CN114150207A - High-strength Ni-Fe-based age-hardening corrosion-resistant alloy and preparation method thereof - Google Patents
High-strength Ni-Fe-based age-hardening corrosion-resistant alloy and preparation method thereof Download PDFInfo
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- 238000003483 aging Methods 0.000 title claims abstract description 15
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- 239000010959 steel Substances 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 43
- 230000009467 reduction Effects 0.000 abstract description 5
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- 239000010955 niobium Substances 0.000 description 12
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/002—Hybrid process, e.g. forging following casting
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING 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
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/06—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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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%
-
- 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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- Heat Treatment Of Steel (AREA)
Abstract
The invention relates to a high-strength Ni-Fe-based age hardening corrosion-resistant alloy and a preparation method thereof, wherein the alloy comprises the following components in percentage by mass: less than or equal to 0.04 percent of C, less than or equal to 0.2 percent of Si, less than or equal to 0.5 percent of Mn, less than or equal to 23 percent of Cr which is more than or equal to 19 percent, less than or equal to 48 percent of Ni which is more than or equal to 46 percent, less than or equal to 5 percent of Mo which is more than or equal to 3 percent, less than or equal to 5 percent of Nb which is more than or equal to 3 percent, less than or equal to 3 percent of Cu which is more than or equal to 1.5 percent, less than or equal to 0.5 percent of Al which is more than or equal to 0.2 percent, less than or equal to 3 percent of Ti which is more than or equal to 0.5 percent, less than or equal to 0.1 percent of trace elements and the balance of Fe. The alloy has lower nickel content, improves the mechanical property and the forgeability of the material compared with other alloys in the similar material property range, and has lower cost. The room-temperature tensile strength of a finished product bar of the alloy is more than or equal to 1300MPa, the yield strength is more than or equal to 950MPa, the elongation is more than or equal to 15%, the reduction of area is more than or equal to 25%, and the grain size is 5-grade or finer.
Description
Technical Field
The invention relates to a metal material, in particular to a high-strength Ni-Fe-based age-hardening corrosion-resistant alloy and a preparation method thereof.
Background
High strength corrosion resistant nickel-based alloys used in the energy industry are required to have excellent physical properties such as strength, hardness and creep resistance at higher operating temperatures, while having good corrosion resistance. The high-strength nickel-base alloy matrix is composed of a gamma-phase, mainly contains Nb and Ni, and solid solution strengthening elements of Cr, Mo, Ti and Al to form a strengthening precipitation phase, wherein the Ni forms a strengthening precipitation phase3(Al, Ti, Nb)) phase. Because the nickel-based alloy has high nickel and niobium content and is easy to form segregation in the solidification process, the hot workability is poor, so that the iron is added on the basis of the nickel base, and the iron-nickel-based corrosion-resistant alloy also has good corrosion resistance and strength through comprehensive optimization of components and processes. However, in recent two years, the price of nickel raw materials fluctuates, the cost of the nickel-based corrosion-resistant alloy rises, and a manufacturing plant sensitive to the cost bears the cost pressure for a long time.
At present, the content of nickel in the alloy with lower nickel content, such as 925 alloy, can be as low as 40%, the content of nickel and iron is more than or equal to 50%, the highest tensile strength can be about 1150MPa, the highest yield strength is about 800MPa, the performance is different from that of the main stream corrosion-resistant alloy 718, and the application scene is limited. In 2008, SMC introduced a new economical corrosion resistant nickel-based alloy (Ni about 47%) with properties similar to 718, good ductility, impact strength and stress corrosion cracking resistance. The economical nickel-based corrosion-resistant alloy has obvious price advantage by adopting cheaper alloy elements to replace expensive Nb, Mo and the like on the premise of reducing the nickel content, has the potential of replacing the traditional high-nickel corrosion-resistant alloy in certain application occasions, is widely applied abroad, receives domestic attention in recent years, and does not have mature similar product production at home.
Although the nickel-based alloy is mature in processing technology, more alloy elements are added in the alloy, and some solid solution strengthening elements are easy to segregate and aggregate in the solidification process, so that a brittle phase is formed, and a hot processing interval is narrow. Meanwhile, the nickel-based alloy needs two indispensable steps of solution treatment and aging treatment when being prepared at present, and the aging treatment usually comprises two different heat treatment temperature sections, so that the preparation cost is high.
Disclosure of Invention
The invention aims at the defects and provides a high-strength Ni-Fe-based age hardening corrosion-resistant alloy and a preparation method thereof, wherein the alloy has lower nickel content (not higher than 49%), improves the performance and the forgeability and has lower cost compared with other alloys in the similar material performance range. The room-temperature tensile strength of a finished product bar of the alloy is more than or equal to 1300MPa, the yield strength is more than or equal to 950MPa, the elongation is more than or equal to 15%, the reduction of area is more than or equal to 25%, and the grain size is 5-grade or finer.
The technical scheme of the invention is as follows:
the high-strength Ni-Fe-based age hardening corrosion resistant alloy comprises the following components in percentage by mass: less than or equal to 0.04 percent of C, less than or equal to 0.2 percent of Si, less than or equal to 0.5 percent of Mn, less than or equal to 23 percent of Cr which is more than or equal to 19 percent, less than or equal to 48 percent of Ni which is more than or equal to 46 percent, less than or equal to 5 percent of Mo which is more than or equal to 3 percent, less than or equal to 5 percent of Nb which is more than or equal to 3 percent, less than or equal to 3 percent of Cu which is more than or equal to 1.5 percent, less than or equal to 0.5 percent of Al which is more than or equal to 0.2 percent, less than or equal to 3 percent of Ti which is more than or equal to 0.5 percent, less than or equal to 0.1 percent of trace elements and the balance of Fe.
The better technical scheme is as follows: the alloy comprises the following components in percentage by mass: 0.012-0.032% of C, 0.113-0.172% of Si, 0.074-0.436% of Mn, 20.58-21.79% of Cr, 46.80-47.93% of Ni, 3.41-3.52% of Mo, 3.06-3.54% of Nb, 1.85-2.02% of Cu, 0.243-0.302% of Al, 1.81-2.46% of Ti, 0.013-0.052% of trace elements and the balance of Fe.
The microelements are V, Mg and B.
The trace elements V + Mg + B are less than 0.1 percent, wherein Mg is not higher than 0.0075 percent.
The preparation method of the alloy comprises the following steps:
taking the components according to the proportion, carrying out vacuum induction melting, casting the components into bars, carrying out electroslag remelting to form steel ingots, carrying out homogenization heat treatment, carrying out hot forging for multiple times to form the bars, carrying out solid solution at 950-1050 ℃, carrying out heat preservation for 0.5-4 hours, carrying out water cooling, carrying out heat preservation for 6-9 hours in air at 680-770 ℃, then cooling to 600-630 ℃ at 40-70 ℃/h, and carrying out heat preservation for 0-8 hours.
The homogenization treatment is carried out at 1100-1190 ℃ for 24-72 hours.
The heat preservation temperature of the hot forging is 1050-1150 ℃, and the heat preservation time is 1-2 hours.
The starting temperature of hot forging is less than or equal to 1050 ℃, the temperature is controlled to be more than or equal to 950 ℃ in the metal deformation process, tempering and forging can be carried out for multiple times in hot rolling, and the forging deformation of the finished product at the last time is ensured to be more than 30%.
The multiple tempering is less than or equal to 4 times.
And in the heat preservation stage at the temperature of 600-630 ℃, when the impact property on the material is less than or equal to 30J, the heat preservation time is zero.
The main functions of the alloy elements in the invention are as follows:
ni is the basis of the alloy, provides a gamma phase matrix, and provides a basis for resisting stress corrosion and hydrogen sulfide ion stress corrosion cracking. Ni and Fe are transition elements in the periodic table of elements, have great similarity, can form a continuous solid solution, and provide basic conditions for solid solution strengthening and second phase strengthening.
Nb, Ti and Al are main components of the strengthening precipitated phases gamma 'and gamma' of the precipitation type hard alloy, and the excessive addition thereof causes the reduction of the hot workability, and the insufficient addition thereof causes the performance deficiency. In addition, Ti and Al are elements easy to segregate and burn, and because excessive addition of Ti and Al in the electroslag remelting smelting process can cause serious component segregation of the prepared electroslag ingot, which is not beneficial to later-stage hot working treatment and material property stabilization, Ti and Al need to be strictly controlled.
Mo and Nb are solid solution strengthening elements of nickel base alloy and form M6The main combination elements of C are excessive and easily form a grain boundary carbide coating film, a topological close-packed phase reduces the toughness of the alloy, and the content of the C needs to be properly controlled.
The Cu element is beneficial to improving the corrosion resistance of the alloy in a reducing medium, and researches show that the Cu element added into the heat-resistant stainless steel can further improve the segregation and the morphology of Nb-containing phases and Z phases and improve the creep and the endurance quality, and the researches are not found in corrosion-resistant alloys.
C. Si and Mn elements can deoxidize and refine the alloy, improve the fluidity of liquid metal and improve the casting performance of the metal, but the elements are sensitive to harmful precipitated intermediate phases, are easy to form TCP phases such as LAVES and the like, and are easy to segregate grain boundaries, so that the grain boundary strength of the alloy is reduced, and therefore, the content of C, Si and Mn is controlled to be less than or equal to 0.02 percent, less than or equal to 0.2 percent and less than or equal to 0.5 percent.
V, Mg and B are trace elements, the hot workability of the alloy is mainly improved, the total content of the V, Mg and B is usually dozens of ppm, wherein excessive B causes segregation grain boundaries, influences the hot strength of the material and easily causes cracking along the grain boundaries in the forging process; mg can improve high-temperature follow-up property and has an inhibiting effect on crack initiation and crack propagation, and more than 0.0075 percent of Mg can cause that the high strength of the alloy cannot be continuously maintained.
The high-strength Ni-Fe-based age hardening corrosion-resistant alloy contains alloy elements such as Fe, Cu, Ti, Al, Nb and the like, particularly, the Cu element is adopted to replace part of solid solution strengthening element Nb, more Fe replaces Ni, and the material cost is lower. The alloy further finely adjusts the content of Mo and Nb strengthening elements to ensure the performance, adds trace elements V, Mg and B to improve the processing performance, reduces the hot cracking tendency and improves the forging performance.
The electroslag ingot of the high-strength Ni-Fe-based age hardening type corrosion resistant alloy needs to be subjected to homogenization treatment and is treated at 1100-1190 ℃ for 24-72 hours to relieve micro segregation.
The invention relates to a hot forging process of a high-strength Ni-Fe-based age hardening type corrosion-resistant alloy, which comprises the following steps: the hot forging starting temperature is less than or equal to 1050 ℃, the hot forging can be performed for a plurality of times, the number of times is not more than 4, and the final forging deformation of the finished product is not less than 30%.
The invention relates to a heat treatment method of a high-strength Ni-Fe-based age hardening type corrosion-resistant alloy, which comprises the following steps: the solid solution is adopted for preserving heat for 0.5-4 hours at 950-1050 ℃, the water is cooled, the heat is preserved for 6-9 hours in air at 680-770 ℃, and then the mixture is cooled to 600-630 ℃ at 40-70 ℃/h and preserved for 0-8 hours.
The high-strength Ni-Fe-based age hardening corrosion-resistant alloy disclosed by the invention precipitates strengthening phases such as gamma ', gamma', delta, carbon nitride and the like after heat treatment, is strengthened by multi-element alloy, has outstanding strength performance and ensures good corrosion resistance. If the material with the impact performance requirement of the material strength lower than 30J is emphasized, the heat treatment process can be adjusted, an aging section at 630-600 ℃ is omitted, the aging heat treatment time is reduced, and on the premise of keeping the performance, the production efficiency is improved and the equipment cost is saved.
The high-strength Ni-Fe-based age hardening type corrosion-resistant alloy is mainly applied to the preparation of the alloy and contains CO2、H2S、Cl-And manufacturing simple substance S oil-gas direct contact mechanism parts.
The alloy of the invention is verified by experiments: the room temperature tensile strength of the finished bar is more than or equal to 1300MPa, the yield strength is more than or equal to 950MPa, the elongation is more than or equal to 15%, the reduction of area is more than or equal to 25%, and the grain size is 5-grade or finer.
The high-strength Ni-Fe-based age hardening corrosion-resistant alloy disclosed by the invention is close to or even better than 718 alloy in performance, but is lower in cost.
Drawings
FIG. 1 is a graph of the performance of the alloy of the present invention at different aging temperatures;
FIG. 2 is a metallographic structure after solid solution and secondary aging at different temperatures, wherein FIG. 2a shows a 700-sample microstructure morphology of 500 ×; FIG. 2b shows 720 microstructures 500X; FIG. 2c shows a 740-like microstructure pattern 500 ×; FIG. 2d shows a 760-sample microstructure 500 ×;
FIG. 3 is a comparison of the properties after solid solution +730 ℃ aging after forging.
Detailed Description
The contents of the components of the high-strength Ni-Fe-based age-hardening corrosion-resistant alloy are shown in the table 1:
TABLE 1
| Numbering | C | Si | Mn | Cr | Ni | Mo |
| P05 | 0.012 | 0.172 | 0.436 | 21.79 | 47.93 | 3.52 |
| P6218 | 0.032 | 0.113 | 0.074 | 20.58 | 46.80 | 3.41 |
| Numbering | Nb | Cu | Ti | Al | Fe | Mg+V+B |
| P05 | 3.06 | 2.02 | 2.46 | 0.243 | Surplus | 0.013 |
| P6218 | 3.54 | 1.85 | 1.81 | 0.302 | Surplus | 0.052 |
The preparation method of the copper-containing high-strength iron-nickel-based corrosion-resistant alloy comprises the following steps:
the components are taken according to the proportion, and are prepared into an electroslag ingot round bar (see patent application number: 202110759505.2) through a vacuum induction smelting and electroslag remelting duplex smelting process, the round bar is subjected to homogenization treatment at 1100-1190 ℃ for 24-72 hours, and air cooling is carried out. Heating to 1080-1120 ℃ before hot forging, keeping the temperature for 1-2 hours, and controlling the temperature to be not lower than 950 ℃ in the metal deformation process in the hot forging process. After air cooling inspection of the forged blank without cracks, carrying out 980-1030 ℃ solid solution on the material, carrying out heat preservation for 2-4 hours, then carrying out water cooling, then carrying out heat preservation for 6-9 hours in air at 680-770 ℃, and cooling to 600-630 ℃ at 40-70 ℃/h for 0-8 hours (if the requirement of the material strength on the impact performance is not higher than 30J, carrying out heat preservation at 600-630 ℃, and if the requirement of the material strength on the impact performance is higher than 30J, carrying out heat preservation at 600-630 ℃), thus obtaining the copper-containing high-strength iron-nickel-based corrosion resistant alloy.
Example 1
Adopting a vacuum melting alloy 50kg furnace and casting the alloy
Connecting a plurality of vacuum ingots, electroslag remelting
The electroslag ingot is numbered as P05, and the electroslag ingot is placed in a heat treatment furnace for homogenization heatingThen forged into
The performance of the rod is tested after the rod is subjected to solution heat treatment, aging heat treatment and wire cutting processing sampling, the performance is shown in table 2, and the material is used for manufacturing underground parts of oil and gas fields.
Example 2
A furnace of 500kg for vacuum melting alloy is adopted and cast into
Welding multiple rods to form re-smelting electrode rods, electroslag re-smelting
The electroslag ingot is numbered P6218, the electroslag ingot is put into a heat treatment furnace for homogenization heat treatment, and is upset, drawn and forged to
The round bar is forged again to obtain
The performance of the bar material after wire cutting processing and sampling is shown in the table 2, and the material is used for manufacturing underground parts of oil and gas fields.
The heat treatment schedule described in table 2: solid solution is carried out at 980-1030 ℃ for 1-4 hours, water cooling is carried out, heat preservation is carried out in air at 680-770 ℃ for 6-9 hours, then cooling is carried out at 40-70 ℃/h to 600-630 ℃, and heat preservation is carried out for 0-8 hours.
TABLE 2
| Numbering | Heat treatment System | Rm/Mpa | Rp0.2/Mpa | A(4D)/％ | Z/％ |
| P6218 | Solid solution at 1010 ℃ for 3h + aging at 770 ℃ for 8h + at 630 ℃ for 8h | 1392 | 1189 | 20 | 22 |
| P6218 | Solid solution at 1010 ℃ for 3h + aging at 760 ℃ for 8h + at 630 ℃ for 8h | 1397 | 1189 | 20 | 22 |
| P6218 | Solid solution at 1010 ℃ for 3h + aging at 740 ℃ for 8h +630 ℃ for 8h | 1383 | 1101 | 28.5 | 34 |
| P6218 | Solid solution at 1010 ℃ for 3h + aging at 730 ℃ for 8h +630 ℃ for 8h | 1401 | 1228 | 24 | 37 |
| P6218 | Solid solution at 1010 ℃ for 3h + aging at 720 ℃ for 6h +630 ℃ for 6h | 1313 | 1024 | 31.5 | 49 |
| P6218 | Solid solution at 1000 ℃ for 3h +730 ℃ for 8h | 1381 | 1099 | 30 | 37 |
| P05 | Solid solution at 1010 ℃ for 1h + aging at 720 ℃ for 6h +630 ℃ for 6h | 1338 | 956 | 31 | 42 |
| P05 | Solid solution at 1000 ℃ for 3h + aging at 730 ℃ for 8h +614 ℃ for 8h | 1368 | 1055 | 28.5 | 43 |
| P05 | Solid solution 1025 ℃ 2h + aging 690 ℃ 8h +614 ℃ 8h | 1301 | 952 | 43 | 55 |
| P05 | Solid solution at 980 ℃ for 1h + aging at 730 ℃ for 8h +620 ℃ for 8h | 1437 | 956 | 36.5 | 38 |
The alloy of the invention is verified by experiments: the room temperature tensile strength of the finished bar is more than or equal to 1300MPa, the yield strength is more than or equal to 950MPa, the elongation is more than or equal to 15%, the reduction of area is more than or equal to 25%, and the grain size is 5-grade or finer.
Claims (10)
1. The high-strength Ni-Fe-based age-hardening corrosion-resistant alloy is characterized by comprising the following components in percentage by mass: less than or equal to 0.04 percent of C, less than or equal to 0.2 percent of Si, less than or equal to 0.5 percent of Mn, less than or equal to 23 percent of Cr which is more than or equal to 19 percent, less than or equal to 48 percent of Ni which is more than or equal to 46 percent, less than or equal to 5 percent of Mo which is more than or equal to 3 percent, less than or equal to 5 percent of Nb which is more than or equal to 3 percent, less than or equal to 3 percent of Cu which is more than or equal to 1.5 percent, less than or equal to 0.5 percent of Al which is more than or equal to 0.2 percent, less than or equal to 3 percent of Ti which is more than or equal to 0.5 percent, less than or equal to 0.1 percent of trace elements and the balance of Fe.
2. The alloy of claim 1, wherein the alloy comprises the following components in percentage by mass: 0.012-0.032% of C, 0.113-0.172% of Si, 0.074-0.436% of Mn, 20.58-21.79% of Cr, 46.80-47.93% of Ni, 3.41-3.52% of Mo, 3.06-3.54% of Nb, 1.85-2.02% of Cu, 0.243-0.302% of Al, 1.81-2.46% of Ti, 0.013-0.052% of trace elements and the balance of Fe.
3. The alloy of claim 1, wherein: the microelements are V, Mg and B.
4. The alloy of claim 3, wherein: the trace elements V + Mg + B are less than 0.1 percent, wherein Mg is not higher than 0.0075 percent.
5. A method for the preparation of an alloy according to any of claims 1-4, characterized by the following steps:
the method comprises the following steps of taking the components according to the proportion of claim 1 or 2, carrying out vacuum induction melting, casting into a bar, carrying out electroslag remelting to form a steel ingot, carrying out homogenization heat treatment, carrying out hot forging for multiple times to form the bar, carrying out solid solution at 950-1050 ℃, carrying out heat preservation for 0.5-4 hours, carrying out water cooling, carrying out heat preservation for 6-9 hours in air at 680-770 ℃, then cooling to 600-630 ℃ at 40-70 ℃/h, and carrying out heat preservation for 0-8 hours.
6. The method of claim 5, wherein: the homogenization heat treatment is carried out at 1100-1190 ℃ for 24-72 hours.
7. The method of claim 5, wherein: the hot forging heat preservation temperature is 1050-1150 ℃, and the heat preservation time is 1-2 hours.
8. The method of claim 7, wherein: the starting temperature of hot forging is less than or equal to 1050 ℃, the temperature is controlled to be more than or equal to 950 ℃ in the metal deformation process, tempering and forging can be carried out for multiple times in hot rolling, and the forging deformation of the finished product at the last time is ensured to be more than 30%.
9. The method of claim 8, wherein: the multiple tempering is less than or equal to 4 times.
10. The method of claim 5, wherein: and in the heat preservation stage at the temperature of 600-630 ℃, if the requirement of the low-temperature impact property of the material is less than or equal to 30J, the heat preservation time is zero.
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