CN110453164B - Processing method for enhancing oxidation resistance of forged Ni-Cr-Co-based alloy - Google Patents
Processing method for enhancing oxidation resistance of forged Ni-Cr-Co-based alloy Download PDFInfo
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Abstract
The invention discloses a processing method for enhancing the oxidation resistance of a forged Ni-Cr-Co-based alloy, which comprises the following steps of 1) stress relief annealing treatment; 2) pre-solid solution treatment; 3) multi-stage solution treatment; 4) pre-stretching treatment; 5) stress relief annealing treatment; 6) repeating the step 4) and the step 5) until the axial tensile deformation of the alloy reaches 8-10 percent; 7) and (5) aging treatment. The method starts from the alloy itself, improves the binding force of the protective oxide film and the matrix through a series of heat treatment means, greatly improves the oxidation resistance of the alloy, prolongs the service life of the alloy, and also improves the comprehensive mechanical property of the alloy.
Description
Technical Field
The invention belongs to the field of high-temperature alloy structural materials, and particularly relates to a treatment method for enhancing the oxidation resistance of a forged Ni-Cr-Co-based alloy.
Background
The high-temperature alloy is a metal material capable of working for a long time at a temperature of more than 600 ℃ and under a certain stress condition, and has excellent high-temperature strength, good fatigue performance, good fracture toughness and other comprehensive properties. The characteristics of superalloys make them an irreplaceable key material in aircraft engines. The nickel-based superalloy is one of the currently widely used superalloys, and many key components of the aircraft engine are made of the nickel-based superalloy. Because the working environment of an aircraft engine is severe and the aircraft engine often needs to work in a high-temperature and high-pressure environment, the improvement of the oxidation resistance of the nickel-based high-temperature alloy is particularly important.
Generally, the oxidation resistance of the nickel-based high-temperature alloy is mainly determined by a protective oxide film generated on the surface of the alloy, and elements playing an oxidation resistance role in the nickel-based high-temperature alloy are mainly an Al element and a Cr element. Al element reacts with oxygen in air to generate compact Al2O3Film, Cr element also reacts with oxygen to form Cr2O3And (3) a membrane. Due to high temperature above 1000 DEG CUnder the condition of Al2O3The stability of the alloy is obviously superior to that of Cr2O3Therefore, if the alloy is used at a temperature higher than 1000 ℃, the Al content is significantly higher than that of Cr, and Al is formed in the final alloy2O3A protective oxide film mainly, and if the service temperature of the alloy is lower than 1000 ℃, the content of Cr element in the alloy is high, and finally Cr is generated2O3A protective oxide film mainly.
Coating is also an important method for improving the oxidation resistance of the alloy, and the basic principle of the coating is similar to that of a protective oxide film, and a barrier is manufactured artificially to isolate the chemical reaction of oxygen and the alloy. However, the coating method has an important disadvantage that for some key components, if the oxidation resistance of the coating is poor, the coating can cause serious damage to the component once the coating fails. Even if the oxidation resistant coating is sufficiently reliable, manufacturable and inexpensive, there are several fundamental issues to consider: (1) there must be a good thermal expansion match between the coating and the substrate, otherwise cracking or other failure behavior may occur; (2) the coating must have good chemical compatibility with the substrate or else poor phases will form; (3) from the viewpoint of mechanical properties, most of the oxidation-resistant coating compositions have relatively low high-temperature strength, and thus fatigue or deformation problems may occur during use, thereby limiting the durability thereof; (4) there may be long-term interdiffusion problems between the coating and the substrate. Therefore, a new method for improving the oxidation resistance of the alloy is needed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a treatment method for enhancing the oxidation resistance of the forged Ni-Cr-Co-based alloy.
The technical scheme for solving the technical problem is to provide a processing method for enhancing the oxidation resistance of a forged Ni-Cr-Co-based alloy, which is characterized by comprising the following steps of:
1) stress relief annealing treatment: preserving the heat of the forged Ni-Cr-Co base alloy at 700-750 ℃ for 1-3 h, then cooling the alloy in a furnace to room temperature, and taking out the alloy;
2) pre-solid solution treatment: keeping the temperature at 820-870 ℃ for 6-8 h, and air-cooling to room temperature after discharging;
3) multi-stage solution treatment: preserving the heat for 1 to 3 hours at the temperature of 950 to 980 ℃; each solid solution treatment is carried out by heating to 10-15 ℃ on the basis of the previous solid solution treatment, keeping the temperature for the same time, and finally discharging and then air cooling to room temperature;
4) pre-stretching treatment: carrying out axial pre-stretching treatment by using a universal material testing machine under the condition of room temperature, wherein the axial stretching amount is 2-5%, the stretching speed is 0.1-0.3mm/min, and discharging from a furnace and cooling to room temperature after the stretching is finished;
5) stress relief annealing treatment: preserving heat for 1-3 h at 700-750 ℃, then cooling the furnace to room temperature and taking out;
6) repeating the step 4) and the step 5) until the axial tensile deformation of the alloy reaches 8-10 percent;
7) aging treatment: keeping the temperature at 770-800 ℃ for 2-8 h; and cooling the furnace to 680-710 ℃, preserving the heat for 6-8 h, and cooling the furnace to room temperature after discharging.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method starts from the alloy itself, improves the binding force of the protective oxide film and the matrix through a series of heat treatment means and stretching treatment, greatly improves the oxidation resistance of the alloy, prolongs the service life of the alloy, and also improves the comprehensive mechanical property of the alloy.
(2) The method is simple to operate, reduces the cost for processing the alloy, and has strong universality.
(3) The treated alloy has uniform structure, more gamma' phases (with the size of 10-36 nm) with round shapes are separated out, eta phases oriented along grain boundaries are reduced, and Cr is greatly improved2O3The binding force of the membrane and the matrix reduces the generation of porous NiO, and other mechanical properties of the alloy are not sacrificed while the oxidation resistance of the alloy is improved.
Drawings
FIG. 1 is a structural morphology diagram of an alloy obtained in example 1 of the present invention;
FIG. 2 is a structural morphology diagram of the alloy obtained in example 1 of the present invention after oxidation for 80 h;
FIG. 3 is a graph showing the oxidation kinetics of a forged Ni-Cr-Co based alloy for 80h oxidation with the alloy obtained in example 1 of the present invention.
Detailed Description
Specific examples of the present invention are given below. The specific examples are only intended to illustrate the invention in further detail and do not limit the scope of protection of the claims of the present application.
The invention provides a processing method (short method) for enhancing the oxidation resistance of a forged Ni-Cr-Co-based alloy, which is characterized by comprising the following steps:
1) stress relief annealing treatment: preserving heat of a forged Ni-Cr-Co-based alloy (alloy for short) in a box-type furnace at the temperature of 700-750 ℃ for 1-3 h, cooling the furnace to room temperature, and taking out; the purpose of stress relief annealing is to eliminate residual stress generated in the forging process of the alloy and effectively improve the bonding force between an oxide film and a substrate;
2) pre-solid solution treatment: preserving the heat of the alloy obtained in the previous step in a box furnace at the temperature of 820-870 ℃ for 6-8 h, and air-cooling the alloy to room temperature after discharging; the pre-solid solution has the function of ensuring that a proper amount of eta phase is precipitated on a grain boundary to improve the notch resistance sensitivity of the alloy;
3) multi-stage solution treatment: preserving the heat of the alloy obtained in the previous step for 1-3 h in a box furnace at the temperature of 950-980 ℃; each solid solution treatment is carried out by heating to 10-15 ℃ on the basis of the previous solid solution treatment, keeping the temperature for the same time, and finally discharging and then air cooling to room temperature; in the embodiment, three times of solution treatment are carried out; the aim of multi-stage solid solution is to fully dissolve the strengthening elements of the alloy into the nickel-based solid solution and dissolve carbides and gamma' in the matrix to be equal so as to obtain a supersaturated solid solution, and the strengthening phase with fine particles can be conveniently separated out again during aging treatment;
4) pre-stretching treatment: carrying out axial pre-stretching treatment on the alloy obtained in the previous step by using a universal material testing machine under the room temperature condition, wherein the axial stretching amount is 2-5%, the stretching speed is 0.1-0.3mm/min, and discharging from a furnace and cooling to the room temperature after the stretching is finished; the mechanical property and the intercrystalline corrosion resistance of the alloy are improved by pre-stretching;
5) stress relief annealing treatment: preserving the heat of the alloy obtained in the previous step in a box type furnace at the temperature of 700-750 ℃ for 1-3 h, cooling the furnace to room temperature, and taking out; the residual stress generated by the alloy after pre-stretching can be eliminated by stress relief annealing, and the bonding force between the oxide film and the substrate is increased;
6) repeating the step 4) and the step 5) until the axial tensile deformation of the alloy reaches 8-10 percent;
7) aging treatment: preserving the heat of the alloy obtained in the previous step in a box furnace at the temperature of 770-800 ℃ for 2-8 h; cooling to 680-710 ℃ in the furnace, preserving heat for 6-8 h, and air cooling to room temperature after discharging; by carrying out aging treatment, a large amount of round and fine gamma' strengthening phases can be precipitated from the alloy, the binding force between an oxidation film and a matrix is improved, the generation of porous NiO during oxidation is reduced, the anti-stripping property of the oxidation film is improved, and the comprehensive mechanical property of the alloy is improved;
preferably, the holding process is carried out in a uniform temperature zone of the box furnace throughout the treatment process. The box-type furnace can adopt a box-type resistance furnace; the box-type furnace has the functions of quickly lifting and lowering temperature and controlling the temperature lifting and lowering speed.
Preferably, the steps 1) to 3) and 5) to 7) are carried out under a protective gas; the protective gas is argon, and the gas flow is 1-15L/min.
Preferably, in the whole treatment process, the alloy is placed in a crucible made of high-temperature-resistant corundum, and the crucible needs to be heated at 700 ℃ for 3 hours before use to remove moisture.
Preferably, the forged Ni-Cr-Co-based alloy is a known nickel-based superalloy, developed by the research and development institute of aviation materials, Beijing, China aviation, and comprises the following components in percentage by mass: 0.024%; cr element: 18.53 percent; al element: 1.55 percent; ti element: 0.80 percent; nb element: 5.34 percent; w element: 1.08 percent; mo element: 2.85 percent; co element: 9.26 percent; fe element: 8.82 percent; p element: 0.011 percent; b element: 0.0072 percent; the balance being Ni element.
Preferably, before the whole process is carried out, the alloy needs to be prepared: cutting the forged Ni-Cr-Co base alloy into cylinders with the diameter of 8mm and the height of 8mm by using a wire cutting machine, then ultrasonically cleaning the cylinders in alcohol for 10min, and drying the cylinders for later use.
The equipment and procedures used in the present process are well known in the art.
Example 1
Preparation before treatment: cutting the forged Ni-Cr-Co-based alloy into cylindrical alloy samples with the diameter of 8mm and the height of 8mm by using a wire cutting machine, then ultrasonically cleaning the cylindrical alloy samples in alcohol for 10min, and drying the cylindrical alloy samples for later use; and (3) placing the corundum crucible into a furnace at 700 ℃ for heat preservation for 3h for dehumidification for later use.
1) Performing stress relief annealing treatment: heating the box furnace to 700 ℃, placing the crucible containing the alloy sample into a uniform temperature area of the box furnace after the temperature is stable, and introducing argon for gas protection; keeping the temperature of the alloy sample in a box-type furnace for 1h, stopping gas protection, cooling the furnace to room temperature, and taking out;
2) carrying out pre-solid solution treatment: heating the box furnace to 820 ℃, placing the crucible containing the alloy sample subjected to stress relief annealing into a uniform temperature area of the box furnace after the temperature is stable, and introducing argon for gas protection; keeping the temperature of the alloy sample in a box furnace for 6 hours, stopping gas protection, taking out the crucible containing the alloy sample, and carrying out air cooling to room temperature;
3) carrying out multistage solution treatment: heating the box furnace to 950 ℃, placing the crucible containing the alloy sample subjected to the pre-solution treatment into a uniform temperature region of the box furnace after the temperature is stable, and introducing argon for gas protection; keeping the temperature of the alloy sample in a box furnace for 1h, then heating the box furnace to 960 ℃, keeping the temperature for 1h, heating the box furnace to 970 ℃, keeping the temperature for 1h, stopping gas protection, then taking out the crucible containing the alloy sample, and carrying out air cooling to the room temperature;
4) performing pre-stretching treatment: carrying out axial pre-stretching treatment on the alloy obtained in the previous step by using a universal material testing machine under the room temperature condition, wherein the axial stretching amount is 2%, the stretching speed is 0.15mm/min, and cooling to the room temperature by water after the stretching is finished;
5) performing stress relief annealing treatment: heating the box furnace to 700 ℃, placing the crucible containing the alloy sample subjected to pre-stretching treatment into a uniform temperature area of the box furnace after the temperature is stable, and introducing argon for gas protection; keeping the temperature of the alloy sample in a box-type furnace for 1h, stopping gas protection, cooling the furnace to room temperature, and taking out;
6) repeating the step 4) and the step 5) until the axial tensile deformation of the whole alloy reaches 8%;
7) and (3) carrying out aging treatment: heating the box furnace to 770 ℃, placing the crucible containing the alloy sample subjected to tensile deformation into a uniform temperature region of the box furnace after the temperature is stable, and introducing argon for gas protection; and (3) keeping the temperature of the alloy sample in a box type furnace for 2h, then cooling the furnace to 680 ℃, keeping the temperature for 6h, stopping gas protection, then taking out the crucible containing the alloy sample, and carrying out air cooling to room temperature to obtain the nickel-based high-temperature alloy with excellent oxidation resistance.
The treated alloy has uniform structure, more gamma' phases (with the size of 10-36 nm) with round shapes are separated out, eta phases oriented along grain boundaries are reduced, and Cr is greatly improved2O3The binding force of the membrane and the matrix reduces the generation of porous NiO, and other mechanical properties of the alloy are not sacrificed while the oxidation resistance of the alloy is improved.
And (3) carrying out a long-term oxidation experiment on the treated alloy in a box type furnace, wherein the temperature is 700 ℃, and the oxidation time is 80 h. Before the alloy was placed in the box furnace, the alloy was weighed with an electronic balance with an accuracy of 0.0001g, and then alloy samples were taken out at time points of oxidation of 1h, 5h, 10h, 20h, 30h, 40h, 50h, 60h, 70h, and 80h, respectively, and the mass thereof was weighed with an electronic balance. As shown in FIG. 3, when oxidized at 700 ℃/80h, compared with the original alloy without heat treatment, the oxidation kinetics curve and the oxidation rate curve of the alloy are relatively stable, and no obvious phenomenon of weight gain or reduction occurs, which indicates that the alloy treated by the method has good oxidation resistance.
Example 1 shows that the alloy obtained by the method not only enhances the oxidation resistance, but also improves the mechanical property to a certain extent. Since the alloy is produced by forging, a large amount of stress is accumulated in the alloy, and if stress relief annealing is not performed, an oxide film is easy to fall off under the action of the stress, and certain influence is exerted on the oxidation resistance of the alloy. The purpose of the pre-solution treatment is to ensure that a small amount of eta phase is present at the grain boundaries, which is not a strengthening phase of the alloy, but if the eta phase in the alloy is completely eliminated, the situation is also unfavorable for the comprehensive mechanical properties of the alloy, and relevant studies show that the eta phase present in the alloy has a certain relationship with the notch fracture resistance, and that when the mass fraction of the eta phase is reduced to about 1.1 wt%, individual samples have higher notch sensitivity, and when the mass fraction of the eta phase is reduced to 0.06 wt%, all samples show obvious notch fracture signs. Therefore, for nickel-base superalloys, the eta phase cannot be completely removed and a portion of the eta phase still needs to be retained. The solution treatment is to dissolve carbides and gamma 'in a matrix to obtain a uniform supersaturated solid solution, so that a gamma' strengthening phase with fine particles and uniform distribution is conveniently precipitated again during aging treatment, and simultaneously stress generated by cold and hot processing is eliminated. The alloy is subjected to certain plastic deformation in advance and then subjected to aging treatment, so that crystal grains can be effectively refined, various harmful phases in the alloy are eliminated, a round and fine gamma' phase is precipitated, and the binding force between an oxide film and a matrix is improved.
Nothing in this specification is said to apply to the prior art.
Claims (7)
1. A treatment method for enhancing the oxidation resistance of a forged Ni-Cr-Co base alloy is characterized by comprising the following steps:
1) stress relief annealing treatment: preserving the heat of the forged Ni-Cr-Co base alloy at 700-750 ℃ for 1-3 h, then cooling the alloy in a furnace to room temperature, and taking out the alloy;
2) pre-solid solution treatment: keeping the temperature at 820-870 ℃ for 6-8 h, and air-cooling to room temperature after discharging;
3) multi-stage solution treatment: preserving the heat for 1 to 3 hours at the temperature of 950 to 980 ℃; each solid solution treatment is carried out by heating to 10-15 ℃ on the basis of the previous solid solution treatment, keeping the temperature for the same time, and finally discharging and then air cooling to room temperature;
4) pre-stretching treatment: carrying out axial pre-stretching treatment by using a universal material testing machine under the condition of room temperature, wherein the axial stretching amount is 2-5%, the stretching speed is 0.1-0.3mm/min, and discharging from a furnace and cooling to room temperature after the stretching is finished;
5) stress relief annealing treatment: preserving heat for 1-3 h at 700-750 ℃, then cooling the furnace to room temperature and taking out;
6) repeating the step 4) and the step 5) until the axial tensile deformation of the alloy reaches 8-10 percent;
7) aging treatment: keeping the temperature at 770-800 ℃ for 2-8 h; cooling the furnace to 680-710 ℃, preserving the heat for 6-8 h, and air-cooling the furnace to room temperature after discharging;
the forged Ni-Cr-Co-based alloy comprises the following components in percentage by mass: 0.024%; cr element: 18.53 percent; al element: 1.55 percent; ti element: 0.80 percent; nb element: 5.34 percent; w element: 1.08 percent; mo element: 2.85 percent; co element: 9.26 percent; fe element: 8.82 percent; p element: 0.011 percent; b element: 0.0072 percent; the balance of Ni element nickel-base high-temperature alloy.
2. The method as claimed in claim 1, wherein the maintaining step is performed in a uniform temperature zone of a chamber furnace during the entire process.
3. The method of claim 1, wherein step 3) comprises three solution treatments.
4. The method for enhancing oxidation resistance of as-forged Ni-Cr-Co based alloy according to claim 1, wherein the steps 1) -3) and 5) -7) are performed under a protective gas.
5. The treatment method for enhancing the oxidation resistance of the as-forged Ni-Cr-Co based alloy according to claim 4, wherein the protective gas is argon, and the gas flow rate is 1-15L/min.
6. The method as claimed in claim 1, wherein the alloy is placed in a crucible made of refractory corundum and the crucible is heated at 700 ℃ for 3 hours before use.
7. The processing method for enhancing the oxidation resistance of the as-forged Ni-Cr-Co based alloy according to claim 1, wherein the as-forged Ni-Cr-Co based alloy is cut into a cylindrical shape having a diameter of 8mm and a height of 8mm by a wire cutter before the whole processing process is performed, and then ultrasonically cleaned in alcohol for 10min and dried for standby.
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| US4019900A (en) * | 1976-04-01 | 1977-04-26 | Olin Corporation | High strength oxidation resistant nickel base alloys |
| US5843244A (en) * | 1996-06-13 | 1998-12-01 | Nitinol Devices And Components | Shape memory alloy treatment |
| US20140373979A1 (en) * | 2011-12-15 | 2014-12-25 | National Institute For Material Science | Nickel-based heat-resistant superalloy |
| KR20150081375A (en) * | 2013-11-27 | 2015-07-14 | 창원대학교 산학협력단 | Method of heat treatment of heat-resistant alloy for excellent resistance to intergranular crack and heat-resistant alloy the same |
| CN104630597B (en) * | 2015-01-27 | 2018-02-02 | 宝钢特钢有限公司 | A kind of iron nickel and chromium high temperature alloy and its manufacture method |
| CN104878248B (en) * | 2015-03-12 | 2017-12-01 | 江苏新华合金电器有限公司 | High temperature alloy 625H and its manufacturing process |
| US10280498B2 (en) * | 2016-10-12 | 2019-05-07 | Crs Holdings, Inc. | High temperature, damage tolerant superalloy, an article of manufacture made from the alloy, and process for making the alloy |
| CN106756253B (en) * | 2016-12-30 | 2019-02-26 | 江苏鑫信润科技有限公司 | Brush seal high-performance high-temperature nickel-base alloy brush filament material |
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