CN108998649B - Method for improving hydrogen resistance of iron-nickel-based alloy by improving proportion of special crystal boundary - Google Patents
Method for improving hydrogen resistance of iron-nickel-based alloy by improving proportion of special crystal boundary Download PDFInfo
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- CN108998649B CN108998649B CN201810784234.8A CN201810784234A CN108998649B CN 108998649 B CN108998649 B CN 108998649B CN 201810784234 A CN201810784234 A CN 201810784234A CN 108998649 B CN108998649 B CN 108998649B
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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
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
- C21D8/0236—Cold rolling
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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
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
Abstract
The invention relates to the field of iron-nickel-based alloys, in particular to a method for improving the hydrogen resistance of an iron-nickel-based precipitation strengthening austenitic alloy by improving the proportion of special grain boundaries, which solves the problems that the existing iron-nickel-based alloy is easy to form hydrogen-induced grain boundary cracks after saturated hydrogen filling, and the hydrogen brittleness sensitivity and the elongation rate are increased caused by the hydrogen-induced grain boundary cracks. By adopting a heat engine treatment (single-step deformation heat treatment) method, the special crystal boundary proportion in the alloy is improved, the hydrogen induced crack initiation and expansion resistance of the alloy is increased, and the hydrogen damage resistance of the alloy is improved, which specifically comprises the following steps: solution treatment → predeformation → heat preservation → water cooling → aging treatment → air cooling. The iron-nickel-based alloy treated by the method has the special crystal boundary proportion of 65-80 percent and the room-temperature tensile elongation of more than 33 percent; after saturated hot hydrogen filling, the room-temperature elongation of the alloy can still be kept above 30%, and the elongation loss caused by hydrogen is reduced within 10%.
Description
Technical Field
The invention relates to the field of iron-nickel-based alloy, in particular to a method for improving the hydrogen resistance of iron-nickel-based precipitation strengthened austenitic alloy by improving the proportion of special (low coincident position lattice sigma is less than or equal to 29) grain boundary
Background
The austenitic hydrogen embrittlement resistant alloy has been widely applied in the fields of energy, chemical industry, national defense and nuclear. Among the austenitic hydrogen embrittlement resistant alloys, the single phase austenitic alloy has the best hydrogen embrittlement resistance, but the strength is not high, and the yield strength (sigma) is0.2) Generally, the pressure is 200MPa or more, and the pressure is 450 to 500MPa or less. Precipitation-strengthened iron-nickel-based austenitic hydrogen-resistant alloys (hereinafter referred to as iron-nickel-based alloys) have been developed by adding alloying elements to single-phase austenitic alloys. The main precipitation strengthening function in the alloy is gamma' -Ni which has a coherent relation with a matrix3(Al, Ti) phase, which guarantees alloy strength and hydrogen resistance by controlling gamma' phase size and distribution, and room temperature yield strength (sigma)0.2) Can reach more than 700 MPa.
Although the strength of the iron-nickel-based alloy is higher than that of a single-phase austenitic alloy, the hydrogen damage resistance is obviously reduced. Taking the iron-nickel-based alloy J75 as an example, the room-temperature elongation of the alloy is 30%, and after saturated hot hydrogen charging, the room-temperature elongation is reduced to 24%, and the hydrogen-induced elongation loss reaches 20% (the hydrogen-induced elongation loss is reduced by delta)L＝(δ0-δH)/δ0，δ0: elongation at room temperature, deltaH: room temperature elongation after saturated hydrogen charge) showing a strong hydrogen induced plasticity loss (table 1). Further research shows that the J75 alloy after saturated hydrogen charging forms more hydrogen to cause cracks along grain boundaries in the process of tensile deformation, which is an important reason for reducing the hydrogen damage resistance of the alloy. Apparently, hydrogen induced crack initiation by increasing grain boundaries of iron-nickel based alloysThe resistance is generated and expanded, and the hydrogen damage resistance of the alloy is expected to be improved.
TABLE 1 tensile Properties of Fe-Ni based J75 alloys in the charged and non-charged states
Note: average of three samples per data
In a number of studies, the boundaries of Σ ≦ 29 were referred to as low Σ value coincident position lattice (CSL) boundaries, while other boundaries were classified as generally high angle boundaries. Among them, the CSL grain boundary whose sigma is less than or equal to 29 has special property, i.e. special grain boundary in the invention.
Disclosure of Invention
The invention aims to provide a method for improving the hydrogen resistance of an iron-nickel-based alloy by improving the proportion of special crystal boundaries, and solves the problem that the hydrogen resistance is reduced because the existing iron-nickel-based alloy is easy to form hydrogen and crack along the crystal boundaries.
The technical scheme of the invention is as follows:
a method for improving the hydrogen resistance of an iron-nickel-based alloy by improving the proportion of special crystal boundaries is characterized in that the proportion of the special crystal boundaries is improved by adopting a heat engine treatment method, and the special crystal boundaries refer to lattice crystal boundaries with low coincidence positions, wherein sigma is less than or equal to 29, and the method specifically comprises the following steps:
(1) the temperature of the iron-nickel base alloy plate is kept at 970-990 ℃ for 0.5-2 h;
(2) performing water quenching treatment on the iron-nickel-based alloy plate subjected to heat preservation treatment in the step (1);
(3) carrying out cold rolling deformation on the iron-nickel base alloy plate subjected to water quenching treatment in the step (2) by 4-6% on a cold rolling mill;
(4) preserving the heat of the iron-nickel base alloy plate subjected to the cold rolling deformation treatment in the step (3) at 980-1000 ℃ for 20-90 min, and then cooling the iron-nickel base alloy plate to room temperature by water;
(5) and (3) preserving the heat of the iron-nickel base alloy plate subjected to the water cooling treatment in the step (4) at 710-730 ℃ for 14-24 h, and then taking out and air-cooling to room temperature.
The method for improving the hydrogen resistance of the iron-nickel-based alloy by improving the special crystal boundary proportion has the advantage that the thickness range of the iron-nickel-based alloy plate is 2-4 mm.
The method for improving the hydrogen resistance of the iron-nickel-based alloy by improving the proportion of the special crystal boundary is characterized in that the grade of the iron-nickel-based alloy is J75.
The method for improving the hydrogen resistance of the iron-nickel-based alloy by improving the special crystal boundary proportion adopts a heat engine treatment method of single-step deformation heat treatment, so that the special crystal boundary proportion in the alloy is 65-80%, more special crystal boundary network structures are formed, the connectivity of random large-angle crystal boundaries is broken, and the resistance of the alloy to hydrogen initiation and expansion along crystal cracks is increased.
The method for improving the hydrogen resistance of the iron-nickel-based alloy by improving the special crystal boundary proportion adopts the iron-nickel-based alloy plate after the heat engine treatment, the hydrogen charging method is high-pressure gas-phase hot hydrogen charging, and the hydrogen charging conditions are as follows: the temperature is 300 +/-20 ℃, the air pressure is 10 +/-2 MPa, and the heat preservation time is 200 +/-20 h.
The method for improving the hydrogen resistance of the iron-nickel-based alloy by improving the proportion of the special crystal boundary is carried out according to GB/T228.1 part 1 room temperature test method of metal material tensile test after high-pressure gas-phase hot hydrogen charging.
The design idea of the invention is as follows:
the invention relates to a method for improving the hydrogen resistance of an iron-nickel-based alloy by improving the proportion of special crystal boundaries, which adopts a heat engine treatment method of single-step deformation heat treatment to improve the proportion of the special crystal boundaries in the alloy from 30-40% to 65-80%, and simultaneously breaks the connectivity of a large-angle random crystal boundary by introducing a high-proportion special crystal boundary, increases the initiation and expansion resistance of the crystal boundary hydrogen-induced edge crystal cracks, and improves the hydrogen resistance of the iron-nickel-based alloy, and specifically comprises the following steps: solution treatment → predeformation → heat preservation → water cooling → aging treatment → air cooling. Solution treatment: keeping the temperature at 970-990 ℃ for 0.5-2 h, on one hand, eliminating the work hardening and dissolving the precipitated phases such as carbide and the like; on the other hand, promote recrystallization and maintain proper grain size. Pre-deformation: and the deformation energy is stored in the grain boundary through pre-deformation, so that preparation is made for later-stage grain boundary migration and improvement of the proportion of special grain boundaries. And (3) heat preservation: keeping the temperature at 980-1000 ℃ for 20-90 min, and in the process, forming a high-proportion special crystal boundary; and in the heat preservation process, different types of crystal boundaries can be subjected to interactive decomposition, so that the connectivity of the large-angle random crystal boundaries is interrupted. Aging treatment: and (3) preserving the heat for 14-24 hours at 710-730 ℃, promoting the precipitation strengthening phase to be separated out in the aging process of the alloy, and ensuring the strength of the J75 alloy.
The invention has the advantages and beneficial effects that:
1. according to the invention, on the premise of not changing the alloy components, 65-80% of special crystal boundary is introduced into the alloy by a single-step thermomechanical treatment method to form a strong special crystal boundary network structure, so that the connectivity of a large-angle random crystal boundary in the alloy is broken, the hydrogen-induced crack initiation and propagation resistance along the crystal boundary of the alloy is obviously increased, and the hydrogen damage resistance of the alloy is effectively improved.
2. The iron-nickel base alloy treated by the method has better room-temperature mechanical property, the yield strength is more than 700MPa, the tensile strength is more than 1050MPa, and the elongation is more than 33%.
3. After saturated hot hydrogen filling treatment, the yield strength of the iron-nickel-based alloy treated by the method is above 700MPa, the tensile strength is above 1050MPa, the elongation is above 30%, and the hydrogen-induced elongation loss of the alloy is reduced within 10%.
Drawings
FIG. 1 is a graph of grain boundary characteristic distribution results of a J75 alloy after conventional treatment and thermomechanical treatment; wherein, (a) the non-heat-treated alloy (special grain boundary ratio 40%) and (b) the heat-treated alloy (special grain boundary ratio 75%).
FIG. 2 is a drawing of a tensile specimen of iron-nickel based alloy J75.
FIG. 3 shows the relationship between surface cracks and grain boundary types of a tensile sample of the J75 alloy after saturated hot hydrogen filling; wherein, (a) is an enlarged view of the rectangular frame region in fig. 3(b), showing that hydrogen induced cracks are formed at large angle random grain boundaries and are divided by sigma 3 grain boundaries, and no through cracks are formed; (b) hydrogen induced edge grain cracks on the surface of the tensile sample; (c) an enlarged view of the circled area in fig. 3(b) shows that hydrogen induced intergranular cracks form only at random high angle grain boundaries, and not at special grain boundaries (Σ 3).
Detailed Description
In the specific implementation process, the invention improves the hydrogen resistance of the iron-nickel-based alloy by increasing the proportion of special grain boundaries. The heat engine treatment method is adopted to promote the proportion of the special crystal boundary to 65-80% (length proportion), break the connectivity of the random crystal boundary with large angle, increase the initiation and expansion resistance of the crystal boundary to the hydrogen induced crack, and improve the hydrogen resistance of the iron-nickel-based alloy, and the process flow is as follows: solution treatment → pre-deformation → heat preservation → water cooling → aging treatment → air cooling. Wherein: the thickness range of the iron-nickel base alloy plate is 2-4 mm, the iron-nickel base alloy is J75, and the iron-nickel base alloy plate comprises the following chemical components: according to weight percentage, Ni: 29.0 to 32.0, Cr: 14.0 to 16.0, Mo: 1.30 to 1.50, titanium: 1.60-2.30, aluminum: 0.2 to 0.5, silicon: 0.1 to 0.3, boron: 0.0008-0.0025, Fe: and (4) the balance.
The present invention will be described in further detail below by way of examples and figures.
Example 1:
in the embodiment, the J75 alloy plate with the thickness of 3.0mm is subjected to heat engine treatment, the proportion of the special grain boundary reaches 75%, and the hydrogen damage resistance of the alloy is improved. The specific implementation process comprises the following steps:
1. the J75 alloy plate is a hot rolled plate, and the chemical composition of the hot rolled plate meets the requirements of GJB 5724-. Putting the J75 alloy plate into a heat treatment furnace, preserving heat for 0.5-2 h (1 h in the embodiment) at 970-990 ℃ (980 ℃ in the embodiment), and taking out for water quenching treatment;
2. and (3) performing cold rolling deformation of 4-6% (4.3% in the embodiment) on the J75 alloy plate subjected to the solution treatment in the step (1) by using a four-roll cold rolling mill.
3. And (3) carrying out heat preservation treatment on the J75 alloy plate subjected to cold rolling deformation in the step (2), wherein the heat preservation is carried out for 20-90 min (30 min in the embodiment) at 980-1000 ℃ (1000 ℃ in the embodiment), and then water cooling is carried out to room temperature.
4. And (3) preserving the heat of the J75 alloy plate subjected to water cooling in the step (3) for 14-24 h (16 h in the embodiment) at 710-730 ℃ (720 ℃ in the embodiment), and cooling the J75 alloy plate to room temperature in an air cooling mode.
5. And (3) cutting a sample from the alloy plate treated in the step (4), and performing EBSD analysis, wherein the result is shown in figure 1, gray represents a special grain boundary (sigma is less than or equal to 29), and black represents a large-angle random grain boundary. Compared with the conventional treatment (no heat treatment, the special grain boundary proportion is 40 percent, see fig. 1(a)), the special grain boundary proportion in the alloy after heat treatment is 65-80 percent (75 percent in the example), a stronger special grain boundary network is formed, and the connectivity of high-angle random grain boundaries is broken (fig. 1 (b)).
6. The J75 alloy treated according to the step 4 is processed into a tensile sample according to the drawing of FIG. 2, and the mechanical property test is carried out according to GB/T228.1 part 1 room temperature test method of metallic material tensile test, and the result is shown in Table 2.
7. The J75 alloy treated according to step 4 was processed into a tensile sample according to FIG. 2, and then placed in a high-pressure gas-phase thermal charging device for gas-phase thermal charging treatment at 300 ℃ for 200h at 10 MPa.
8. The J75 alloy sample after hydrogen filling treatment in the step 7 is subjected to tensile test according to GB/T228.1 part 1 room temperature test method for metal material tensile test, and the results are shown in Table 3.
9. And (3) intercepting the sample subjected to the tensile test according to the step (8) to perform microstructure and EBSD analysis, and displaying the result that the hydrogen induced crack propagation in the alloy is hindered by a special grain boundary, wherein the details are shown in figure 3. As can be seen from FIG. 3, hydrogen induced cracking occurs mainly at large angle Random Grain Boundaries (RGB); and the cracks do not grow and expand at special crystal boundaries (sigma is less than or equal to 29).
TABLE 2 mechanical properties of the alloy of J75 without hydrogen
TABLE 3 mechanical properties of J75 alloy hydrogen-filled test specimens
In the J75 alloy plate with the plate thickness of 3mm, a large number of special crystal boundaries appear in the alloy after the heat engine treatment, and the proportion reaches 75%. The room temperature elongation of the alloy is more than or equal to 35 percent, after high-pressure gas phase hot hydrogen charging, the room temperature elongation of the alloy is more than or equal to 30 percent, and the hydrogen-induced elongation loss of the alloy is reduced to 9.3 percent.
Example 2:
the difference from the example 1 is that the thickness of the J75 alloy plate is 3.8mm, 6% of pre-deformation is adopted, and the proportion of special grain boundary in the alloy is 72.4% by the heat preservation time of 40min at 1000 ℃.
A hot rolled sheet of J75 alloy having a thickness of 3.8mm and the same chemical composition as in example 1 was subjected to a heat treatment. Keeping the temperature at 980 ℃ for 1h, and then carrying out water quenching treatment; after 6% cold rolling deformation, heat preservation treatment at 1000 ℃ for 40min is carried out, and then water cooling is carried out to the room temperature. And (4) preserving the heat of the sample subjected to the heat engine treatment at 720 ℃ for 16h, taking out the sample, and air-cooling the sample to room temperature. The EBSD is adopted to carry out grain boundary structure analysis, and the result shows that the proportion of the special grain boundary in the alloy reaches 72.4 percent, and the connectivity of the high-angle random grain boundary is interrupted. Tensile samples of the J75 alloy sheet are processed according to the drawing of FIG. 2, and the mechanical property test is carried out according to GB/T228.1 'part 1 room temperature test method of metal material tensile test', and the results are shown in Table 4. After the J75 alloy plate subjected to aging treatment is subjected to high-pressure gas-phase hot hydrogen charging, tensile test is carried out according to GB/T228.1 part 1 room temperature test method of metal material tensile test, and the results are shown in Table 5.
TABLE 4 mechanical properties of the alloy of J75 without hydrogen
TABLE 5 mechanical properties of J75 alloy hydrogen-filled specimens
In the J75 alloy plate with the plate thickness of 3.8mm, the proportion of special grain boundaries in the alloy after the heat treatment reaches 72.4 percent. The room temperature elongation of the alloy is more than or equal to 34.8 percent, after high-pressure gas phase hot hydrogen charging, the room temperature elongation of the alloy is more than or equal to 31.5 percent, and the elongation loss caused by hydrogen is reduced to 9.7 percent.
Example 3:
the difference from the embodiment 1 is that the thickness of the selected J75 alloy plate is 4mm, 5% of pre-deformation is adopted, heat preservation treatment is carried out at 1000 ℃ for 25min, and the proportion of the special grain boundary is 77.4%.
A hot-rolled sheet of J75 alloy having a thickness of 4mm and the same chemical composition as in example 1 was subjected to a heat-engine treatment. Keeping the temperature at 980 ℃ for 2h, and then carrying out water quenching treatment; after cold rolling deformation of 5%, heat preservation treatment is carried out at 1000 ℃ for 25min, and then the steel is taken out and cooled to room temperature. And (4) preserving the heat of the sample subjected to the heat engine treatment at 720 ℃ for 16h, taking out the sample, and air-cooling the sample to room temperature. The EBSD is adopted to carry out grain boundary structure analysis, and the result shows that the proportion of the special grain boundary in the alloy reaches 77.4 percent, and the connectivity of the high-angle random grain boundary is interrupted. Tensile samples of the J75 alloy sheet are processed according to the drawing of FIG. 2, and the mechanical property test is carried out according to GB/T228.1 'part 1 room temperature test method of metal material tensile test', and the results are shown in Table 6. After the aging treatment, the J75 alloy plate is subjected to high-pressure gas-phase hot hydrogen charging, and then tensile test is carried out according to GB/T228.1 part 1 room temperature test method for metal material tensile test, and the results are shown in Table 7.
TABLE 6 mechanical properties of the alloy of J75 without hydrogen
TABLE 7 mechanical properties of J75 alloy hydrogen-filled test specimens
In the J75 alloy plate with the plate thickness of 4mm, the proportion of special grain boundaries in the alloy after the heat engine treatment reaches 77.4 percent. The room temperature elongation of the alloy is more than or equal to 35.2 percent, after high-pressure gas phase hot hydrogen charging, the room temperature elongation of the alloy is more than or equal to 32 percent, and the elongation loss caused by hydrogen is reduced to 9 percent.
The results of the examples show that the purpose of the invention can be achieved within the technological parameter range of the technical scheme of the invention, the special grain boundary proportion is effectively improved, and the hydrogen resistance of the alloy is obviously improved.
Claims (2)
1. A method for improving the hydrogen resistance of an iron-nickel-based alloy by improving the proportion of special crystal boundaries is characterized in that the proportion of the special crystal boundaries is improved by adopting a heat engine treatment method, and the special crystal boundaries refer to low-coincidence-position lattice crystal boundaries with sigma being less than or equal to 29, and specifically comprises the following steps:
(1) the temperature of the iron-nickel base alloy plate is kept at 970-990 ℃ for 0.5-2 h;
(2) performing water quenching treatment on the iron-nickel-based alloy plate subjected to heat preservation treatment in the step (1);
(3) carrying out cold rolling deformation on the iron-nickel base alloy plate subjected to water quenching treatment in the step (2) by 4-6% on a cold rolling mill;
(4) preserving the heat of the iron-nickel base alloy plate subjected to the cold rolling deformation treatment in the step (3) at 980-1000 ℃ for 20-90 min, and then cooling the iron-nickel base alloy plate to room temperature by water;
(5) preserving the heat of the iron-nickel base alloy plate subjected to water cooling treatment in the step (4) at 710-730 ℃ for 14-24 h, and taking out and air-cooling to room temperature;
the thickness range of the iron-nickel base alloy plate is 2-4 mm;
the iron nickel base alloy is under the trade mark J75;
by adopting a heat engine treatment method of single-step thermomechanical treatment, the proportion of special crystal boundaries in the alloy is 65-80%, more special crystal boundary network structures are formed, the connectivity of random large-angle crystal boundaries is broken, and the resistance of the alloy to hydrogen initiation and expansion along crystal cracks is increased;
the method for filling hydrogen into the iron-nickel-based alloy plate subjected to the heat engine treatment comprises the following steps: the temperature is 300 +/-20 ℃, the air pressure is 10 +/-2 MPa, and the heat preservation time is 200 +/-20 h.
2. The method for improving the hydrogen resistance of the iron-nickel-based alloy by increasing the proportion of the special grain boundaries according to claim 1, wherein the mechanical properties of the alloy are performed according to GB/T228.1 part 1 Room temperature test method of tensile test of metallic materials after high-pressure gas-phase hot hydrogen charging.
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| CN110964995A (en) * | 2019-11-27 | 2020-04-07 | 中国科学院金属研究所 | Increase sigma 3 IN IN718 nickel-base superalloynMethod for proportion of type crystal boundary |
| CN111411210B (en) * | 2020-04-26 | 2021-11-16 | 陕西理工大学 | Multi-angle grain boundary pure iron material and preparation method thereof |
| CN114032477B (en) * | 2021-10-20 | 2023-03-17 | 中国科学院金属研究所 | High-strength hydrogen embrittlement-resistant membrane with MP-7 mark and preparation method thereof |
| CN115679230B (en) * | 2022-10-25 | 2024-01-05 | 重庆理工大学 | Surface treatment process for improving hydrogen embrittlement resistance of nickel-based corrosion-resistant alloy |
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