CN110923569A - Nuclear grade high-strength high-intergranular corrosion-resistant large-section stainless steel forged pipe and manufacturing method thereof - Google Patents
Nuclear grade high-strength high-intergranular corrosion-resistant large-section stainless steel forged pipe and manufacturing method thereof Download PDFInfo
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/10—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies
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Abstract
The invention discloses a nuclear-grade high-strength high-intergranular corrosion-resistant large-section stainless steel forged pipe and a manufacturing method thereof, and a nuclear-grade high-strength high-intergranular corrosion-resistant large-size stainless steel pipeline component with excellent performance is obtained through reasonable stainless steel forged pipe component design, electroslag remelting and radial forging processes, wherein the inner diameter of the large-size stainless steel pipeline component is not less than 500mm, or the wall thickness of the large-size stainless steel pipeline component is not less than 60 mm.
Description
Technical Field
The invention belongs to the technical field of stainless steel materials and preparation processes thereof, and particularly relates to a nuclear-grade high-strength high-intergranular corrosion-resistance large-section stainless steel forged pipe and a manufacturing method thereof.
Background
Nuclear power is one of clean energy sources with low resource consumption, stable operation, reliable technology, small environmental influence and strong supply capacity, and plays a more active and important role in a future energy structure system. With the continuous development of nuclear power technology and equipment, the performance requirements on key parts of the nuclear power equipment are higher and higher. Particularly, the large-scale pipe fittings such as a main pipe for connecting a reactor pressure vessel and a steam generator, a control rod driving mechanism stroke sleeve, a fluctuation pipe and the like belong to nuclear power-grade parts, and are easy to generate intercrystalline corrosion, micro-deformation and the like under the conditions of high temperature and high pressure for long-term operation and sometimes even suffer from strong radiation and high-speed fluid corrosion. Therefore, higher safety performance requirements are placed on these large pipelines.
At present, 300 series austenitic stainless steel is mostly forged in large nuclear power pipelines, such as 304, 316(L) and the like, intergranular corrosion resistance, toughness and processability are improved compared with an as-cast state, the problems of coarse austenite grains, mixed grains and the like still exist, the intergranular corrosion resistance and strength are mismatched, and the problem of inconsistent distribution of austenite grains on the cross section is easy to occur particularly for large-section pipelines.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a nuclear-grade large-section stainless steel forged pipe with high strength and high intergranular corrosion resistance and a manufacturing method thereof, and solves the technical problems that austenite grains are large, distribution of the austenite grains on the cross section is inconsistent, and intergranular corrosion resistance and strength are not matched.
In order to solve the technical problems, the invention provides a nuclear-grade high-strength high-intergranular corrosion-resistance large-section stainless steel forged pipe, which comprises the following chemical components in percentage by mass: 0.01 to 0.035% of C, 0.5 to 1.0% of Si, 2.0 to 4.0% of Mn, less than or equal to 0.03% of P, less than or equal to 0.015% of S, 18 to 21% of Cr, 5.0 to 7.0% of Ni, 2.0 to 4.0% of Cu, 0.2 to 0.4% of N, less than or equal to 0.10% of Co, 0.05 to 0.10% of B, 2.5 to 3.5% of Mo, 0.10 to 0.20% of Nb, 0.1 to 0.6% of Ti0.05 to 0.12% of Al, and the balance of Fe.
Correspondingly, the invention also provides a method for manufacturing the nuclear-grade high-strength high-intergranular corrosion-resistant large-section stainless steel forging pipe, which is characterized by comprising the following steps of:
step one, material preparation → electric furnace smelting → AOD refining → steel ingot;
secondly, cutting the head/tail → electroslag remelting → electroslag ingot;
thirdly, cutting head/tail → upsetting, drawing out and cogging → extruding and perforating;
fourthly, radial forging → controlled cooling → tubing;
fifthly, solid solution aging heat treatment → machining → hydraulic pressure test;
sixth, acid washing → product.
Further, in the first step, the process of batching → electric furnace smelting → AOD refining → steel ingot specifically comprises:
the method comprises the following steps of proportioning raw materials according to the content of the components, baking the raw materials, adding the baked raw materials into an electric arc furnace for smelting, adding common glass cullet serving as a slagging material in the smelting process, keeping the smelting temperature at 1620 ℃ and 1650 ℃ after the raw materials are completely molten into molten steel, tilting the molten steel for slagging, adding low-carbon ferromanganese and ferrosilicon for deoxidation, and then increasing the power of the electric furnace to ensure that the temperature of the molten steel reaches 1640-1680 ℃ for multi-point aluminum feeding for deoxidation;
argon and oxygen are blown in during the argon oxygen decarburization smelting process, the ratio of the argon to the oxygen is changed along with the degree of oxidation reaction during the smelting process until the oxygen blowing is stopped finally, and the argon is continuously blown to stir the molten steel, so that the refining reaction is fully carried out;
and keeping the temperature of the molten liquid at 1550-1580 ℃, then pouring the molten liquid into a steel ingot mold, covering a heat insulating agent on a riser of the mold cavity after pouring, and naturally cooling to obtain the stainless steel ingot.
Furthermore, the solution is poured by adopting a bottom pouring method when poured into the steel ingot mold, molten steel flows through a guide pipe protected by inert gas during pouring, and the vertical distance between a pouring opening and a mold cavity ladle opening is kept to be 50-100 mm during pouring.
Further, in the second step, the cutting head/tail → electroslag remelting → electroslag ingot comprises:
cutting off the head and the tail of the stainless steel ingot, carrying out electroslag remelting, smelting by adopting a three-phase slag furnace, adding 20-25% of CaO and 75-80% of CaF2+ 0.5-1% cryolite, Ca: si ═ 3: 7, adhering the silico-calcium powder on an electrode for deoxidation, wherein the adding proportion is 0.5-0.6 wt%, argon blowing is arranged at the bottom of the furnace at an interval of 90 degrees, the flow is 0.4-0.6L/min, the time is 8-15 min, the voltage at the initial stage of smelting is reduced from 80V to 50V, the current is reduced from 14KA to 13KA, the voltage and the current are kept constant in the melting period, and feeding treatment is carried out at the final stage of solidification: 12000A (18min) → 8500A (18min) → 6000A (10-15 min) → 3500A (5-8 min) → 2000A (2-4 min) → 0, and finally performing die cooling for 3-4 h to obtain the stainless steel electroslag ingot.
Further, the third step of the heading/tail → upsetting, drawing out and cogging → extruding and perforating process comprises:
cutting off the head and the tail of a stainless steel electroslag ingot, performing double heading and double drawing cogging, heating to 1100 ℃ for the first time, upsetting with the deformation of 20-28%, returning to the furnace and heating to 1140 ℃, performing first drawing and second upsetting with the deformation of 15-20%, returning to the furnace and heating to 1140 ℃, and performing second drawing and cogging to a set size; and carrying out hot extrusion perforation on the blank.
Further, the radial forging → controlled cooling → tube material in the fourth step comprises:
in the radial forging process, slowly heating a stainless steel pipe blank to 580-650 ℃ at a speed of 80 ℃/h, preserving heat for 0.5-1 hour, further continuously heating to 1050-1150 ℃ at a speed of 90 ℃/h, preserving heat for 1-2 hours, then starting forging at 1000-1060 ℃, wherein in the radial forging process, the angular rotation parameter of an ingot blank is 12-18 DEG/hammer, the blank feeding speed is 8-10 m/min, forging is carried out in multiple passes, the blank rotation angle of each forging is gradually increased at an angle of 1 DEG, the blank feeding speed of each forging is gradually reduced at a speed of 1m/min, the forging ratio is 3.0-4.5, the final forging temperature is 860-920 ℃, cooling is carried out to 550-590 ℃, isothermal temperature is 1.5-2 hours, and air cooling is carried out to room temperature, and finally a forged pipe is obtained.
Further, the fifth step of solution aging heat treatment → machining → hydrostatic test comprises:
heating the forged pipe in a vacuum furnace at a heating speed of less than or equal to 80 ℃/h to 1000-1100 ℃, preserving heat for 1-4 h, carrying out solid solution treatment, and then rapidly cooling to room temperature by adopting a water cooling mode; and then, preserving the temperature of the forged pipe at 430-480 ℃ for 1.5-3.0 h for aging treatment.
Further, the sixth step of acid washing → product, comprising:
and carrying out acid pickling passivation on the stainless steel forged pipe to obtain the stainless steel pipe.
Compared with the prior art, the invention has the following beneficial effects: the nuclear-grade large stainless steel pipeline component with high strength and high intergranular corrosion resistance and excellent performance is obtained through reasonable component design, electroslag remelting and radial forging processes, and the inner diameter of the large stainless steel pipeline component is not less than 500mm or the wall thickness of the large stainless steel pipeline component is not less than 60 mm.
Detailed Description
The invention is further described below. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
A nuclear-grade large-section stainless steel forged pipe with high strength and high intergranular corrosion resistance comprises the following chemical components in percentage by mass: 0.01 to 0.035% of C (carbon), 0.5 to 1.0% of Si (silicon), 2.0 to 4.0% of Mn (manganese), 0.03% or less of P (phosphorus), 0.015% or less of S (sulfur), 18 to 21% of Cr (chromium), 5.0 to 7.0% of Ni (nickel), 2.0 to 4.0% of Cu (copper), 0.2 to 0.4% of N (nitrogen), 0.10% or less of Co (cobalt), 0.05 to 0.10% of B (boron), 2.5 to 3.5% of Mo (molybdenum), 0.10 to 0.20% of Nb (niobium), 0.1 to 0.6% of Ti (titanium), 0.05 to 0.12% of Al (aluminum), and the balance of Fe (iron).
The action of the individual components is described in detail below:
carbon: the higher the carbon content in the austenitic stainless steel is, the more serious the intergranular corrosion tendency is, but the carbon content is reduced, the strength is reduced, and the formed dispersed carbide strengthening phase is reduced, therefore, the carbon content is controlled to be 0.01-0.035 wt%.
Silicon: on one hand, silicon guarantees the deoxidation effect in steel, and on the other hand, silicon is dissolved in austenite in a solid solution manner to improve the strength of austenite, however, when the silicon content is more than 1.0 wt%, the band-shaped structure is more and the anisotropy is remarkable, and therefore, the silicon content is controlled to be 0.5-1.0 wt%.
Manganese: manganese is dissolved in austenite in a solid solution, has the function of strengthening austenite, so that the phenomenon of strength reduction caused by reduction of carbon content is replaced, in addition, manganese can also replace the function of nickel element, austenite is stabilized, an austenite structure formed at high temperature can be kept to normal temperature, and the function of manganese for stabilizing austenite in austenitic steel is about 1/2 of nickel, so that the problem of austenite stability reduction caused by reduction of nickel content is solved. The invention controls the manganese content to be 2.0-4.0 wt% and is beneficial to maintaining the strength and the austenitic structure of the steel.
Sulfur and phosphorus: the content of these two elements is required to be as low as possible to reduce their adverse effects.
Chromium: improve the intergranular corrosion resistance of austenitic stainless steel, can also form a protective film at high temperature and simultaneously form fine Cr7C3The dispersion distribution is favorable for improving the strength of the austenitic stainless steel matrix, and therefore, the chromium is controlled to be 18-21 wt%.
Nickel: the Ni-based alloy is an austenite forming element, but the cost is high, and the content of the Ni is high, so that the precipitation tendency of carbide is increased, therefore, Mn, Cu and N are used for replacing the Ni element, and the content of the Ni is controlled to be 5.0-7.0 wt%.
Copper: copper is a weak austenite forming element, improves the intergranular corrosion resistance, can form a nano-scale precipitate, is beneficial to improving the strength of an austenitic stainless steel matrix, but the hot forming performance is reduced when the content is higher, so the copper content is controlled to be 2.0-4.0 wt%.
Nitrogen: the element can be an austenite stabilizing element instead of nickel, but is a gas and is easily to form BN due to its excessive content, and therefore, the nitrogen content is controlled to be 0.2 to 0.4 wt%.
Boron: the addition of boron is beneficial to improving the hot forming performance, but if the content of boron is higher, the boron is easy to react with nitrogen element to generate BN, so that the beneficial effect of nitrogen in austenite is eliminated, and therefore, the content of boron is controlled to be 0.05-0.10 wt%.
Molybdenum: the high-temperature strength of the austenitic stainless steel is improved along with the increase of the molybdenum content, but when the content is higher, the hot working performance is deteriorated, and the intergranular corrosion resistance is reduced, therefore, the molybdenum content is controlled to be 2.5-3.5 wt%.
Niobium: can strengthen the austenitic stainless steel matrix, preferentially form Nb (C, N), reduce Cr23C6The precipitation of (2) improves the intergranular corrosion resistance, but the higher content of niobium tends to lower the toughness, so the content of niobium is 0.10 to 0.20 wt%.
Titanium: the chromium-poor grain boundary can be avoided, the intergranular corrosion resistance is improved, the formation of an austenite structure is facilitated, but inclusions such as TiN are easily formed when the titanium content is too high, and therefore, the titanium content is 0.1-0.6 wt%.
Aluminum: the deoxidizer is mainly used as a deoxidizer, can strengthen an austenitic stainless steel matrix and improve the strength, but is easy to form AlN inclusions when the content is high, and has the function of eliminating N, so the aluminum content is 0.05-0.12 wt%.
Correspondingly, the method for manufacturing the nuclear-grade high-strength high-intergranular corrosion-resistant large-section stainless steel forging pipe comprises the following steps:
the preparation process flow of the stainless steel forged pipe comprises the following steps: batching → electric furnace smelting → AOD refining → steel ingot → cutting head/tail → electroslag remelting → electroslag ingot → cutting head/tail → upsetting and drawing long and cogging → extrusion and perforation → radial forging → controlled cooling → pipe → solution and aging heat treatment → machining → hydraulic pressure test → acid pickling → product. The specific process comprises the following steps:
firstly, proportioning raw materials according to the component contents, in order to avoid gas in the raw materials from being brought into a smelting furnace, roasting the raw materials, adding the roasted raw materials into an electric arc furnace for smelting, and adding common cullet (the main component of Na) in the smelting process2O·CaO·aSiO2) The added amount of the slag-making material is about 1.5-3.0 wt% of the total weight of the raw materials, after the raw materials are completely melted into molten steel, the power of an electric furnace is reduced to keep the melting temperature at 1620-1650 ℃, the electric furnace is tilted to remove slag, then low-carbon ferromanganese and ferrosilicon are added to deoxidize, the power of the electric furnace is increased to make the temperature of the molten steel reach 1640-1680 ℃, multi-point aluminum feeding and deoxidation are carried out, 4 or 8 points of aluminum feeding are respectively carried out at the radius 1/2 of a melting furnace mouth, and the speed is about 1.0-1.5 kg/t; argon and oxygen are blown in during Argon Oxygen Decarburization (AOD) smelting, the ratio of argon to oxygen is changed along with the degree of oxidation reaction in the smelting process, and is 4:1, 3:1, 1:3 and 1:6 in sequence, until the blowing of oxygen is stopped, the argon is continuously blown to stir molten steel, so that the refining reaction is fully carried out, and the flow is 1-3 m3And h, standing the AOD furnace for about 5-10 minutes before pouring, keeping the temperature of the molten liquid at 1550-1580 ℃, pouring the molten liquid into an ingot mold, keeping the ingot mold oilless, waterless and rustless before pouring, baking the ingot mold for 1-2 hours at 300-450 ℃, pouring by adopting a bottom pouring method, allowing the molten steel to flow through a guide pipe protected by inert gas during pouring, keeping the vertical distance between a pouring gate and a mold cavity opening at 50-100 mm during pouring, avoiding the reaction of elements such as Cr, Mn and Si in the molten steel and oxygen and nitrogen in the air, covering a mold cavity riser with a heat insulating agent such as plant ash after pouring, and naturally cooling to obtain the stainless steel ingot.
Secondly, cutting off the head and the tail of the stainless steel ingot, carrying out electroslag remelting, smelting by adopting a three-phase slag furnace, and adding 20-25% of CaO and 75-80% of CaF2+ 0.5-1% cryolite, Ca: si ═ 3: 7, adhering the calcium silicate powder on an electrode for deoxidation, wherein the adding proportion is 0.5-0.6 wt%, argon blowing is arranged at the bottom of the furnace at an interval of 90 degrees, the flow is 0.4-0.6L/min, the time is 8-15 min, the voltage at the initial stage of smelting is reduced from 80V to 50V, the current is 14VAnd (3) decreasing KA to 13KA, keeping the voltage and the current constant in the melting period, and performing feeding treatment in the final solidification period: 12000A (18min) → 8500A (18min) → 6000A (10-15 min) → 3500A (5-8 min) → 2000A (2-4 min) → 0, and finally performing die cooling for 3-4 h to obtain a stainless steel electroslag ingot, wherein the size of the stainless steel electroslag ingot is about phi 550-700 mm x 1700-3000 mm.
And thirdly, cutting off the head and the tail of the stainless steel electroslag ingot, performing double heading and double drawing cogging, heating to 1100 ℃ for the first time, upsetting with the deformation of 20-28%, returning to the furnace and heating to 1140 ℃, performing first drawing and second upsetting with the deformation of 15-20%, returning to the furnace and heating to 1140 ℃, and performing second drawing and cogging to the set size. And (3) carrying out hot extrusion perforation on the blank, heating the blank at the temperature of 650-750 ℃, and perforating by using an extrusion perforating machine.
And fourthly, in the radial forging process, slowly heating the stainless steel pipe blank to 580-650 ℃ at a speed of 80 ℃/h, preserving heat for 0.5-1 hour, further continuously heating to 1050-1150 ℃ at a speed of 90 ℃/h, preserving heat for 1-2 hours, then starting forging at 1000-1060 ℃, in the radial forging process, the angular rotation parameter of the ingot blank is 12-18 DEG/hammer, the feeding speed of the blank is 8-10 m/min, forging is carried out in multiple passes, the rotating angle of the blank in each forging is gradually increased at an angle of 1 DEG, the feeding speed of the blank in each forging is gradually reduced at a speed of 1m/min, the forging ratio is 3.0-4.5, the final forging temperature is 860-920 ℃, cooling to 550-590 ℃, keeping the temperature for 1.5-2 hours, and then air cooling to room temperature, and finally obtaining the forged pipe. The forged pipe has the inner diameter of not less than 500mm or the wall thickness of not less than 60 mm.
Fifthly, heating the forged pipe in a vacuum furnace at a heating speed of less than or equal to 80 ℃/h to 1000-1100 ℃ and preserving heat for 1-4 h for solution treatment, then rapidly cooling to room temperature in a water cooling mode, completely immersing the forged pipe in water, and circulating with water, wherein the water temperature is not more than 60 ℃; and then, preserving the temperature of the forged pipe at 430-480 ℃ for 1.5-3.0 h for aging treatment.
Sixthly, carrying out acid pickling passivation, wherein acid pickling solution is as follows: 20% nitric acid, 5% hydrofluoric acid, 5% phosphono-carboxylic acid and 70% water, performing flaw detection on the stainless steel pipe subjected to heat treatment, and marking and warehousing qualified pipes.
The large-section stainless steel forged pipe has the safety performance of I, II, can be used as a nuclear power pipeline part, can replace stainless steel such as 316 and 316L, and is more excellent in performance, the grain size fluctuation range of the large-section stainless steel forged pipe prepared by the technology is less than 10% and A, B, C, D type inclusions are less than 1 level from the surface layer to the center on the cross section, the tensile strength Rm is more than or equal to 600MPa, the yield strength Rp0.2 is more than or equal to 300MPa, the face shrinkage A is more than or equal to 35%, the high temperature is 360 ℃, Rm is more than or equal to 450MPa, Rp0.2 is more than or equal to 200MPa, A is more than or equal to 45%, the impact toughness KV is more than or equal to 100J, the large-section stainless steel forged pipe can be kept for 15min under the pressure of 26.2MPa in a hydraulic pressure experiment, the forged pipe has no sweating or leakage phenomenon. According to the standard, the bending test after the intergranular corrosion of the forged tube has no obvious cracks under a microscope of 100 times and 200 times.
Example 1
The nuclear grade high-strength high-intergranular corrosion-resistance large-section stainless steel forged pipe disclosed by the invention has the advantages that the contents of different components of products of each stainless steel forged pipe example are shown in the table 1.
TABLE 1 chemical composition of the examples (wt%)
| Numbering | C | Si | Mn | Cr | Ni | Cu | N | Co | B | Mo | Nb | Ti | Al | P | S | Fe |
| Example 1 | 0.01 | 1.0 | 4.0 | 18.0 | 7.0 | 2.0 | 0.4 | 0.05 | 0.07 | 2.5 | 0.2 | 0.6 | 0.05 | 0.028 | 0.011 | Balance of |
| Example 2 | 0.035 | 0.5 | 2.0 | 21.0 | 5.0 | 3.1 | 0.22 | 0.01 | 0.08 | 3.5 | 0.13 | 0.11 | 0.07 | 0.021 | 0.008 | Balance of |
| Example 3 | 0.26 | 0.77 | 3.8 | 19.4 | 6.4 | 4.0 | 0.35 | 0.03 | 0.54 | 2.8 | 0.16 | 0.52 | 0.12 | 0.03 | 0.015 | Balance of |
| Example 4 | 0.32 | 0.81 | 2.2 | 20.7 | 5.5 | 3.5 | 0.37 | 0.04 | 0.63 | 3.1 | 0.14 | 0.33 | 0.11 | 0.01 | 0.007 | Balance of |
| Example 5 | 0.015 | 0.55 | 3.0 | 18.7 | 6.8 | 2.3 | 0.2 | 0.02 | 0.28 | 2.9 | 0.10 | 0.10 | 0.06 | 0.02 | 0.011 | Balance of |
The embodiment of the invention is a manufacturing process of the nuclear-grade high-strength high-intergranular corrosion-resistant large-section stainless steel forging pipe, which comprises the following steps: batching → electric furnace smelting → AOD refining → steel ingot → cutting head/tail → electroslag remelting → electroslag ingot → cutting head/tail → upsetting and drawing long and cogging → extrusion and perforation → radial forging → controlled cooling → pipe → solution and aging heat treatment → machining → water pressure → acid washing → product. The specific operation process is as follows.
Step one, a smelting process: the chemical components are calculated and proportioned according to the embodiment 1, and during the smelting process, ordinary cullet (the main component is Na)2O·CaO·6SiO2) The adding amount of the slag-making material is about 1.5 wt% of the total weight of the raw materials, after the raw materials are completely melted into molten steel, the power of the electric furnace is reduced to keep the melting temperature of 1620 ℃, the electric furnace is tilted to remove slag, low-carbon ferromanganese and ferrosilicon are added for deoxidation, the power of the electric furnace is increased to make the temperature of the molten steel reach 1640 ℃, multi-point aluminum feeding deoxidation is carried out, 4 or 8 points of aluminum feeding is respectively carried out at the radius 1/2 of a melting furnace mouth, and the speed is about 1.0 kg/t. Argon and oxygen are blown in during the AOD smelting process, the ratio of the argon to the oxygen is changed along with the degree of oxidation reaction in the smelting process, and is 4:1, 3:1, 1:3 and 1:6 according to the ratio, the blowing of the oxygen is stopped until the oxygen is finally stopped, the argon is continuously blown to stir the molten steel, and the flow rate is 1m3H is used as the reference value. The AOD furnace stands for about 5 minutes before casting, keeps the temperature of the molten liquid at 1550 ℃, and then the molten liquid is cast into an ingot mould, the ingot mould keeps oilless, anhydrous and rustless before casting, and is baked for 2 hours at 300 ℃, a bottom pouring method is adopted for casting, the molten steel flows through a flow guide pipe protected by inert gas during casting, the vertical distance between a casting opening and a mould cavity ladle opening is kept at 50mm during the casting process, the reaction of elements such as Cr, Mn, Si and the like in the molten steel with oxygen and nitrogen in the air is avoided, after the casting, a riser of the mould cavity is covered with a heat preservation agent such as plant ash, and the like, and a stainless steel ingot is obtained after natural cooling.
Step two, electroslag remelting process: cutting off the head and the tail of a stainless steel ingot casting before electroslag remelting, smelting by adopting a three-phase slag furnace, adding 20% of CaO, 79.5% of CaF2 and 0.5% of cryolite, and adopting Ca: si ═ 3: 7, adhering the calcium silicate powder on an electrode for deoxidation, wherein the adding proportion is 0.5 wt%, argon blowing is arranged at the bottom of the furnace at an interval of 90 degrees, the flow is 0.4L/min, the time is 8min, the voltage at the initial stage of smelting is reduced from 80V to 50V, the current is reduced from 14KA to 13KA, the voltage and the current are kept constant in the melting period, and then feeding treatment is carried out: 12000A (18min) → 8500A (18min) → 6000A (10-15 min) → 3500A (5-8 min) → 2000A (2-4 min) → 0, and finally performing die cooling for 3h to obtain a stainless steel electroslag ingot, wherein the size of the stainless steel electroslag ingot is about phi 550 x 1700 mm.
Step three, double heading and double blank pulling-out process: the first heating to 1100 deg.C for upsetting with deformation of 28%, the second heating to 1140 deg.C for first drawing and second upsetting with deformation of 20%, and the second heating to 1140 deg.C for drawing and cogging to 250 × 1000 mm. And (3) carrying out hot extrusion perforation on the blank, heating the blank to 650 ℃, and carrying out perforation by using an extrusion perforating machine.
Step four, a radial forging procedure: slowly heating the cogging stainless steel pipe blank to 580 ℃ at a speed of 80 ℃/h, preserving heat for 0.5 hour, continuously heating to 1050 ℃ at a speed of 90 ℃/h, preserving heat for 1 hour, then starting forging at 1000 ℃, wherein in the radial forging process, the angular rotation parameter of the ingot blank is 12 DEG/hammer, the feeding speed of the blank is 8m/min, the forging is carried out by multiple passes, the rotation angle of the blank for each forging is gradually increased by an angle of 1 DEG, the feeding speed of the blank for each forging is gradually reduced by a speed of 1m/min, the forging ratio is 4.5, the final forging temperature is 860 ℃, cooling to 550 ℃, keeping the temperature for 2 hours, and then air cooling to room temperature. The inner diameter of the forged pipe is less than 350mm, and the wall thickness is less than 60 mm.
Step five, a solid solution aging heat treatment process: heating the forged pipe in a vacuum furnace at a heating speed of less than or equal to 80 ℃ to 1000 ℃, preserving heat for 4 hours, carrying out solid solution treatment, then rapidly cooling to room temperature in a water cooling mode, completely immersing the forged pipe in water, and circulating the water with the water temperature not more than 60 ℃; then the forged tube is subjected to aging treatment at 430 ℃ for 3.0 h.
Sixthly, an acid washing passivation process: the pickling solution is as follows: 20% nitric acid, 5% hydrofluoric acid, 5% phosphono-carboxylic acid and 70% water, performing flaw detection on the stainless steel pipe subjected to heat treatment, and marking and warehousing the qualified pipe.
The grain size of the large-section stainless steel forged pipe is grade 8, and the A, B, C, D-type inclusions are grade 1.
Big sectionThe mechanical properties of the surface stainless steel forged pipe are as follows: at room temperature, Rm＝680MPa、Rp0.2390MPa, A41%, high temp. 360 deg.C, Rm＝490MPa、Rp0.2260MPa, A52%, and impact toughness KV＝152J。
The large-section stainless steel forged pipe has intercrystalline corrosion resistance: in the hydraulic pressure test, the pipe is kept for 15min under the pressure of 26.2MPa, and the forged pipe has no sweating or leakage phenomenon, abnormal sound and visible deformation. No obvious cracks exist in the bending test after the forged tube intergranular corrosion under a microscope of 100 times and 200 times.
Example 2
Step one, a smelting process: the chemical components are calculated and proportioned according to the embodiment 1, and during the smelting process, ordinary cullet (the main component is Na)2O·CaO·aSiO2) The added amount of the slag-forming material is about 3.0 wt% of the total weight of the raw materials, after the raw materials are fully melted into molten steel, the power of the electric furnace is reduced to keep the melting temperature at 1650 ℃, the electric furnace is tilted to remove slag, then low-carbon ferromanganese and ferrosilicon are added for deoxidation, the power of the electric furnace is increased to make the temperature of the molten steel reach 1680 ℃, multi-point aluminum feeding deoxidation is carried out, 4 or 8 points of aluminum feeding are respectively carried out at the radius 1/2 of a melting furnace mouth, and the speed is about 1.5 kg/t; argon and oxygen are blown in during the AOD smelting process, the ratio of the argon to the oxygen is changed along with the degree of oxidation reaction in the smelting process, and is 4:1, 3:1, 1:3 and 1:6 according to the ratio, the blowing of the oxygen is stopped until the oxygen is finally stopped, the argon is continuously blown in order to stir the molten steel, so that the refining reaction is fully carried out, and the flow is 3m3And h, standing the AOD furnace for about 10 minutes before pouring, keeping the temperature of the molten liquid at 1580 ℃, pouring the molten liquid into the steel ingot mold, keeping the steel ingot mold oilless, anhydrous and rustless before pouring, baking the steel ingot mold for 1 hour at 450 ℃, pouring by adopting a bottom pouring method, enabling the molten steel to flow through a flow guide pipe protected by inert gas during pouring, keeping the vertical distance between a pouring gate and a mold cavity ladle gate at 100mm in the pouring process, avoiding the reaction of elements such as Cr, Mn and Si in the molten steel and oxygen and nitrogen in the air, covering a mold cavity riser with a heat preservation agent such as plant ash after pouring, and naturally cooling to obtain the stainless steel ingot.
Step two, electroslag remelting process: cutting off the head and the tail of the stainless steel ingot, carrying out electroslag remelting, smelting by adopting a three-phase slag furnace, adding 24% of CaO, 75% of CaF2 and 1% of cryolite, and adopting Ca: si ═ 3: 7, adhering the calcium silicate powder on an electrode for deoxidation, wherein the adding proportion is 0.6%, argon blowing is arranged at the bottom of the furnace at an interval of 90 degrees, the flow is 0.6L/min, the time is 15min, the voltage at the initial stage of smelting is reduced from 80V to 50V, the current is reduced from 14KA to 13KA, the voltage and the current are kept constant in the melting period, and feeding treatment is carried out at the final stage of solidification: 12000A (18min) → 8500A (18min) → 6000A (10-15 min) → 3500A (5-8 min) → 2000A (2-4 min) → 0, and finally performing die cooling for 4h to obtain a stainless steel electroslag ingot, wherein the size of the stainless steel electroslag ingot is about phi 700mm multiplied by 3000 mm.
Step three, double heading and double blank pulling-out process: cutting off the head and the tail of the electroslag remelting stainless steel ingot, performing double upsetting and double drawing cogging, heating to 1100 ℃ for the first time, upsetting with the deformation of 20 percent, returning to the furnace and heating to 1140 ℃, performing first drawing and second upsetting with the deformation of 15 percent, returning to the furnace and heating to 1140 ℃, and performing second drawing and cogging to phi 500mm multiplied by 2000 mm. The blank was subjected to hot extrusion piercing at a heating temperature of 750 ℃ using an extrusion piercing machine.
Step four, a radial forging procedure: slowly heating a stainless steel pipe blank to 650 ℃ at a speed of 80 ℃/h, preserving heat for 0.5 hour, continuously heating to 1150 ℃ at a speed of 90 ℃/h, preserving heat for 1 hour, then starting forging at 1060 ℃, wherein in the radial forging process, the angular rotation parameter of an ingot blank is 18 DEG/hammer, the blank feeding speed is 10m/min, the forging is carried out by multiple passes, the blank rotation angle of each forging is gradually increased by an angle of 1 DEG, the blank feeding speed of each forging is gradually reduced by a speed of 1m/min, the forging ratio is 3.0, the final forging temperature is 920 ℃, cooling to 590 ℃, keeping the temperature isothermal for 2 hours, then air-cooling to room temperature, and finally obtaining a forged pipe. The forged pipe has the inner diameter of not less than 500mm or the wall thickness of not less than 60 mm.
Step five, a solid solution aging heat treatment process: heating the forged pipe in a vacuum furnace at a heating speed of less than or equal to 80 ℃/h to 1100 ℃, preserving heat for 1, carrying out solid solution treatment, then rapidly cooling to room temperature in a water cooling mode, completely immersing the forged pipe in water, and circulating the water with the water temperature not more than 60 ℃; then the forged tube is subjected to aging treatment by keeping the temperature at 480 ℃ for 1.0 h.
Sixthly, an acid washing passivation process: the pickling solution is as follows: 20% nitric acid, 5% hydrofluoric acid, 5% phosphono-carboxylic acid and 70% water, performing flaw detection on the stainless steel pipe subjected to heat treatment, and marking and warehousing qualified pipes.
The grain size of the large-section stainless steel forged tube is 6-8 grade, and the A, B, C, D-type inclusions are 1 grade.
The mechanical properties of the large-section stainless steel forged pipe are as follows: at room temperature, Rm＝630MPa、Rp0.2More than or equal to 350MPa, A more than or equal to 38 percent, high temperature of 360 ℃ and Rm≥470MPa、Rp0.2Not less than 250MPa, A not less than 45 percent and impact toughness KV≥110J。
The large-section stainless steel forged pipe has intercrystalline corrosion resistance: in the hydraulic pressure test, the pipe is kept for 15min under the pressure of 26.2MPa, and the forged pipe has no sweating or leakage phenomenon, abnormal sound and visible deformation. No obvious cracks exist in the bending test after the forged tube intergranular corrosion under a microscope of 100 times and 200 times.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A nuclear-grade high-strength high-intergranular corrosion-resistant large-section stainless steel forged pipe is characterized by comprising the following chemical components in percentage by mass: 0.01 to 0.035% of C, 0.5 to 1.0% of Si, 2.0 to 4.0% of Mn, less than or equal to 0.03% of P, less than or equal to 0.015% of S, 18 to 21% of Cr, 5.0 to 7.0% of Ni, 2.0 to 4.0% of Cu, 0.2 to 0.4% of N, less than or equal to 0.10% of Co, 0.05 to 0.10% of B, 2.5 to 3.5% of Mo, 0.10 to 0.20% of Nb, 0.1 to 0.6% of Ti, 0.05 to 0.12% of Al and the balance of Fe.
2. A method for manufacturing a nuclear-grade large-section stainless steel forging pipe with high strength and high intergranular corrosion resistance is characterized by comprising the following steps:
step one, material preparation → electric furnace smelting → AOD refining → steel ingot;
secondly, cutting the head/tail → electroslag remelting → electroslag ingot;
thirdly, cutting head/tail → upsetting, drawing out and cogging → extruding and perforating;
fourthly, radial forging → controlled cooling → tubing;
fifthly, solid solution aging heat treatment → machining → hydraulic pressure test;
sixth, acid washing → product.
3. The method for manufacturing the nuclear-grade high-strength high-intergranular corrosion-resistance large-section stainless steel forging pipe according to claim 2, wherein the first step is a process of batching → electric furnace melting → AOD refining → steel ingot, and specifically comprises the following steps:
the raw material proportioning according to the component content of claim 1, baking the raw material, adding the baked raw material into an electric arc furnace for smelting, adding common cullet as a slagging material in the smelting process, keeping the smelting temperature at 1620-;
argon and oxygen are blown in during the argon oxygen decarburization smelting process, the ratio of the argon to the oxygen is changed along with the degree of oxidation reaction during the smelting process until the oxygen blowing is stopped finally, and the argon is continuously blown to stir the molten steel, so that the refining reaction is fully carried out;
keeping the temperature of the molten liquid at 1550-1580 ℃, then pouring the solution into a steel ingot mold, pouring the solution by adopting a bottom pouring method when pouring the solution into the steel ingot mold, wherein molten steel flows through a guide pipe protected by inert gas during pouring, and the vertical distance between a pouring gate and a mold cavity ladle gate is kept at 50-100 mm in the pouring process; and after pouring, covering a heat insulating agent on a mould cavity riser, and naturally cooling to obtain the stainless steel cast ingot.
4. The method as claimed in claim 3, wherein the second step of cutting the head/tail → remelting electroslag → ingot electroslag comprises:
cutting off the head and tail of the stainless steel ingot, and electroslag remelting by adoptingSmelting in a three-phase slag furnace, and adding 20-25% of CaO and 75-80% of CaF2+ 0.5-1% cryolite, Ca: si ═ 3: and 7, adhering the silicon calcium powder on an electrode for deoxidation, wherein the adding proportion is 0.5-0.6 wt%, argon blowing is arranged at the bottom of the furnace at an interval of 90 degrees, the flow is 0.4-0.6L/min, the time is 8-15 min, the voltage at the initial stage of smelting is reduced from 80V to 50V, the current is reduced from 14KA to 13KA, the voltage and the current are kept constant in the melting period, feeding treatment is carried out at the final stage of solidification, and finally, the stainless steel electroslag ingot is obtained after mould cooling is carried out for 3-4 hours.
5. The method as claimed in claim 4, wherein the third step of the process of heading/tailing → upsetting, drawing and cogging → extruding and piercing comprises:
cutting off the head and the tail of a stainless steel electroslag ingot, performing double heading and double drawing cogging, heating to 1100 ℃ for the first time, upsetting with the deformation of 20-28%, returning to the furnace and heating to 1140 ℃, performing first drawing and second upsetting with the deformation of 15-20%, returning to the furnace and heating to 1140 ℃, and performing second drawing and cogging to a set size; and carrying out hot extrusion perforation on the blank.
6. The method as claimed in claim 5, wherein the fourth step of radial forging → controlled cooling → tube material comprises:
in the radial forging process, slowly heating a stainless steel pipe blank to 580-650 ℃ at a speed of 80 ℃/h, preserving heat for 0.5-1 hour, further continuously heating to 1050-1150 ℃ at a speed of 90 ℃/h, preserving heat for 1-2 hours, then starting forging at 1000-1060 ℃, wherein in the radial forging process, the angular rotation parameter of an ingot blank is 12-18 DEG/hammer, the blank feeding speed is 8-10 m/min, forging is carried out in multiple passes, the blank rotation angle of each forging is gradually increased at an angle of 1 DEG, the blank feeding speed of each forging is gradually reduced at a speed of 1m/min, the forging ratio is 3.0-4.5, the final forging temperature is 860-920 ℃, cooling is carried out to 550-590 ℃, isothermal temperature is 1.5-2 hours, and air cooling is carried out to room temperature, and finally a forged pipe is obtained.
7. The method for manufacturing a nuclear grade high strength high intergranular corrosion resistant large cross section stainless steel forging pipe according to claim 6, wherein the fifth step of solution aging heat treatment → machining → hydraulic pressure test comprises:
heating the forged pipe in a vacuum furnace at a heating speed of less than or equal to 80 ℃/h to 1000-1100 ℃, preserving heat for 1-4 h, carrying out solid solution treatment, and then rapidly cooling to room temperature by adopting a water cooling mode; and then, preserving the temperature of the forged pipe at 430-480 ℃ for 1.5-3.0 h for aging treatment.
8. The method of claim 7, wherein the sixth step of pickling → manufacture of the forged tube of stainless steel with large cross section comprises:
and carrying out acid pickling passivation on the stainless steel forged pipe to obtain the stainless steel pipe.
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