CN115679230A - Surface treatment process for improving hydrogen embrittlement resistance of nickel-based corrosion-resistant alloy - Google Patents
Surface treatment process for improving hydrogen embrittlement resistance of nickel-based corrosion-resistant alloy Download PDFInfo
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- CN115679230A CN115679230A CN202211341487.0A CN202211341487A CN115679230A CN 115679230 A CN115679230 A CN 115679230A CN 202211341487 A CN202211341487 A CN 202211341487A CN 115679230 A CN115679230 A CN 115679230A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 64
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 48
- 239000001257 hydrogen Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 37
- 238000004381 surface treatment Methods 0.000 title claims abstract description 30
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- 238000013532 laser treatment Methods 0.000 claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
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- 229910052742 iron Inorganic materials 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
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- 239000011651 chromium Substances 0.000 claims description 3
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- 239000010949 copper Substances 0.000 claims description 3
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011572 manganese Substances 0.000 claims description 3
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- 239000010955 niobium Substances 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
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Abstract
The invention discloses a surface treatment process for improving hydrogen embrittlement resistance of nickel-based corrosion-resistant alloy, which comprises the following steps: (1) laser fusing treatment: carrying out laser processing on a nickel-based corrosion-resistant alloy sample, wherein the laser power is 100-200W, and the laser processing speed is 5-10 mm/s; (2) solution treatment: carrying out solid solution on the sample subjected to the laser treatment at the temperature of 1000-1040 ℃ for 0.25-0.5 h, and then carrying out air cooling; (3) aging treatment: and (3) aging the air-cooled sample at 600-800 ℃ for 10-22 h, and then air-cooling to finish surface treatment. On the premise of not changing alloy components, the hydrogen brittleness resistance of the material can be improved by a simpler method such as solid solution aging after laser, the method has the characteristics of simple production process, high production speed, lower requirement on equipment, high production efficiency, small thermal influence, reliable quality and the like, and can also be used for processing parts with certain complexity.
Description
Technical Field
The invention relates to the technical field of alloy surface treatment, in particular to a surface treatment process for improving the hydrogen embrittlement resistance of a nickel-based corrosion-resistant alloy.
Background
Hydrogen embrittlement refers to the phenomenon that when a metal material is used in smelting, processing, heat treatment, acid washing, electroplating and other processes or in a hydrogen-containing medium for a long time, the mechanical property of the material is seriously degraded due to hydrogen absorption or hydrogen permeation, and brittle failure occurs. The hydrogen embrittlement phenomenon is found not only in general steel but also in stainless steel, aluminum alloy, titanium alloy, nickel-base corrosion-resistant alloy, and zirconium alloy. From the mechanical point of view, hydrogen embrittlement is shown as follows: the hydrogen has little influence on the yield strength and the ultimate strength of the metal material, but the elongation and the reduction of area are seriously reduced, the fatigue life is obviously shortened, and the impact toughness value is obviously reduced. Under the continued action of tensile stress below the breaking strength, the material will snap over a period of time.
The nickel-based corrosion-resistant alloy has unique corrosion resistance and even high-temperature corrosion resistance in various industrial corrosion environments, has the properties of high strength, good plasticity and toughness, and the like, can be smelted, cast, deformed in cold and hot modes, processed and formed, welded and the like, and is widely applied to the industries such as nuclear industry, petroleum and natural gas exploitation, storage and transportation equipment, hydroelectric power generation, chemical industry, high-temperature paper pulp production equipment and the like. The nickel-based corrosion-resistant alloy has excellent hydrogen embrittlement resistance and is widely used for manufacturing parts such as oil pipeline valves, bolts and the like in the petroleum industry. With the wide application of the nickel-based corrosion-resistant alloy in various industries, the performance requirement of the nickel-based corrosion-resistant alloy in the industry is higher and higher, and the market demand of the nickel-based corrosion-resistant alloy with better hydrogen embrittlement resistance is increased.
In the aspect of improving the hydrogen brittleness resistance of the nickel-based corrosion-resistant alloy, the hydrogen brittleness resistance of the nickel-based corrosion-resistant alloy is improved by a special heat treatment method. For example, chinese patent application CN 110564948A proposes a method for transforming a part of straight grain boundaries in an alloy into zigzag grain boundaries by heat treatment with a controlled cooling rate, which can transform high-energy straight grain boundaries into low-energy zigzag grain boundaries, and to some extent, improve the hydrogen embrittlement resistance of an iron-nickel based corrosion resistant alloy. The process belongs to the integral heat treatment of materials, and the possibility of deterioration of the mechanical property of a base material often exists when the hydrogen embrittlement resistance is improved. On the other hand, the air cooling heat treatment method only aims at one J100 alloy, so the method has certain limitation.
For example, chinese patent application CN 108130528A proposes a method for cladding a nickel-based corrosion-resistant alloy coating on the surface of a Monel 400 alloy, and the method is mainly to improve the performance of a base material by cladding a layer of self-prepared nickel-based corrosion-resistant alloy powder on a Monel 400 base body by laser. The method can obviously improve the hardness and the wear resistance of the material, but does not relate to the hydrogen resistance. In addition, the method needs to prepare proper nickel-based corrosion-resistant alloy powder in advance, which undoubtedly increases a plurality of working procedures and brings uncertainty to experimental results.
At present, no method for improving the hydrogen brittleness resistance of the alloy by adopting laser melting and solid solution aging is reported. The laser fusion process is a process in which a high power density laser interacts with the metal in a very short time, causing a localized area of the metal surface to be instantaneously heated to a relatively high temperature to fuse it. The melted surface metal is then rapidly solidified by the heat absorption and conduction of the liquid metal matrix. Solution treatment is to heat the alloy to a suitable temperature and for a sufficient time to dissolve some of the constituents of the alloy into the matrix to form a homogeneous solid solution, and then to rapidly cool the alloy to leave the constituents dissolved in the matrix as a supersaturated solid solution in the matrix, which improves the ductility and toughness of the alloy and allows for further precipitation hardening. Solution treatment is often used for nonferrous alloys. The aging treatment refers to a heat treatment process in which a metal or alloy workpiece (such as low-carbon steel and the like) is subjected to solution treatment, quenched at high temperature or deformed by cold working to a certain extent, and then placed at a higher temperature or room temperature to maintain the shape and size of the workpiece, and the properties of the workpiece change with time. Generally, the hardness, strength, plastic toughness, and internal stresses of the material change over time.
Disclosure of Invention
The invention aims to solve the problems and provides a surface treatment process for a nickel-based corrosion-resistant alloy, which reduces the hydrogen brittleness sensitivity of the nickel-based corrosion-resistant alloy by improving the hydrogen crystal boundary ratio of a surface layer and improves the hydrogen damage resistance of the conventional nickel-based corrosion-resistant alloy.
In order to achieve the purpose, the invention adopts the technical scheme that:
a surface treatment process for improving the hydrogen embrittlement resistance of a nickel-based corrosion-resistant alloy is characterized by comprising the following steps:
(1) Laser fusing treatment: carrying out laser processing on a nickel-based corrosion-resistant alloy sample, wherein the laser power is 100-200W, and the laser processing speed is 5-10 mm/s;
(2) Solution treatment: carrying out solid solution on the sample subjected to the laser treatment at the temperature of 1000-1040 ℃ for 0.25-0.5 h, and then carrying out air cooling;
(3) Aging treatment: and (3) aging the air-cooled sample at 600-800 ℃ for 10-22 h, and then air-cooling to finish surface treatment.
Preferably, the alloy sample is polished to remove scale and ensure surface flatness prior to laser processing in step (1) to facilitate laser processing.
Preferably, the laser treatment in step (1) is laser-scanned along the rolling direction of the plate material, and the diameter of a laser spot is 1-2 mm.
Preferably, the nickel-based corrosion-resistant alloy is an iron-nickel-based corrosion-resistant alloy.
Preferably, the chemical composition of the nickel-based corrosion-resistant alloy is as follows by weight percent: 45.0-55.0%, chromium: 19.5-23.0%, titanium: 0.5-2.5%, aluminum: 0.01-0.7%, silicon: less than or equal to 0.5 percent, carbon: 0.005-0.04%, molybdenum: 3.0 to 4.0%, niobium: 2.5-4.5%, copper: 1.5-3.0%, manganese: less than or equal to 1.0%, fe: and the balance.
Preferably, the laser power of the laser fusing treatment is 100-180W or 100-150W or 150-200W, and the laser processing speed is 5-7 mm/s or 7-10 mm/s.
Preferably, the solution treatment is carried out for 0.3 to 0.5h, 0.4 to 0.5h or 0.5h at the temperature of 1000 to 1040 ℃.
Preferably, the aging treatment is carried out for 12 to 20 hours at the temperature of 600 to 750 ℃.
Further preferably, the aging treatment is carried out for 14 to 18 hours, 15 to 17 hours or 16 hours at the temperature of 600 to 730 ℃, 615 to 730 ℃ or 620 to 725 ℃.
In the technical scheme, the thickness of the nickel-based corrosion-resistant alloy sample plate is 2-4 mm or 2-3 mm, and the plate is straight and has no obvious bending.
The invention has the beneficial effects that:
1. on the premise of not changing alloy components, the hydrogen brittleness resistance of the material can be improved by a simpler method such as solid solution aging after laser, and the method has the characteristics of simple production process, high production speed, lower requirement on equipment and the like.
2. The invention adopts laser melting treatment, not only has the characteristics of high production efficiency, small thermal influence, reliable quality and the like, but also can be used for processing parts with certain complexity.
Drawings
FIG. 1 is an SEM image of a laser fused nickel-base corrosion-resistant alloy of the experimental group of example 1.
FIG. 2 is an EBSD map of the experimental group of nickel-base corrosion-resistant alloys in example 1 after laser consolidation.
FIG. 3 is a graph of EBSD of the experimental set of nickel-based corrosion resistant alloys after the solution treatment in example 1.
FIG. 4 is an EBSD map of the experimental set of nickel-base corrosion resistant alloy aging processes in example 1.
FIG. 5 is an SEM photograph of the Ni-based corrosion resistant alloy of example 2 after being subjected to laser and solid solution.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to be limiting.
The nickel-based corrosion-resistant alloy in each embodiment of the invention is Incoloy alloy945, the thickness of a sample plate is 2mm, and the nickel-based corrosion-resistant alloy comprises the following chemical components: nickel: 45.0-55.0%, chromium: 19.5-23.0%, titanium: 0.5-2.5%, aluminum: 0.01-0.7%, silicon: less than or equal to 0.5 percent, carbon: 0.005-0.04%, molybdenum: 3.0 to 4.0%, niobium: 2.5-4.5%, copper: 1.5-3.0%, manganese: less than or equal to 1.0%, fe: and the balance.
Example 1
1. Alloy surface treatment
3 parallel experimental group samples according to the invention were prepared, operating according to the following steps:
1. a945 nickel-based corrosion-resistant alloy sample is ground to remove iron scales and ensure the surface flatness so as to facilitate laser processing and ensure the uniformity of the surface quality after laser processing.
2. Laser fusing treatment: and carrying out laser treatment on the polished sample, carrying out laser scanning along the plate rolling direction, wherein the laser power is 100W, the laser processing speed is 5mm/s, the spot diameter is 1mm, the lap joint rate is 50%, and the defocusing amount is 2mm. After the laser treatment, SEM analysis is carried out, as shown in figure 1, the grain size of the molten pool area after laser is far smaller than that of the substrate area, the upper part of the molten pool is columnar crystal, and the bottom part of the molten pool is isometric crystal.
3. Solution treatment: and (3) carrying out solid solution on the sample subjected to the laser treatment at 1000 ℃ for 0.5h, and then cooling in air.
4. And (3) aging treatment: the sample after air cooling is aged for 16h at 621 ℃ and then air cooled, thus finishing the surface treatment.
3 parallel control samples were prepared simultaneously, and the control samples were treated using steps 1, 3, and 4 above (i.e., solution aging treatment alone, without laser consolidation).
2. Performance detection
And (4) performing hydrogen-filled stretching on the sample after the surface treatment is finished. The hydrogen filling liquid is a mixture of phosphoric acid and a poisoning agent, the hydrogen filling temperature is 75 ℃, the normal pressure is realized, and the hydrogen filling time is 5 hours. The stretching is carried out according to GB/T228.1-2010 part 1 room temperature test method for metal material tensile test, and the mechanical properties of 3 parallel samples are averaged. The mechanical properties of the experimental and control samples are shown in table 1 below:
TABLE 1
As is clear from the results in Table 1, the nickel-base corrosion-resistant alloy surface-treated by the method of the present invention has an average tensile strength of 1135MPa, a yield strength of 833MPa, and an elongation of 13.4%. The comparison group is only processed without laser, other processing steps are the same as those of the experimental group, and the mechanical properties of the comparison group sample after being charged with hydrogen are as follows: the tensile strength is 1028MPa, the yield strength is 758MPa, and the elongation is 9.2%. The comparison of the two results shows that the tensile strength, the yield strength and the elongation of the material after laser treatment are obviously improved, and the hydrogen brittleness resistance of the material is obviously improved.
The invention adopts the laser solid solution aging to carry out surface treatment on the nickel-based corrosion-resistant alloy, the mechanism is that the hydrogen brittleness resistance of the material is improved by mainly improving the proportion of sigma 3 crystal boundary, and the increase of the sigma 3 crystal boundary can not only improve the corrosion resistance of the alloy, but also improve the hydrogen brittleness resistance of the material. Firstly, the rapid heating and cooling of laser melting refines the crystal grains, and achieves the effect of fine-grained strengthening, the average grain size of the molten pool area is only about one third of that of the matrix crystal grains (fig. 2), the grain size of the molten pool bottom is about one fiftieth of that of the matrix crystal grains, but the proportion of the sigma 3 hydrogen-resistant crystal boundary is only 2%. Secondly, the solid solution process increased the proportion of Σ 3 hydrogen resistant grain boundaries, increasing Σ 3 grain boundaries from 2% to 43.3% in the surface layer fusion region (fig. 3). Finally, the aging process increases the Σ 3 grain boundary to 54.2% (fig. 4), which further improves the hardness and plasticity of the material.
Example 2
1. Alloy surface treatment
3 parallel experimental group samples according to the invention were prepared, operating according to the following steps:
1. a945 nickel-based corrosion-resistant alloy sample is polished to remove iron scales, ensure the surface flatness to facilitate laser processing and ensure the uniformity of the surface quality after laser processing.
2. Laser fusing treatment: and carrying out laser treatment on the polished sample, carrying out laser scanning along the plate rolling direction, wherein the laser power is 200W, the laser processing speed is 10mm/s, the spot diameter is 1mm, the lap joint rate is 50%, and the defocusing amount is 2mm.
3. Solution treatment: and (3) carrying out solid solution on the sample subjected to the laser treatment at 1040 ℃ for 0.5h, and finally carrying out air cooling. Then, SEM analysis is carried out, as shown in FIG. 5, the grain size of the laser region after solid solution is still smaller than that of the substrate region, and the grown fine grains at the bottom of the molten pool can still be observed.
4. And (3) aging treatment: the samples after air cooling were aged at 721 ℃ for 16h and then air cooled to complete the surface treatment.
3 parallel control samples were prepared simultaneously, and the control samples were treated using steps 1, 3, and 4 above (i.e., solution aging treatment alone, without laser consolidation).
2. Performance detection
And (4) performing hydrogen-filled stretching on the sample after the surface treatment is finished. The hydrogen filling liquid is a mixture of phosphoric acid and a poisoning agent, the hydrogen filling temperature is 75 ℃, the normal pressure is realized, and the hydrogen filling time is 5 hours. The stretching is carried out according to GB/T228.1-2010 part 1 room temperature test method for metal material tensile test, and the mechanical properties of 3 parallel samples are averaged. The mechanical properties of the experimental and control samples are shown in table 2 below:
TABLE 2
As is clear from the results in Table 2, the nickel-base corrosion-resistant alloy surface-treated by the method of the present invention has an average tensile strength of 1097MPa, a yield strength of 784MPa and an elongation of 17.7%. The comparison group is only processed without laser, other processing steps are the same as those of the experimental group, and the mechanical properties of the comparison group sample after being charged with hydrogen are as follows: the tensile strength is 1012MPa, the yield strength is 773MPa, and the elongation is 11.5%. The comparison of the two results shows that the tensile strength and the elongation of the material after laser treatment are obviously improved, and the hydrogen brittleness resistance of the material is obviously improved.
Example 3
1. Alloy surface treatment
3 parallel experimental group samples according to the invention were prepared, operating according to the following steps:
1. a945 nickel-based corrosion-resistant alloy sample is polished to remove iron scales, ensure the surface flatness to facilitate laser processing and ensure the uniformity of the surface quality after laser processing.
2. Laser fusing treatment: and carrying out laser treatment on the polished sample, carrying out laser scanning along the plate rolling direction, wherein the laser power is 150W, the laser processing speed is 7mm/s, the spot diameter is 1mm, the lap joint rate is 50%, and the defocusing amount is 2mm.
3. Solution treatment: the laser treated sample is subjected to solid solution for 0.5h at 1020 ℃ and then air cooled.
4. And (3) aging treatment: the sample after air cooling is aged for 16h at 721 ℃ and then air cooled, and the surface treatment is finished.
3 parallel control samples were prepared simultaneously, and the control samples were treated using steps 1, 3, and 4 above (i.e., solution aging treatment alone, without laser consolidation).
2. Performance detection
And (4) performing hydrogen-filled stretching on the sample after the surface treatment is finished. The hydrogen filling liquid is a mixture of phosphoric acid and a poisoning agent, the hydrogen filling temperature is 75 ℃, the normal pressure is realized, and the hydrogen filling time is 5 hours. The stretching is carried out according to GB/T228.1-2010 room temperature test method part 1 of the metal material tensile test, and the mechanical properties of 3 parallel samples are averaged. The mechanical properties of the experimental and control samples are shown in table 3 below:
TABLE 3
As can be seen from the results in Table 3, the nickel-based corrosion-resistant alloy surface-treated by the method of the present invention has an average tensile strength of 1197MPa, a yield strength of 875MPa, and an elongation of 15.6%. The comparison group is only processed without laser, other processing steps are the same as those of the experimental group, and the mechanical properties of the comparison group sample after being charged with hydrogen are as follows: the tensile strength is 1075MPa, the yield strength is 768MPa, and the elongation is 10.8 percent. The comparison of the two results shows that the tensile strength, the yield strength and the elongation of the material after laser treatment are obviously improved, and the hydrogen brittleness resistance of the material is obviously improved.
Claims (10)
1. A surface treatment process for improving the hydrogen embrittlement resistance of a nickel-based corrosion-resistant alloy is characterized by comprising the following steps:
(1) Laser fusing treatment: carrying out laser processing on a nickel-based corrosion-resistant alloy sample, wherein the laser power is 100-200W, and the laser processing speed is 5-10 mm/s;
(2) Solution treatment: carrying out solid solution on the sample subjected to the laser treatment at the temperature of 1000-1040 ℃ for 0.25-0.5 h, and then carrying out air cooling;
(3) Aging treatment: and (3) aging the air-cooled sample at 600-800 ℃ for 10-22 h, and then air-cooling to finish surface treatment.
2. A surface treatment process according to claim 1, characterized in that: before the laser processing in the step (1), the alloy sample is polished to remove the iron scale and ensure the surface flatness so as to facilitate the laser processing.
3. A surface treatment process according to claim 1, characterized in that: in the step (1), laser processing is carried out along the rolling direction of the plate by laser scanning, and the diameter of a laser spot is 1-2 mm.
4. A surface treatment process according to claim 1, characterized in that: the nickel-based corrosion-resistant alloy is an iron-nickel-based corrosion-resistant alloy.
5. A surface treatment process according to claim 4, characterized in that: the nickel-based corrosion-resistant alloy comprises the following chemical components in percentage by weight: 45.0-55.0%, chromium: 19.5-23.0%, titanium: 0.5-2.5%, aluminum: 0.01-0.7%, silicon: less than or equal to 0.5%, carbon: 0.005-0.04%, molybdenum: 3.0 to 4.0%, niobium: 2.5-4.5%, copper: 1.5-3.0%, manganese: less than or equal to 1.0%, fe: and (4) the balance.
6. A surface treatment process according to claim 1, characterized in that: the laser power of the laser fusing treatment is 100-180W or 100-150W or 150-200W, and the laser processing speed is 5-7 mm/s or 7-10 mm/s.
7. A surface treatment process according to claim 1, characterized in that: solid solution treatment is carried out for 0.3 to 0.5h, 0.4 to 0.5h or 0.5h at the temperature of 1000 to 1040 ℃.
8. A surface treatment process according to claim 1, characterized in that: the aging treatment is carried out for 12 to 20 hours at the temperature of 600 to 750 ℃.
9. A surface treatment process according to claim 8, characterized in that: the aging treatment is carried out for 14 to 18 hours, 15 to 17 hours or 16 hours at the temperature of between 600 and 730 ℃, 615 to 730 ℃ or 620 to 725 ℃.
10. A surface treatment process according to claim 1, characterized in that: the thickness of the nickel-based corrosion-resistant alloy sample plate is 2-4 mm or 2-3 mm, and the plate is straight and has no obvious bending.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211341487.0A CN115679230B (en) | 2022-10-25 | 2022-10-25 | Surface treatment process for improving hydrogen embrittlement resistance of nickel-based corrosion-resistant alloy |
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