CN115323153B - Heat treatment method of superalloy seamless tube, superalloy heat treated seamless tube and application of superalloy heat treated seamless tube - Google Patents

Heat treatment method of superalloy seamless tube, superalloy heat treated seamless tube and application of superalloy heat treated seamless tube Download PDF

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CN115323153B
CN115323153B CN202210962683.3A CN202210962683A CN115323153B CN 115323153 B CN115323153 B CN 115323153B CN 202210962683 A CN202210962683 A CN 202210962683A CN 115323153 B CN115323153 B CN 115323153B
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temperature
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superalloy
heat
heat preservation
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CN115323153A (en
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陈乐利
尹添威
罗锐
程晓农
郑琦
刘天
丁恒楠
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Jiangsu University
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Jiangsu University
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/08Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/76Adjusting the composition of the atmosphere
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21DNUCLEAR POWER PLANT
    • G21D1/00Details of nuclear power plant
    • G21D1/02Arrangements of auxiliary equipment
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C30/00Alloys containing less than 50% by weight of each constituent
    • C22C30/02Alloys containing less than 50% by weight of each constituent containing copper
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00Energy generation of nuclear origin
    • Y02E30/30Nuclear fission reactors

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Heat Treatment Of Articles (AREA)

Abstract

The invention provides a heat treatment method of a superalloy seamless pipe, the superalloy heat treatment seamless pipe and application thereof, and relates to the technical field of metal materials. The heat treatment method can ensure that the high-temperature alloy seamless pipe has good structure and mechanical property, and the product has excellent tensile strength and elongation under the conditions of room temperature and high temperature. The results of the examples show that the seamless pipe obtained by the heat treatment method provided by the invention has the room temperature tensile strength of 865-877 MPa and the room temperature elongation of 30.1-33.2%; the high temperature (650 ℃) tensile strength is 674-688 MPa, the high temperature elongation is 13.2-13.6%, and the grain grade of the structure is between 4-8 stages.

Description

Heat treatment method of superalloy seamless tube, superalloy heat treated seamless tube and application of superalloy heat treated seamless tube
Technical Field
The invention relates to the technical field of metal materials, in particular to a heat treatment method of a superalloy seamless tube, the superalloy heat treatment seamless tube and application thereof.
Background
Nuclear power has been highly valued as a safe, clean, low-carbon and efficient energy source. Currently, the global nuclear power plant under construction has gradually transitioned to the third generation nuclear power technology, and the safer fourth generation nuclear power technology has become the subject of important research by nuclear power researchers in the coming years. The high-temperature gas cooled reactor in the fourth generation nuclear power technology has the advantages that the inherent safety attribute is adopted, the off-site emergency safety is not needed, and the like, so that the nuclear power center reactor cannot be destroyed under any accident condition, and the radioactive substance leakage accident can be avoided. The steam generator of the core component of the high-temperature gas cooled reactor mainly comprises 19 spiral tube bundle assemblies, each assembly comprises five layers of 35 multi-head spiral tubes, and the longest tube length can reach 60m. The fourth generation nuclear energy of the high temperature gas cooled reactor steam generator works under the service condition of high temperature, high pressure and high radiation for a long time by using a heat exchange tube, which puts an extremely high requirement on the organization performance of the fourth generation nuclear energy; simultaneously, as the three elements of the inner diameter, the wall thickness and the outer diameter are required to be controlled simultaneously on the basis of the size requirement, the heat treatment process has extremely high requirements.
Disclosure of Invention
The invention aims to provide a heat treatment method of a high-temperature alloy seamless pipe, the high-temperature alloy heat treatment seamless pipe and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a heat treatment method of a superalloy seamless tube, which comprises the following steps of sequentially carrying out heat treatment on a straight tube and heat treatment on a coil;
the heat treatment of the straight pipe comprises the following steps: heating the high-temperature alloy seamless pipe to a first temperature in a reducing atmosphere, performing first heat preservation, and air-cooling to room temperature; then heating to a second temperature, carrying out second heat preservation, and cooling to room temperature along with the furnace; the first temperature is 970-990 ℃, and the first heat preservation time is 35-45 min; the second temperature is 730-750 ℃, and the second heat preservation time is 40-50 min;
the coil heat treatment includes: heating to a third temperature under vacuum condition, carrying out third heat preservation, and then cooling to 560-580 ℃ in a furnace; then cooling to a fourth temperature in oxygen atmosphere, carrying out furnace cooling to not more than 200 ℃ after fourth heat preservation, and discharging and air cooling; the third temperature is 670-690 ℃, and the third heat preservation time is 30-40 min; the fourth temperature is 540-560 ℃, and the fourth heat preservation time is 40-50 min.
Preferably, the temperature rising rate from the room temperature to the first temperature is 8-10 ℃/s.
Preferably, the first incubation is performed in a mixed atmosphere of hydrogen and nitrogen; the flow ratio of the hydrogen to the nitrogen is 3-4:6.
Preferably, the temperature rise rate from the room temperature to the second temperature is 8-10 ℃/s.
Preferably, the second incubation is performed in a mixed atmosphere of hydrogen and nitrogen; the flow ratio of the hydrogen to the nitrogen is 4-5:5.
Preferably, the heat treatment of the straight pipe further comprises coil pipe forming, and the coil pipe is subjected to coil pipe heat treatment.
Preferably, the temperature rise rate from the room temperature to the third temperature is 8 to 10 ℃/s.
Preferably, the pressure of the fourth heat preservation is 0.01-0.03 MPa.
The invention provides the superalloy heat treatment seamless pipe prepared by the heat treatment method.
The invention provides application of the superalloy heat treatment seamless tube in a nuclear reaction unit.
The invention provides a heat treatment method of a superalloy seamless tube, which comprises the following steps of sequentially carrying out heat treatment on a straight tube and heat treatment on a coil; the heat treatment of the straight pipe comprises the following steps: heating the high-temperature alloy seamless pipe to a first temperature in a reducing atmosphere, performing first heat preservation, and air-cooling to room temperature; then heating to a second temperature, carrying out second heat preservation, and cooling to room temperature along with the furnace; the first temperature is 970-990 ℃, and the first heat preservation time is 35-45 min; the second temperature is 730-750 ℃, and the second heat preservation time is 40-50 min; the coil heat treatment includes: heating to a third temperature under vacuum condition, carrying out third heat preservation, and then cooling to 560-580 ℃ in a furnace; then cooling to a fourth temperature in oxygen atmosphere, carrying out furnace cooling to not more than 200 ℃ after fourth heat preservation, and discharging and air cooling; the third temperature is 670-690 ℃, and the third heat preservation time is 30-40 min; the fourth temperature is 540-560 ℃, and the fourth heat preservation time is 40-50 min.
The heat treatment method can effectively refine grains, regulate and control alloy performance, reduce internal stress and microcrack generation, smoothly implement a coil pipe process through heat treatment, ensure that the high-temperature alloy seamless pipe has good structure and mechanical property, and ensure that the product has excellent tensile strength and elongation under room temperature conditions and high temperature conditions. The results of the examples show that the seamless pipe obtained by the heat treatment method provided by the invention has the room temperature tensile strength of 865-877 MPa and the room temperature elongation of 30.1-33.2%; the high temperature (650 ℃) tensile strength is 674-688 MPa, the high temperature elongation is 13.2-13.6%, and the grain grade of the structure is between 4-8 stages.
Drawings
FIG. 1 is an EBSD image of a superalloy heat treated seamless tube obtained by the heat treatment of example 1;
FIG. 2 is an EBSD image of a superalloy heat treated seamless tube obtained by the heat treatment of example 2;
FIG. 3 is an EBSD image of a superalloy heat treated seamless tube obtained by the heat treatment of comparative example 1;
FIG. 4 is an EBSD image of a superalloy heat treated seamless tube obtained by the heat treatment of comparative example 2.
Detailed Description
The invention provides a heat treatment method of a superalloy seamless tube, which comprises the following steps of sequentially carrying out heat treatment on a straight tube and heat treatment on a coil;
the heat treatment of the straight pipe comprises the following steps: heating the high-temperature alloy seamless pipe to a first temperature in a reducing atmosphere, performing first heat preservation, and air-cooling to room temperature; then heating to a second temperature, carrying out second heat preservation, and cooling to room temperature along with the furnace; the first temperature is 970-990 ℃, and the first heat preservation time is 35-45 min; the second temperature is 730-750 ℃, and the second heat preservation time is 40-50 min;
the coil heat treatment includes: heating to a third temperature under vacuum condition, carrying out third heat preservation, and then cooling to 560-580 ℃ in a furnace; then cooling to a fourth temperature in oxygen atmosphere, carrying out furnace cooling to not more than 200 ℃ after fourth heat preservation, and discharging and air cooling; the third temperature is 670-690 ℃, and the third heat preservation time is 30-40 min; the fourth temperature is 540-560 ℃, and the fourth heat preservation time is 40-50 min.
In the invention, the superalloy seamless tube is a straight tube. In the present invention, the superalloy seamless tube is preferably made of a nickel-based superalloy. In the invention, the wall thickness unevenness of the superalloy seamless tube is preferably less than or equal to 80% of the wall thickness allowable deviation; the surface of the superalloy seamless tube is preferably free of buffeting, oil stains and burrs and foreign matters at the tube end.
In the present invention, the straight pipe heat treatment includes: heating the high-temperature alloy seamless pipe to a first temperature in a reducing atmosphere, performing first heat preservation, and air-cooling to room temperature; then heating to a second temperature, carrying out second heat preservation, and cooling to room temperature along with the furnace; the first temperature is 970-990 ℃, and the first heat preservation time is 35-45 min; the second temperature is 730-750 ℃, and the second heat preservation time is 40-50 min. In the present invention, the temperature rise rate from the room temperature to the first temperature is preferably 8 to 10 ℃/s, more preferably 9 ℃/s. In the present invention, the first temperature is preferably 980 ℃; the time of the first incubation is preferably 40min. In the present invention, the first heat preservation is preferably performed in a mixed atmosphere of hydrogen and nitrogen; the flow ratio of the hydrogen to the nitrogen is preferably 3-4:6, more preferably 1:2. According to the invention, the grains can be refined and the toughness of the material can be improved by carrying out the first heat preservation under the atmosphere.
In the present invention, the temperature rise rate from the room temperature to the second temperature is preferably 8 to 10 ℃/s, more preferably 10 ℃/s. In the present invention, the second temperature is preferably 740 ℃; the second incubation time is preferably 45 minutes. In the present invention, the second incubation is preferably performed in a mixed atmosphere of hydrogen and nitrogen; the flow ratio of the hydrogen to the nitrogen is preferably 4 to 5:5, more preferably 4:5. The invention can eliminate the internal stress of the material and reduce the brittleness by carrying out the second heat preservation under the atmosphere.
In the present invention, the heat treatment of the straight pipe preferably further comprises coil forming, and the coil is subjected to heat treatment. In the invention, the coil pipe forming method is preferably flexible three-dimensional synchronous bending. In the present invention, the surface of the coil is preferably defect-free, scale-free, the inner surface allowing slight discoloration; the wall thickness non-uniformity of the coil is preferably 80% or less of the wall thickness tolerance. In the specific embodiment of the invention, a special ultra-long spiral tube forming machine is used for forming the multi-head spiral tube so as to obtain the spiral tube which meets the size requirement of the spiral tube for the high-temperature gas cooled reactor steam generator.
In the present invention, the coil heat treatment includes: heating to a third temperature under vacuum condition, carrying out third heat preservation, and then cooling to 560-580 ℃ in a furnace; then cooling to a fourth temperature in oxygen atmosphere, carrying out furnace cooling to not more than 200 ℃ after fourth heat preservation, and discharging and air cooling; the third temperature is 670-690 ℃, and the third heat preservation time is 30-40 min; the fourth temperature is 540-560 ℃, and the fourth heat preservation time is 40-50 min. In the present invention, the vacuum degree of the vacuum condition is preferably 5×10 or less -3 Pa, more preferably 4X 10 -3 Pa. In the present invention, the temperature rise rate from the room temperature to the third temperature is preferably 8 to 10 ℃/s, more preferably 10 ℃. In the present invention, the third temperature is preferably 680 ℃; the time of the third incubation is preferably 30min. In the present invention, the cooling mode from the third temperature to the fourth temperature is preferably furnace cooling. In the present invention, the fourth temperature is preferably 550 ℃; the fourth incubation time is preferably 45min. In the present invention, the pressure of the fourth heat preservation is preferably 0.01 to 0.03MPa, more preferably 0.01MPa.
The invention provides the superalloy heat treatment seamless pipe prepared by the heat treatment method. In the specific embodiment of the invention, the room temperature tensile strength of the superalloy heat-treated seamless pipe is 866.7-872.6 MPa, and the room temperature elongation is 30.7-32.1%; the high temperature (650 ℃) tensile strength is 676.7-684.7 MPa, the high temperature elongation is 13.2-13.5%, and the grain grade of the structure is between 4-6 stages.
The invention also provides application of the superalloy heat treatment seamless pipe in a nuclear reaction unit, preferably a high-temperature gas cooled reactor steam generator, and more preferably a fourth-generation nuclear energy high-temperature gas cooled reactor steam generator.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) Heat treatment of a straight pipe:
fixing a seamless straight pipe of a nickel-based superalloy (concrete components of the alloy comprise, by mass, 22% of Cr, 42% of Fe, 34% of Ni, 0.80% of Mn, 0.30% of Al, 0.30% of Ti, 0.45% of Cu, 0.06% of C and the balance of unavoidable impurities) on a fixing frame, and conveying a finished pipe into an industrial heat treatment furnace after the fixing is completed;
introducing hydrogen and nitrogen, wherein H 2 Is 10m 3 /h,N 2 Is 20m 3 Heating to 980 ℃ at a heating rate of 10 ℃/s, keeping the temperature for 35min, and cooling to room temperature after the heat preservation is finished;
adjusting the flow rate of hydrogen and nitrogen, H 2 20m of 3 /h,N 2 25m of 3 And/h, heating to 740 ℃ at a heating rate of 10 ℃/s, keeping the temperature for 40min, and then cooling to room temperature along with the furnace.
(2) Coil heat treatment
The pipe obtained after the heat treatment of the straight pipe is subjected to multi-head spiral pipe forming by using a special ultra-long spiral pipe forming machine to obtain a coil pipe, the coil pipe is fixed by adopting a special fixing frame after being checked to be qualified, the geometric size and the shape of the spiral pipe are ensured to be consistent with the requirements of drawing, and the spiral pipe and the fixing frame are placed into a vacuum heat treatment furnace after the fixation is completed;
the vacuum degree in the vacuum heat treatment furnace reaches 4 multiplied by 10 -3 After Pa, the temperature is raised to 680 ℃ at a heating rate of 10 ℃/s,the heat preservation time is 30min, and O is introduced into the furnace after the heat preservation is finished and the furnace is cooled to 570 DEG C 2 Closing an oxygen valve when the oxygen content is 0.01MPa, cooling to 550 ℃ in a furnace cooling mode, preserving heat for 45min, and discharging and air cooling when the furnace cooling is not more than 200 ℃.
FIG. 1 is an EBSD image of a superalloy heat-treated seamless tube obtained by the heat treatment of example 1. As can be seen from fig. 1, the alloy grains after heat treatment have uniform size, and a large number of twin crystals are distributed in the grains, so that a good alloy microstructure is shown.
Example 2
(1) Heat treatment of a straight pipe:
fixing a seamless straight pipe of a nickel-based superalloy (concrete components of the alloy comprise, by mass, 22% of Cr, 42% of Fe, 34% of Ni, 0.80% of Mn, 0.30% of Al, 0.30% of Ti, 0.45% of Cu, 0.06% of C and the balance of unavoidable impurities) on a fixing frame, and conveying a finished pipe into an industrial heat treatment furnace after the fixing is completed;
introducing hydrogen and nitrogen, wherein H 2 Is 10m 3 /h,N 2 Is 20m 3 Heating to 970 ℃ at a heating rate of 10 ℃/s, keeping the temperature for 35min, and cooling to room temperature after the heat preservation is finished;
adjusting the flow rate of hydrogen and nitrogen, H 2 20m of 3 /h,N 2 25m of 3 And/h, heating to 730 ℃ at a heating rate of 10 ℃/s, keeping the temperature for 40min, and then cooling to room temperature along with the furnace.
(2) Coil heat treatment
The pipe obtained after the heat treatment of the straight pipe is subjected to multi-head spiral pipe forming by using a special ultra-long spiral pipe forming machine to obtain a coil pipe, the coil pipe is fixed by adopting a special fixing frame after being checked to be qualified, the geometric size and the shape of the spiral pipe are ensured to be consistent with the requirements of drawing, and the spiral pipe and the fixing frame are placed into a vacuum heat treatment furnace after the fixation is completed;
the vacuum degree in the vacuum heat treatment furnace reaches 4 multiplied by 10 -3 After Pa, heating to 670 ℃ at a heating rate of 10 ℃/s, keeping the temperature for 30min, cooling the furnace to 560 ℃ after the heat preservation is finished, and introducing O into the furnace 2 Closing an oxygen valve when the oxygen content is 0.01MPa, cooling to 540 ℃ in a furnace cooling mode, preserving heat for 40min, and discharging and air cooling when the furnace cooling is not more than 200 ℃.
FIG. 2 is an EBSD image of a superalloy heat treated seamless tube obtained by the heat treatment of example 2. As can be seen from fig. 2, the alloy grains after heat treatment have uniform size, and a large number of twin crystals are distributed in the grains, so that a good alloy microstructure is shown.
Comparative example 1
(1) Heat treatment of a straight pipe:
fixing a seamless straight pipe of a nickel-based superalloy (concrete components of the alloy comprise, by mass, 22% of Cr, 42% of Fe, 34% of Ni, 0.80% of Mn, 0.30% of Al, 0.30% of Ti, 0.45% of Cu, 0.06% of C and the balance of unavoidable impurities) on a fixing frame, and conveying a finished pipe into an industrial heat treatment furnace after the fixing is completed;
introducing hydrogen and nitrogen, wherein H 2 Is 10m 3 /h,N 2 Is 20m 3 Heating to 950 ℃ at a heating rate of 10 ℃/s, keeping the temperature for 35min, and cooling to room temperature after the heat preservation is finished;
adjusting the flow rate of hydrogen and nitrogen, H 2 20m of 3 /h,N 2 25m of 3 And/h, heating to 700 ℃ at a heating rate of 10 ℃/s, keeping the temperature for 40min, and then cooling to room temperature along with the furnace.
(2) Coil heat treatment
The pipe obtained after the heat treatment of the straight pipe is subjected to multi-head spiral pipe forming by using a special ultra-long spiral pipe forming machine to obtain a coil pipe, the coil pipe is fixed by adopting a special fixing frame after being checked to be qualified, the geometric size and the shape of the spiral pipe are ensured to be consistent with the requirements of drawing, and the spiral pipe and the fixing frame are placed into a vacuum heat treatment furnace after the fixation is completed;
the vacuum degree in the vacuum heat treatment furnace reaches 4 multiplied by 10 -3 After Pa, heating to 670 ℃ at a heating rate of 10 ℃/s, keeping the temperature for 30min, cooling to 550 ℃ after the heat preservation is finished, and introducing O into the furnace 2 Closing the oxygen valve when the oxygen content is 0.01MPa, and cooling the furnaceCooling to 500 ℃, preserving heat for 40min, and then cooling to 200 ℃ or less, discharging and air cooling.
Fig. 3 is an EBSD image of a superalloy heat-treated seamless tube obtained by the heat treatment of comparative example 1. As can be seen from fig. 3, under this heat treatment method, the alloy grain size was not uniform, and coarse grains were present, and the microstructure was significantly inferior to that of examples 1 and 2.
Comparative example 2
(1) Heat treatment of a straight pipe:
fixing a seamless straight pipe of a nickel-based superalloy (concrete components of the alloy comprise, by mass, 22% of Cr, 42% of Fe, 34% of Ni, 0.80% of Mn, 0.30% of Al, 0.30% of Ti, 0.45% of Cu, 0.06% of C and the balance of unavoidable impurities) on a fixing frame, and conveying a finished pipe into an industrial heat treatment furnace after the fixing is completed;
introducing hydrogen and nitrogen, wherein H 2 Is 8m 3 /h,N 2 Is 20m 3 Heating to 980 ℃ at a heating rate of 10 ℃/s, keeping the temperature for 35min, and cooling to room temperature after the heat preservation is finished;
adjusting the flow rate of hydrogen and nitrogen, H 2 15m of 3 /h,N 2 25m of 3 And/h, heating to 740 ℃ at a heating rate of 10 ℃/s, keeping the temperature for 40min, and then cooling to room temperature along with the furnace.
(2) Coil heat treatment
The pipe obtained after the heat treatment of the straight pipe is subjected to multi-head spiral pipe forming by using a special ultra-long spiral pipe forming machine to obtain a coil pipe, the coil pipe is fixed by adopting a special fixing frame after being checked to be qualified, the geometric size and the shape of the spiral pipe are ensured to be consistent with the requirements of drawing, and the spiral pipe and the fixing frame are placed into a vacuum heat treatment furnace after the fixation is completed;
the vacuum degree in the vacuum heat treatment furnace reaches 4 multiplied by 10 -3 After Pa, heating to 680 ℃ at a heating rate of 10 ℃/s, keeping the temperature for 30min, cooling the furnace to 570 ℃ after the heat preservation is finished, and introducing O into the furnace 2 Closing an oxygen valve when the oxygen content is 0.01MPa, cooling to 550 ℃ in a furnace cooling mode, preserving heat for 45min, and discharging and air cooling when the furnace cooling is not more than 200 ℃.
FIG. 4 is an EBSD image of a superalloy heat treated seamless tube obtained by the heat treatment of comparative example 2. As can be seen from FIG. 4, the alloy after heat treatment had uneven grain size and coarse grains were distributed in the grains, and the microstructure was significantly inferior to examples 1-2.
Test case
The properties of the spiral coil products prepared in examples and comparative examples were tested according to GB/T228-2002 method for tensile test of metallic Material at room temperature, and the results are shown in Table 1.
Table 1 comparison of the properties of examples and comparative examples
It can be seen that the heat treatment method of the invention can make the high-temperature alloy seamless pipe have good structure and mechanical properties, and the product has excellent tensile strength and elongation under the conditions of room temperature and high temperature. And the spiral coil product obtained under the condition of slightly higher temperature is better than lower temperature in the aspects of both tissue and mechanical property. The heat treatment method can effectively regulate and control the structure, optimize the alloy performance, and is particularly suitable for producing the high-temperature gas cooled reactor heat exchange seamless pipe of the nuclear power station.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (8)

1. The heat treatment method of the superalloy seamless tube is characterized by comprising the following steps of sequentially carrying out heat treatment on a straight tube and heat treatment on a coil; the superalloy seamless tube is made of nickel-based superalloy; the nickel-based superalloy comprises the following specific components in percentage by mass: 22% of Cr, 42% of Fe, 34% of Ni, 0.80% of Mn, 0.30% of Al, 0.30% of Ti, 0.45% of Cu, 0.06% of C and the balance of unavoidable impurities;
the heat treatment of the straight pipe comprises the following steps: heating the high-temperature alloy seamless pipe to a first temperature in a reducing atmosphere, performing first heat preservation, and air-cooling to room temperature; then heating to a second temperature, carrying out second heat preservation, and cooling to room temperature along with the furnace; the first temperature is 970-990 ℃, and the first heat preservation time is 35-45 min; the second temperature is 730-750 ℃, and the second heat preservation time is 40-50 min;
the first heat preservation is carried out in a mixed atmosphere of hydrogen and nitrogen, and the flow rate of the hydrogen is 10m 3 Flow rate of nitrogen was 20m 3 /h;
The second heat preservation is carried out in a mixed atmosphere of hydrogen and nitrogen, and the flow rate of the hydrogen is 20m 3 Flow rate of nitrogen was 25m 3 /h;
The coil heat treatment includes: heating to a third temperature under a vacuum condition, carrying out third heat preservation, and then cooling to 560-580 ℃ in a furnace; then cooling to a fourth temperature in oxygen atmosphere, carrying out furnace cooling to not more than 200 ℃ after fourth heat preservation, and discharging and air cooling; the third temperature is 670-690 ℃, and the third heat preservation time is 30-40 min; the fourth temperature is 540-560 ℃, and the fourth heat preservation time is 40-50 min.
2. The heat treatment method according to claim 1, wherein a temperature rising rate from room temperature to the first temperature is 8-10 ℃/s.
3. The heat treatment method according to claim 1, wherein a temperature rising rate from room temperature to the second temperature is 8-10 ℃/s.
4. The heat treatment method according to claim 1, wherein the heat treatment of the straight pipe further comprises coil forming, and the coil is subjected to heat treatment.
5. The heat treatment method according to claim 1, wherein a temperature rising rate from room temperature to the third temperature is 8-10 ℃/s.
6. The heat treatment method according to claim 1, wherein the fourth heat preservation pressure is 0.01-0.03 mpa.
7. A superalloy heat-treated seamless tube produced by the heat treatment method according to any one of claims 1 to 6.
8. Use of the superalloy heat treated seamless tube of claim 7 in a nuclear reactor train.
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CN110218940A (en) * 2019-06-24 2019-09-10 江苏大学 A kind of high-temperature alloy seamless pipe and preparation method thereof
WO2021248755A1 (en) * 2020-06-12 2021-12-16 江苏银环精密钢管有限公司 Novel nickel-chromium-cobalt-molybdenum high-temperature alloy seamless pipe for use in power station and manufacturing method therefor
CN114632837A (en) * 2022-03-07 2022-06-17 江苏银环精密钢管有限公司 Preparation method of spiral heat exchange tube of high-temperature gas cooled reactor steam generator

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CN110218940A (en) * 2019-06-24 2019-09-10 江苏大学 A kind of high-temperature alloy seamless pipe and preparation method thereof
WO2021248755A1 (en) * 2020-06-12 2021-12-16 江苏银环精密钢管有限公司 Novel nickel-chromium-cobalt-molybdenum high-temperature alloy seamless pipe for use in power station and manufacturing method therefor
CN114632837A (en) * 2022-03-07 2022-06-17 江苏银环精密钢管有限公司 Preparation method of spiral heat exchange tube of high-temperature gas cooled reactor steam generator

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