel-based high-temperature alloy sample in an electrolyte for electrolytic treatment. After the electrolytic treatment is completed, hydrogen damage defects on the surface of the nickel-based high-temperature alloy sample, including stress layer, microcracks, and micropores, can be removed; Step 5: randomly select a nickel-based high-temperature alloy sample from a plurality of nickel-based high-temperature alloy samples after electrolysis, take out a nickel-based high-temperature alloy test block from the surface of the nickel-based high-temperature alloy sample, and use sandpaper to polish its surface flat, then put the polished nickel-based high-temperature alloy test block into a thermal desorption instrument, and perform a thermal desorption test according to the design requirements. After the thermal desorption test is completed, a curve of the thermal desorption rate of the nickel-based high-temperature alloy test block changing with temperature can be obtained; Step 6: Place the remaining nickel-based high-temperature alloy sample after electrolysis into a vacuum heat treatment furnace for cyclic heating treatment. After the cyclic heating treatment is completed, the average hydrogen concentration of the nickel-based high-temperature alloy sample can be reduced.

2. The multi-dimensional removal method of hydrogen damage in nickel-based high-temperature alloy according to claim 1, characterized in that: In step one, the test section of the nickel-based high-temperature alloy sample is in the shape of a flat plate, with a length of 25 mm, a width of 5 mm, and a height of 1.5 mm; the test conditions of the creep test are as follows: 90% oxygen and 10% hydrogen in the test environment, a test temperature of 850°C, an applied stress of 360 MPa, and a test time of 100 h; the nickel-based high-temperature alloy sample produces hydrogen damage, including the generation of hydrogen or an increase in the hydrogen content inside the nickel-based high-temperature alloy sample, and hydrogen damage defects on the surface or near the surface of the nickel-based high-temperature alloy sample.

3. The multi-dimensional removal method of hydrogen damage in nickel-based high-temperature alloy according to claim 2, characterized in that: In step 2, the nickel-based high-temperature alloy sample is rinsed with clean water for 1-2 minutes.

4. The multi-dimensional removal method of hydrogen damage in nickel-based high-temperature alloy according to claim 3, characterized in that: In step three, an ultrasonic cleaning machine is used to clean the nickel-based high-temperature alloy sample, and the ultrasonic cleaning time is 5-10 minutes.

5. The multi-dimensional removal method of hydrogen damage in nickel-based high-temperature alloy according to claim 4, characterized in that: In step 4, the conditions for the electrolytic treatment are: the nickel-based high-temperature alloy sample is used as the anode, the platinum electrode is used as the cathode, the electrolyte contains 20% sulfuric acid and 80% methanol, the voltage intensity is 3-8V, and the electrolysis time is 2-3 times the time from the start of electrolysis to the emergence of all bubbles on the surface of the nickel-based high-temperature alloy sample.

6. The multi-dimensional removal method of hydrogen damage in nickel-based high-temperature alloy according to claim 5, characterized in that: In step five, the length of the nickel-based high-temperature alloy test block is 10 mm, the width is 5 mm, and the height is 1 mm; the surface of the nickel-based high-temperature alloy test block is polished to 800# sandpaper.

7. The multi-dimensional removal method of hydrogen damage in nickel-based high-temperature alloy according to claim 6, characterized in that: In step five, the process system of the thermal desorption test is as follows: placing the nickel-based high-temperature alloy test block into a thermal desorption instrument, heating the temperature from room temperature to 200°C at a heating rate of 5-10°C / min, and keeping it warm for 5-15min; continuing to heat the temperature from 200°C to 500°C at a heating rate of 10-15°C / min, and keeping it warm for 5-15min; continuing to heat the temperature from 500°C to 850°C at a heating rate of 8-12°C / min, and keeping it warm for 10-15min; during the entire thermal desorption test of the nickel-based high-temperature alloy test block, the change of the thermal desorption rate with temperature is observed in real time.

8. The multi-dimensional removal method of hydrogen damage in nickel-based high-temperature alloy according to claim 7, characterized in that: In step six, the cyclic heating treatment includes the following steps in order: Step (1): placing a nickel-based high-temperature alloy sample into a vacuum heat treatment furnace and evacuating the furnace to a vacuum degree of no more than 1 Pa; Step (2): Heat the temperature from room temperature to Keep warm for 5-10 minutes; continue heating at a rate of 10-20℃ / min. Rise to Keep warm for 5-10 minutes; continue heating at a rate of 10-20℃ / min. Heat to T1, keep warm for 5-10 minutes; continue to cool from T1 to T2 at a cooling rate of 20-30°C / min, keep warm for 5-10 minutes; step (3): repeat step (2) three to five times, after the cycle heating treatment is completed, fill the vacuum heat treatment furnace with argon gas for cooling; Wherein, T1 is the temperature corresponding to the highest hydrogen desorption peak in the thermal desorption test, °C; T2 is the temperature corresponding to the lowest hydrogen desorption peak in the thermal desorption test, °C.

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