CN113969380A - Manufacturing method of nuclear-grade nickel-based alloy high-performance bar, bar and application - Google Patents
Manufacturing method of nuclear-grade nickel-based alloy high-performance bar, bar and application Download PDFInfo
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- CN113969380A CN113969380A CN202010718980.4A CN202010718980A CN113969380A CN 113969380 A CN113969380 A CN 113969380A CN 202010718980 A CN202010718980 A CN 202010718980A CN 113969380 A CN113969380 A CN 113969380A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F22—STEAM GENERATION
- F22B—METHODS OF STEAM GENERATION; STEAM BOILERS
- F22B1/00—Methods of steam generation characterised by form of heating method
- F22B1/02—Methods of steam generation characterised by form of heating method by exploitation of the heat content of hot heat carriers
- F22B1/04—Methods of steam generation characterised by form of heating method by exploitation of the heat content of hot heat carriers the heat carrier being hot slag, hot residues, or heated blocks, e.g. iron blocks
Abstract
The invention discloses a method for manufacturing a nuclear-grade nickel-based alloy high-performance bar, which comprises the following steps: graded high temperature diffusion annealing: high-temperature diffusion is carried out in two stages; the forging adopts a composite forging method of quick forging and precision forging; adopting rapid forging cogging, controlling pass deformation amount to be 40-60% and forging temperature to be 1200-1230 ℃; forging by adopting a precision forging rapid forging method, controlling the pass deformation by 30-40%, gradually forging to obtain a finished bar, and rapidly cooling after the final forging temperature is 1000-1050 ℃; performing heat treatment on the finished bar, wherein the heat treatment temperature is 1140-: dx (0.25-0.35) min/mm, followed by rapid cooling. Also disclosed are bars, and uses of the bars. The invention effectively improves the high-temperature performance, especially the long-term durability, of the UNS N06625 alloy bar by optimizing and adjusting the proportion of C and Ti elements and simultaneously adopting a graded high-temperature diffusion, quick forging and finish forging composite forging method and the heat treatment of the finished bar.
Description
Technical Field
The invention belongs to the technical field of nickel-based alloy, and particularly relates to a method for manufacturing a nickel-based alloy bar for nuclear-grade high-temperature long-time use.
Background
Nuclear power is advanced clean energy, is an important component of the national energy strategy, and is one of the most important measures for realizing the national energy-saving and emission-reducing targets. The modular high-temperature gas cooled reactor nuclear power station has the characteristics of high safety, simple system, high power generation efficiency, wide application, economic competitiveness and the like, and is one of the fourth generation advanced nuclear reactor types required by the future energy market.
The UNS N06625 nickel-based alloy is a Ni-Cr-Mo solid solution strengthening type nickel-based corrosion-resistant alloy with high Mo content, has good comprehensive performance, and is widely applied to the field of petrochemical industry. The alloy contains high Cr and Ni elements, high Mo and Nb elements and high alloying degree, so that the steel ingot is easy to segregate during solidification, has high deformation resistance in processing and is easy to crack. The traditional UNS N06625 alloy bar is mainly applied to the traditional fields of petrochemical industry and the like, the high-temperature strength and the high-temperature long-term endurance strength of the material are not generally required in the industry, and the bar meeting the requirements can be produced by adopting a conventional forging process.
However, the temperature of helium at the inlet of a steam generator in a high-temperature gas-cooled reactor nuclear power station is up to 750 ℃, so that the long-term working temperature of parts in a steam generator inlet chamber and a heat exchange assembly also reaches 750 ℃, the manufacturing of the parts puts higher requirements on the room temperature performance, 750 ℃ instantaneous performance and 750 ℃ long-term durability of materials compared with the traditional application field, and the performance of bars produced by adopting a conventional forging process cannot meet the harsh requirements of the high-temperature gas-cooled reactor steam generator.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide a method for manufacturing a high-performance bar suitable for manufacturing a high-temperature gas-cooled reactor steam generator.
The technical scheme of the invention is that the manufacturing method of the nuclear-grade nickel-based alloy high-performance bar comprises the following steps of high-temperature diffusion annealing and forging:
a. graded high temperature diffusion annealing: first-stage high-temperature diffusion temperature: 1110 ℃ -1130 ℃, heat preservation time: d is multiplied by (0.03-0.05) h/mm, D is the diameter of the steel ingot, and the unit is mm; then directly heating to the second stage at 1200-1250 ℃, and keeping the temperature for: d is multiplied by (0.08-0.10) h/mm, D is the diameter of the steel ingot, and the unit is mm;
b. the forging adopts a composite forging method of quick forging and precision forging; firstly, adopting rapid forging cogging, controlling pass deformation amount to be 40-60% and forging temperature to be 1200-1230 ℃; secondly, forging by adopting a precision forging rapid forging method, controlling the pass deformation to be 30-40%, gradually forging the finished bar material, and rapidly cooling by water after the final forging temperature is 1000-1050 ℃;
c. performing heat treatment on the finished bar, wherein the heat treatment temperature is 1140-: d x (0.25-0.35) min/mm, D being the diameter of the bar in mm, followed by rapid water cooling.
And carrying out long-time homogenization treatment on the cast ingot by adopting a graded high-temperature diffusion method, and eliminating intermetallic laves phases of low-temperature eutectic in the steel ingot solidification process and redistribution of Mo and Nb easily-segregated elements, so that the structure and the components of the forged rod are more uniform.
The above contents are mutually restricted, and are all indispensable, and are an organic whole. Any one of the bars cannot reach the comprehensive performance index due to unreasonable design.
According to the method for manufacturing the high-performance rod of the nuclear-grade nickel-based alloy, the high-temperature diffusion temperature of the first stage in the step a is preferably 1115-1125 ℃, and the heat preservation time is preferably Dx (0.04-0.05) h/mm. More preferably, the first-stage high-temperature diffusion temperature is 1119-.
According to the manufacturing method of the nuclear grade nickel base alloy high-performance bar, the temperature of the second-stage high-temperature diffusion in the step a is preferably 1225-.
According to the manufacturing method of the nuclear grade nickel base alloy high-performance bar, the cooling mode in the step b is preferably water cooling.
According to the manufacturing method of the nuclear grade nickel base alloy high-performance bar, the cooling mode in the step c is preferably water cooling.
The invention also provides a nuclear grade nickel-based alloy high-performance bar prepared by the method,
the weight percentage of the chemical components is as follows: 0.03-0.04%, P is less than or equal to 0.010%, S is less than or equal to 0.010%, Cr: 20.0-23.0%, Ni is more than or equal to 58.0%, Mo: 8.5-9.5%, Nb: 3.3-3.8%, Al: 0.35-0.50%, and the balance of inevitable impurities; and Ti/C is 9.0-13.0.
On the basis of the distribution ratio of the chemical composition of the existing UNS N06625 alloy, the proportion of C and Ti elements is adjusted, the content of C element is reduced to 0.03-0.04%, and Ti/C is 9.0-13.0. Forming the optimized component proportion.
The high-performance bar of the nuclear-grade nickel-based alloy has the Ti content of 0.27-0.52 percent. More preferably, the Ti content is 0.36% to 0.52%.
According to the high-performance bar of the nuclear-grade nickel-based alloy, preferably, the bar has the following properties: the tensile strength at the high temperature of 750 ℃ is more than or equal to 530MPa, the yield strength is more than or equal to 250MPa, and the elongation is more than or equal to 90 percent.
According to the high-performance bar of the nuclear-grade nickel-based alloy, the bar is further extrapolated by 10 at 750 DEG C5The hour endurance strength is more than or equal to 90 MPa. The impact energy at room temperature of 750 ℃ aged for 5000 hours is more than or equal to 45J.
The invention also discloses application of the nuclear-grade nickel-based alloy high-performance bar in a high-temperature gas cooled reactor nuclear power station component. The temperature of helium at the inlet of a steam generator in a high-temperature gas cooled reactor nuclear power station is up to 750 ℃, so that the long-term working temperature of parts in a steam generator inlet chamber and a heat exchange assembly is up to 750 ℃, the manufacturing of the parts has higher requirements on the room temperature performance, 750 ℃ instantaneous performance and 750 ℃ long-term lasting performance of materials, and the bar disclosed by the invention can meet the requirements.
The technical principle of the invention is as follows:
1. the long-term service temperature of the high-temperature gas-cooled reactor is 750 ℃, which is in the sensitization temperature range of UNS N06625. When the temperature is kept for a long time, a large amount of secondary carbides are precipitated from grain boundaries, and the carbides cause embrittlement of the grain boundaries, so that the service life of the alloy is shortened. The Ti element in the alloy has strong affinity with the C, more stable high-temperature primary TiC is formed in the structure by regulating the proportion of the C element to the Ti element, and the precipitation of the C element in a grain boundary is reduced, so that the precipitation of secondary carbide when the alloy is used at the high temperature of 750 ℃ for a long time is avoided, the binding force of the grain boundary is improved, and the lasting life of the alloy is prolonged.
2. 625 alloy contains a large amount of Nb and Mo easy segregation elements, and during solidification, a brittle intermetallic laves phase of 1100-1120 ℃ low-temperature eutectic can be formed in an as-cast structure, and meanwhile, micro segregation of Nb and Mo can be formed. On one hand, the intermetallic laves phase of the low-temperature eutectic can be partially dissolved in the subsequent high-temperature forging, and can be solidified into a crack source after the forging, so that the alloy can be broken when being used at high temperature for a long time, and the lasting life of the alloy is shortened. On the other hand, micro-segregation of Nb and Mo causes structural unevenness, thereby reducing the alloy life. Therefore, there is a need to improve the longevity of alloys by eliminating these brittle intermetallic laves phases and microsegregation by reasonable high temperature diffusion methods.
3. As is known, the size and uniformity of grain size have important influence on the high-temperature endurance life of the alloy, and the grain size is generally considered to be within the range of 3-5 grade, so that the short-time strength of the alloy can be ensured, and the alloy has better endurance life. Under the condition of a certain component proportion, the main factors influencing the grain size of the alloy are deformation, temperature and a final heat treatment system. Based on this, controlling the amount of deformation, temperature and final heat treatment regime in bar manufacturing is critical to obtaining a reasonable grain size structure.
The invention has the following beneficial effects:
on the basis of the unchanged chemical composition system of the existing UNS N06625 alloy, the invention effectively improves the UNS N06625 alloy by optimizing and adjusting the proportioning of C and Ti elements, simultaneously adopting a graded high-temperature diffusion, quick forging and finish forging composite forging method and heat treatment of finished bars and four organically integrated matching processesThe high-temperature performance, especially the long-term durability, of the gold bar meets the following requirements: the tensile strength at high temperature of 750 ℃ is more than or equal to 530MPa, the yield strength is more than or equal to 250MPa, the elongation is more than or equal to 90 percent, and particularly the extrapolation rate is 10 percent at 750 DEG C5The hour endurance strength is more than or equal to 90MPa, and the impact energy at room temperature of long-term aging (5000 hours) at 750 ℃ is more than or equal to 45J.
The use of the alloy in a high-temperature long-term environment at 750 ℃ is widened, and the alloy is particularly suitable for manufacturing high-temperature components of a high-temperature gas cooled reactor steam generator.
Drawings
FIG. 1 is a comparison of room temperature impact toughness after extended use at elevated temperatures for pre-and post-optimized bars of the present invention.
Detailed Description
Example 1
The method for manufacturing the nuclear-grade nickel-based alloy high-performance bar comprises the following steps:
step 1: adopting a vacuum induction and electroslag remelting mode to smelt steel ingots, wherein the components meet the optimized components, and the weight percentage of the chemical components is C: 0.03%, P is less than or equal to 0.010%, S is less than or equal to 0.010%, Cr: 20.0-23.0%, Ni is more than or equal to 58.0%, Mo: 8.5-9.5%, Nb: 3.3-3.8%, Al: 0.35 to 0.50%, 9.0% Ti/C, and the balance unavoidable impurities. The diameter of the steel ingot is 510 mm.
Step 2: and carrying out long-time homogenization treatment on the cast ingot by adopting a graded high-temperature diffusion method. The grading high-temperature diffusion process comprises the following steps: first-stage high-temperature diffusion temperature: the temperature is 1120 ℃, and the heat preservation time is 25.5 h. Then directly heating to the second stage at 1230 ℃, and keeping the temperature for 51 h.
And step 3: and (3) performing composite forging of quick forging and finish forging. Heating the steel ingot after high-temperature diffusion to 1200 ℃ in a heating furnace, forging the steel ingot to a 390mm octagonal shape on a quick forging press once, then heating the steel ingot to 1200 ℃ in the furnace, forging the steel ingot on a finish forging machine twice to a finished bar with the diameter of 240mm, wherein the finish forging temperature is 1000 ℃, and then rapidly cooling the steel ingot by water.
And 4, step 4: carrying out heat treatment on the finished bar, wherein the heat treatment temperature is 1140 ℃, and the heat preservation time is as follows: 84min, then rapidly water-cooling.
And (3) performing 750 ℃ high-temperature mechanical property test on the finished forged rod after heat treatment: tensile strength: 560MPa, yield strength: 260MPa, elongation: 98%, extrapolated 105 hour endurance at 750 ℃: 95MPa, long-term aging (5000 hours) at 750 ℃ and impact energy at room temperature: 58J.
Example 2
The method for manufacturing the nuclear-grade nickel-based alloy high-performance bar comprises the following steps:
step 1: adopting a vacuum induction and electroslag remelting mode to smelt steel ingots, wherein the components meet the optimized components, and the weight percentage of the chemical components is C: 0.04%, P is less than or equal to 0.010%, S is less than or equal to 0.010%, Cr: 20.0-23.0%, Ni is more than or equal to 58.0%, Mo: 8.5-9.5%, Nb: 3.3-3.8%, Al: 0.35 to 0.50%, 13.0% Ti/C, and the balance unavoidable impurities. The diameter of the steel ingot is 510 mm.
Step 2: and carrying out long-time homogenization treatment on the cast ingot by adopting a graded high-temperature diffusion method. The grading high-temperature diffusion process comprises the following steps: first-stage high-temperature diffusion temperature: the temperature is 1120 ℃, and the heat preservation time is 25.5 h. Then directly heating to the second stage at 1230 ℃, and keeping the temperature for 51 h.
And step 3: and (3) performing composite forging of quick forging and finish forging. Heating the steel ingot after high-temperature diffusion to 1210 ℃ in a heating furnace, forging the steel ingot to a 250mm octagonal shape in one step on a quick forging press, then heating the steel ingot to 1210 ℃ in the furnace, forging the steel ingot in three steps on a finish forging machine to obtain a finished bar with the diameter of 110mm, wherein the finish forging temperature is 1050 ℃, and then rapidly cooling the steel ingot by water.
And 4, step 4: carrying out heat treatment on the finished bar, wherein the heat treatment temperature is 1160 ℃, and the heat preservation time is as follows: 27.5min, then rapidly water-cooled.
And (3) performing 750 ℃ high-temperature mechanical property test on the finished forged rod after heat treatment: tensile strength: 565MPa, yield strength: 265MPa, elongation: 98%, extrapolated 105 hour endurance at 750 ℃: 94MPa, long-term aging (5000 hours) at 750 ℃ and impact energy at room temperature: 60J.
Example 3
The method for manufacturing the nuclear-grade nickel-based alloy high-performance bar comprises the following steps:
step 1: adopting a vacuum induction and electroslag remelting mode to smelt steel ingots, wherein the components meet the optimized components, and the weight percentage of the chemical components is C: 0.035%, P is less than or equal to 0.010%, S is less than or equal to 0.010%, Cr: 20.0-23.0%, Ni is more than or equal to 58.0%, Mo: 8.5-9.5%, Nb: 3.3-3.8%, Al: 0.35 to 0.50%, Ti/C of 11.0, and the balance being unavoidable impurities. The diameter of the steel ingot is 660 mm.
Step 2: and carrying out long-time homogenization treatment on the cast ingot by adopting a graded high-temperature diffusion method. The grading high-temperature diffusion process comprises the following steps: first-stage high-temperature diffusion temperature: 1120 ℃ and the heat preservation time is 33 h. Then directly heating to the second stage at 1230 ℃, and keeping the temperature for 66 h.
And step 3: and (3) performing composite forging of quick forging and finish forging. Heating the steel ingot after high-temperature diffusion to 1230 ℃ in a heating furnace, forging to 480mm octagonal in one step on a quick forging press, then heating to 1200 ℃ in the furnace, forging for the second time on a finish forging machine, forging finished bars with the diameter of 300mm in 2 passes, and then rapidly cooling by water.
And 4, step 4: carrying out heat treatment on the finished bar, wherein the heat treatment temperature is 1150 ℃, and the heat preservation time is as follows: 90min, then rapidly water-cooling.
And (3) performing 750 ℃ high-temperature mechanical property test on the finished forged rod after heat treatment: tensile strength: 570MPa, yield strength: 270MPa, elongation: 95%, extrapolated 105 hours permanent strength at 750 ℃: impact work at room temperature of 96MPa and 750 ℃ long-term aging (5000 hours): 61.
the invention effectively improves the high-temperature performance, especially the long-term durability, of the UNS N06625 alloy bar by optimizing and adjusting the proportion of C and Ti elements and simultaneously adopting a graded high-temperature diffusion, quick forging and finish forging composite forging method and the heat treatment of the finished bar.
Claims (10)
1. A manufacturing method of a nuclear-grade nickel-based alloy high-performance bar comprises high-temperature diffusion annealing and forging, and is characterized in that: the method comprises the following steps:
a. graded high temperature diffusion annealing: first-stage high-temperature diffusion temperature: 1110 ℃ -1130 ℃, heat preservation time: d is multiplied by (0.03-0.05) h/mm, and D is the diameter of the steel ingot; then directly heating to the second stage at 1200-1250 ℃, and keeping the temperature for: d is multiplied by (0.08-0.10) h/mm, and D is the diameter of the steel ingot;
b. the forging adopts a composite forging method of quick forging and precision forging; firstly, adopting rapid forging cogging, controlling pass deformation amount to be 40-60% and forging temperature to be 1200-1230 ℃; secondly, forging by adopting a precision forging rapid forging method, controlling the pass deformation to be 30-40%, gradually forging the finished bar material, and rapidly cooling by water after the final forging temperature is 1000-1050 ℃;
c. performing heat treatment on the finished bar, wherein the heat treatment temperature is 1140-: d x (0.25-0.35) min/mm, D being the diameter of the bar, followed by rapid water cooling.
2. The method for manufacturing the high-performance bar of the nuclear-grade nickel-based alloy according to claim 1, wherein the method comprises the following steps: the high-temperature diffusion temperature of the first stage in the step a is 1115-1125 ℃, and the heat preservation time is Dx (0.04-0.05) h/mm.
3. The method for manufacturing the high-performance bar of the nuclear-grade nickel-based alloy according to claim 1, wherein the method comprises the following steps: the second-stage high-temperature diffusion temperature in the step a is 1225-1235 ℃, and the heat preservation time Dx (0.09-0.10) h/mm.
4. The method for manufacturing the high-performance bar of the nuclear-grade nickel-based alloy according to claim 1, wherein the method comprises the following steps: and the cooling mode of the step b is water cooling.
5. The method for manufacturing the high-performance bar of the nuclear-grade nickel-based alloy according to claim 1, wherein the method comprises the following steps: and c, cooling by water.
6. The nuclear grade nickel-based alloy high-performance bar prepared by the method of claim 1, which is characterized in that:
the weight percentage of the chemical components is as follows: 0.03-0.04%, P is less than or equal to 0.010%, S is less than or equal to 0.010%, Cr: 20.0-23.0%, Ni is more than or equal to 58.0%, Mo: 8.5-9.5%, Nb: 3.3-3.8%, Al: 0.35-0.50%, and the balance of inevitable impurities; and Ti/C is 9.0-13.0.
7. The nuclear grade nickel-based alloy high-performance bar according to claim 6, wherein: the properties of the bar are as follows: the tensile strength at the high temperature of 750 ℃ is more than or equal to 530MPa, the yield strength is more than or equal to 250MPa, and the elongation is more than or equal to 90 percent.
8. The nuclear grade nickel-based alloy high-performance bar according to claim 7, wherein: the bars were extrapolated 10 at 750 ℃5The hour endurance strength is more than or equal to 90 MPa.
9. The nuclear grade nickel-based alloy high-performance bar according to claim 7, wherein: the impact energy at room temperature of 750 ℃ aged for 5000 hours is more than or equal to 45J.
10. Use of the nuclear grade nickel base alloy high performance rod of claim 6 in a high temperature gas cooled reactor nuclear power plant component.
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