CN117965929A - Gadolinium-enriched nickel-based alloy plate preparation method, gadolinium-enriched nickel-based alloy plate and component - Google Patents
Gadolinium-enriched nickel-based alloy plate preparation method, gadolinium-enriched nickel-based alloy plate and component Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 210
- 229910052688 Gadolinium Inorganic materials 0.000 title claims abstract description 116
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 239000000956 alloy Substances 0.000 title claims abstract description 108
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 106
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000005098 hot rolling Methods 0.000 claims abstract description 57
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 238000005242 forging Methods 0.000 claims abstract description 23
- 230000006698 induction Effects 0.000 claims abstract description 20
- 229910002056 binary alloy Inorganic materials 0.000 claims abstract description 16
- 238000003723 Smelting Methods 0.000 claims abstract description 15
- 238000010521 absorption reaction Methods 0.000 claims abstract description 10
- 229910001566 austenite Inorganic materials 0.000 claims abstract description 10
- 239000011159 matrix material Substances 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 210000001787 dendrite Anatomy 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims description 24
- 230000008018 melting Effects 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000003825 pressing Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 238000005266 casting Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 238000009849 vacuum degassing Methods 0.000 claims description 5
- 238000005275 alloying Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 11
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 229910000601 superalloy Inorganic materials 0.000 description 12
- 239000002915 spent fuel radioactive waste Substances 0.000 description 9
- 230000007797 corrosion Effects 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 6
- 238000005336 cracking Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910000712 Boron steel Inorganic materials 0.000 description 4
- 239000011358 absorbing material Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 229910000619 316 stainless steel Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000003758 nuclear fuel Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 229910019589 Cr—Fe Inorganic materials 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- WHXSMMKQMYFTQS-IGMARMGPSA-N lithium-7 atom Chemical compound [7Li] WHXSMMKQMYFTQS-IGMARMGPSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010308 vacuum induction melting process Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention discloses a preparation method of a gadolinium-enriched nickel-based alloy plate. The gadolinium-enriched nickel-based alloy is used for thermal neutron absorption and comprises an austenite matrix and a second-phase compound Ni 5 Gd distributed among dendrites of the austenite matrix; according to the invention, ni 87Gd13 binary alloy is used as an intermediate raw material, a vacuum induction smelting method with a specific feeding sequence is used to obtain a gadolinium-enriched nickel-based alloy cast ingot with more uniform gadolinium element distribution, and then the cast ingot is processed into a plate through a processing technology combining hot forging and hot rolling. The invention also discloses a gadolinium-enriched nickel-based alloy plate and a component. Compared with the prior art, the invention can prepare the large gadolinium-enriched nickel-based alloy plate, and the prepared gadolinium-enriched nickel-based alloy plate has excellent comprehensive performance.
Description
Technical Field
The invention relates to a preparation method of a gadolinium-enriched nickel-based alloy plate for thermal neutron absorption, belonging to the technical field of metallurgy.
Background
Nuclear energy, which is a clean, efficient and stable energy source, has become a strategic focus of long-term planning in world energy. The electricity generation amount of China nuclear power is reported to be only 5% of the total electricity generation amount, the expected installed capacity of China nuclear power reaches 1.5 hundred million kilowatts by 2035, and the electricity generation amount is about 10%; by 2050, the installed capacity of the Chinese nuclear power needs to reach 3.5 hundred million kilowatts, the nuclear power generation amount accounts for about 15% -20%, and the development space of the nuclear power is huge.
In a nuclear reactor core, when the concentration of the fissionable isotopes in the nuclear fuel falls to a level at which a given power cannot be maintained, the nuclear fuel becomes spent fuel which needs to be discharged from the core, but is still extremely radioactive and accompanied by heat release, so the problem of handling spent fuel becomes a global problem. The better treatment mode is to adopt the closed cycle of the spent fuel, carry out post-treatment on the spent fuel and recycle the usable materials and elements in the spent fuel. This inevitably increases the flow of spent fuel handling, transportation, handling and storage. In view of the special properties of spent fuel, it is important to avoid the thermal neutrons absorbed by the number of fissionable nuclei in the spent fuel to reach subcritical during transportation or storage. The thermal neutron absorbing material widely used at present is boron steel, which has high strength, excellent corrosion resistance and good neutron absorbing capacity. However, boron is hardly dissolved in stainless steel and precipitates in the form of boride (Fe, cr) 2 B having a low melting point, resulting in a great reduction in hot ductility and hot workability of boron steel; in addition, when elemental boron is irradiated by neutrons, boron - reacts with neutrons to produce lithium - 7 and helium -. Helium-4 releases two neutrons with an accompanying exothermic reaction. If the heat cannot be timely dissipated, bubbles are generated in the material, and the mechanical property is seriously reduced. The B 4 C/Al neutron absorption material has the problems of complex process, severe interface reaction between B 4 C and Al, corrosion resistance, irradiation resistance, aging in the use process and the like, and limits the application and development of the boron neutron absorption material. Therefore, a thermal neutron absorbing material with integrated structure and function is urgently needed, and the thermal neutron absorbing material has the characteristics of easy processing, good plasticity and toughness and corrosion resistance, and can serve at normal temperature and high temperature.
The gadolinium element has a larger equivalent thermal neutron absorption section which is tens of times that of the boron element, so that the gadolinium element has stable thermal neutron radiation and better thermal stability, and the gadolinium element has recently received attention from students at home and abroad. Robino et al studied the corrosion resistance and mechanical properties of gadolinium-enriched 304L alloys of 316 stainless steel with different gadolinium contents, ha and Kim et al. However, since gadolinium is also insoluble in iron-based austenite such as 304 stainless steel and 316 stainless steel, and is formed of low melting point compound (Fe, cr, ni) 3 Gd, its melting point is around 1060 ℃, the solidification temperature range is widened, the hot working window is lowered, which results in difficult working of the material, and solidification cracks are easily generated during welding, so that it is difficult to make a large-sized member satisfying thermal neutron absorption. In order to solve the problem of the low melting point second phase, various gadolinium-rich nickel-based alloys based on Ni-Mo-Cr were developed by the United Lehigh University of national laboratory in Eda state in 2005; ni-Cr-Fe and Ni-Cr-W based gadolinium-enriched nickel-base alloys and Ni-Cr-Mo-Fe based gadolinium-enriched iron-nickel-base alloy materials with different gadolinium contents were developed by Shanghai university in 2022. In these alloys, gd is also insoluble in the matrix, but exists as a high melting point compound, ni 5 Gd, with a melting point around 1260 ℃, which greatly reduces the solidification temperature range, expands the hot working window, and is very beneficial to hot working.
Although gadolinium-enriched nickel-base alloy has good thermal neutron absorption, excellent mechanical property and excellent corrosion resistance, the problems of easy cracking and mechanical property reduction of coarse second-phase Ni 5 Gd in the processing procedures of forging, rolling and the like are not solved, so that a large gadolinium-enriched nickel-base alloy plate is difficult to process, and industrialization of the gadolinium-enriched nickel-base superalloy is seriously hindered. It is reported that only 8kg of small ingots are made at Shanghai university to prepare small plates, but the processing of large plates is not successful, and the details of the preparation process are not disclosed. Therefore, there is an urgent need to accelerate research on the preparation process of gadolinium-rich nickel-based superalloy for preparing large-scale plates.
Disclosure of Invention
The invention aims to solve the technical problems of overcoming the defects of the prior art, and provides a preparation method of a gadolinium-enriched nickel-based alloy plate, which can be used for successfully preparing a large gadolinium-enriched nickel-based alloy plate, and the prepared gadolinium-enriched nickel-based alloy plate has higher yield strength, tensile strength and better plasticity, toughness, corrosion resistance and irradiation resistance.
The technical scheme adopted by the invention specifically solves the technical problems as follows:
A preparation method of a gadolinium-enriched nickel-based alloy plate, wherein the gadolinium-enriched nickel-based alloy is used for thermal neutron absorption and comprises an austenite matrix and a second-phase compound Ni 5 Gd distributed among dendrites of the austenite matrix; the preparation method of the gadolinium-enriched nickel-based alloy plate comprises the following steps:
Step 1, preparing Ni 87Gd13 binary alloy with corresponding mass according to the mass ratio of the gadolinium-enriched nickel-based alloy; step 2, weighing other raw materials according to the mass ratio of the gadolinium-enriched nickel-based alloy, and carrying out vacuum induction smelting by using the following method:
Step 2.1, firstly, vacuum induction smelting nickel and other main component raw materials to alloying, and then vacuum degassing to obtain a molten alloy solution;
Step 2.2, adding Ni 87Gd13 binary alloy into the alloy solution and melting;
step 2.3, adding the rest raw materials into the alloy solution and melting;
Step 2.4, pouring to obtain a gadolinium-enriched nickel-based alloy cast ingot;
Step 3, hot forging the gadolinium-enriched nickel-base alloy cast ingot by using an air hammer of not more than 750kg, and hot rolling the gadolinium-enriched nickel-base alloy cast ingot with a reduction of not more than 3 mm/pass; the intermediate furnace return heat treatment temperature in the hot forging and hot rolling process is 1170+/-30 ℃;
And step 4, finally, carrying out heat treatment at 1170-1200 ℃ for 30 min+/-10 min on the gadolinium-enriched nickel-based alloy plate after hot forging and hot rolling.
Preferably, in step 2.1, the nickel raw material is placed on the upper and lower layers of the vacuum induction melting apparatus, the other main component raw material is placed between the two layers of nickel raw material, and then vacuum induction melting is performed.
Preferably, in step 1a vacuum electromagnetic suspension smelting method is used to prepare a Ni 87Gd13 binary alloy of corresponding mass.
Preferably, in the hot rolling process, hot rolling is performed at a reduction of 2 mm/pass at a plate thickness of 40 to 20 mm; when the thickness of the plate is 20-12 mm, hot rolling is carried out by the pressing amount of 1.5 mm/pass; when the thickness of the plate is 12-7 mm, hot rolling is carried out by the pressing amount of 1.0 mm/pass; when the thickness of the sheet is 7mm or less, hot rolling is performed at a reduction of 0.5 mm/pass.
Preferably, in the hot rolling process, hot rolling is performed at a reduction of 3 mm/pass at a plate thickness of 40 to 10mm; when the thickness of the plate is 11-7 mm, hot rolling is carried out by the pressing amount of 1 mm/pass; when the thickness of the sheet is 7mm or less, hot rolling is performed at a reduction of 0.5 mm/pass.
Preferably, the gadolinium-enriched nickel-based alloy comprises the following components in percentage by mass: c is less than or equal to 0.05, mn is less than or equal to 0.5, si is less than or equal to 0.5, fe is less than or equal to 5, cr: 6-8, mo: 16-18, gd less than or equal to 3.0, and the balance of Ni and unavoidable impurities.
Preferably, a casting process of power failure before live casting is used in step 2.4.
A gadolinium-enriched nickel-based alloy sheet material prepared by the method according to any one of the above technical schemes.
A gadolinium-rich nickel-based alloy component manufactured using the gadolinium-rich nickel-based alloy sheet material as described above.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
According to the invention, ni 87Gd13 binary alloy is used as an intermediate raw material, a vacuum induction smelting method with a specific feeding sequence is used to obtain a gadolinium-enriched nickel-based alloy cast ingot with more uniform gadolinium element distribution, and then the cast ingot is processed into a plate through a processing technology combining hot forging and hot rolling, so that the problems of cracking and mechanical property deterioration in the processing process can be effectively avoided, and a large gadolinium-enriched nickel-based alloy plate with excellent performance which cannot be obtained by the existing processing method can be produced; the method of the invention is applicable to various existing or to-be-existing gadolinium-enriched nickel-based alloy materials, and provides a new way for developing and producing the structural function integrated thermal neutron absorbing material.
Drawings
FIG. 1 is a schematic illustration of the vacuum induction melting process flow in example 1;
fig. 2 is a mirror image of the gadolinium-rich nickel-base superalloy ingot of example 1.
Detailed Description
The gadolinium-enriched nickel-based alloy is easy to crack and the mechanical property is reduced in the processing process due to coarse second-phase Ni 5 Gd, and the prior art is difficult to process a large gadolinium-enriched nickel-based alloy plate; aiming at the problem, the invention aims to optimize the preparation process, firstly, ni 87Gd13 binary alloy is used as an intermediate raw material, a vacuum induction smelting method with a specific feeding sequence is used for obtaining the gadolinium-enriched nickel-based alloy cast ingot with more uniform gadolinium element distribution, and then, the cast ingot is processed into a plate by a processing process combining hot forging and hot rolling, so that the problems of cracking and mechanical property deterioration in the processing process can be effectively avoided.
The technical scheme adopted by the invention specifically solves the technical problems as follows:
A preparation method of a gadolinium-enriched nickel-based alloy plate, wherein the gadolinium-enriched nickel-based alloy is used for thermal neutron absorption and comprises an austenite matrix and a second-phase compound Ni 5 Gd distributed among dendrites of the austenite matrix; the preparation method of the gadolinium-enriched nickel-based alloy plate comprises the following steps:
Step 1, preparing Ni 87Gd13 binary alloy with corresponding mass according to the mass ratio of the gadolinium-enriched nickel-based alloy; step 2, weighing other raw materials according to the mass ratio of the gadolinium-enriched nickel-based alloy, and carrying out vacuum induction smelting by using the following method:
Step 2.1, firstly, vacuum induction smelting nickel and other main component raw materials to alloying, and then vacuum degassing to obtain a molten alloy solution;
Step 2.2, adding Ni 87Gd13 binary alloy into the alloy solution and melting;
step 2.3, adding the rest raw materials into the alloy solution and melting;
Step 2.4, pouring to obtain a gadolinium-enriched nickel-based alloy cast ingot;
Step 3, hot forging the gadolinium-enriched nickel-base alloy cast ingot by using an air hammer of not more than 750kg, and hot rolling the gadolinium-enriched nickel-base alloy cast ingot with a reduction of not more than 3 mm/pass; the intermediate furnace return heat treatment temperature in the hot forging and hot rolling process is 1170+/-30 ℃;
And step 4, finally, carrying out heat treatment at 1170-1200 ℃ for 30 min+/-10 min on the gadolinium-enriched nickel-based alloy plate after hot forging and hot rolling.
Preferably, in step 2.1, the nickel raw material is placed on the upper and lower layers of the vacuum induction melting apparatus, the other main component raw material is placed between the two layers of nickel raw material, and then vacuum induction melting is performed.
Preferably, in step 1a vacuum electromagnetic suspension smelting method is used to prepare a Ni 87Gd13 binary alloy of corresponding mass.
Preferably, in the hot rolling process, hot rolling is performed at a reduction of 2 mm/pass at a plate thickness of 40 to 20 mm; when the thickness of the plate is 20-12 mm, hot rolling is carried out by the pressing amount of 1.5 mm/pass; when the thickness of the plate is 12-7 mm, hot rolling is carried out by the pressing amount of 1.0 mm/pass; when the thickness of the sheet is 7mm or less, hot rolling is performed at a reduction of 0.5 mm/pass.
Preferably, in the hot rolling process, hot rolling is performed at a reduction of 3 mm/pass at a plate thickness of 40 to 10mm; when the thickness of the plate is 11-7 mm, hot rolling is carried out by the pressing amount of 1 mm/pass; when the thickness of the sheet is 7mm or less, hot rolling is performed at a reduction of 0.5 mm/pass.
Preferably, the gadolinium-enriched nickel-based alloy comprises the following components in percentage by mass: c is less than or equal to 0.05, mn is less than or equal to 0.5, si is less than or equal to 0.5, fe is less than or equal to 5, cr: 6-8, mo: 16-18, gd less than or equal to 3.0, and the balance of Ni and unavoidable impurities.
Preferably, a casting process of power failure before live casting is used in step 2.4.
A gadolinium-enriched nickel-based alloy sheet material prepared by the method according to any one of the above technical schemes.
A gadolinium-rich nickel-based alloy component manufactured using the gadolinium-rich nickel-based alloy sheet material as described above.
For the convenience of public understanding, the following detailed description of the technical solution of the present invention will be made with reference to several examples, comparative examples and accompanying drawings:
Example 1:
The gadolinium-enriched nickel-based alloy in the embodiment comprises the following components in percentage by mass: c is less than or equal to 0.05, mn is less than or equal to 0.5, si is less than or equal to 0.5, fe is less than or equal to 5, cr: 6-8, mo: 16-18, gd:2, the balance being Ni and unavoidable impurities.
The preparation method of the gadolinium-enriched nickel-based alloy plate comprises the following steps:
Step 1, preparing Ni 87Gd13 binary alloy with corresponding mass according to the mass ratio of the gadolinium-enriched nickel-based alloy; the preparation of the Ni 87Gd13 binary alloy can adopt various existing processes, such as vacuum induction melting, vacuum electromagnetic suspension melting and the like, and in order to improve the purity of the prepared Ni 87Gd13 binary alloy as much as possible, the embodiment adopts a vacuum electromagnetic suspension melting method.
Step 2, weighing other raw materials according to the mass ratio of the gadolinium-enriched nickel-based alloy, and carrying out vacuum induction smelting by using the following method:
Step 2.1, firstly, vacuum induction smelting nickel and other main component raw materials to alloying, and then vacuum degassing to obtain a molten alloy solution;
In the embodiment, the main component raw material of the gadolinium-enriched nickel-based alloy is Ni, cr, mo, fe; firstly, putting about half of Ni at the bottom of a vacuum induction melting furnace, then putting Cr, mo and Fe on the Ni, and finally covering the rest Ni on the uppermost layer; as shown in FIG. 1, the furnace is vacuumized for 20min until the vacuum degree is less than or equal to 10 -2 Pa; vacuum induction smelting (power transmission 40kw/10 min) is carried out after argon is filled for protection (0.06 Mpa); vacuum degassing (power transmission 60kw/10 min); finally obtaining molten alloy solution (power transmission 80kw/20 min), and powering off for 2min;
Step 2.2, adding Ni 87Gd13 binary alloy into the alloy solution, melting the alloy solution (power transmission is 80kw/10 min), and refining the alloy solution for 10min (power transmission is 40 kw);
Step 2.3, adding the rest of Si, mn and C raw materials into the alloy solution and melting down (power transmission is 50kw/5 min);
Step 2.4, cooling for 5min in a power failure mode, transmitting power for 40kw finally, and pouring to obtain a gadolinium-enriched nickel-based alloy cast ingot;
As shown in fig. 1, in the embodiment, a casting process of firstly cutting off and then carrying out live casting is adopted, and 50 kg of gadolinium-enriched nickel-based superalloy cast ingots are finally obtained; gd content is measured at the 1/2 position of the upper part, the middle part and the lower part of the ingot and is respectively 1.74 percent, 1.73 percent and 1.77 percent by mass, and the Gd element is more uniformly distributed in the ingot after the process is adopted; further optical microscopic metallographic analysis of the ingots was carried out, as shown in fig. 2, wherein (a) and (b) are mirror images at low power and high power, respectively, and it was seen that in the gadolinium-enriched nickel-base alloy, ni 5 Gd was distributed among austenite dendrites in the base, and that a trace amount of carbide was attached to Ni 5 Gd.
Step 3, hot forging the gadolinium-enriched nickel-base alloy cast ingot by using an air hammer of not more than 750kg, and hot rolling the gadolinium-enriched nickel-base alloy cast ingot with a reduction of not more than 3 mm/pass; the intermediate furnace return heat treatment temperature in the hot forging and hot rolling process is 1170+/-30 ℃;
Taking an ingot, adopting a 750kg air hammer to carry out hot forging, and carrying out intermediate furnace return heat treatment at 1170+/-30 ℃ for 10-20 min; then hot rolling is carried out, wherein in the hot rolling process, when the thickness of the plate is 40-20 mm, the plate is hot rolled with the pressing quantity of 2 mm/pass, and the plate is subjected to furnace return heat treatment after two passes of hot rolling, wherein the heat treatment temperature is 1170+/-30 ℃, and the treatment time is 10-20 min; when the thickness of the plate is 20-12 mm, hot rolling is carried out with the pressing quantity of 1.5 mm/pass, and furnace returning heat treatment is carried out after two passes of hot rolling, wherein the heat treatment temperature is 1170+/-30 ℃, and the treatment time is 10-20 min; when the thickness of the plate is 12-7 mm, hot rolling is carried out with the pressing quantity of 1.0 mm/pass, and furnace returning heat treatment is carried out after two passes of hot rolling, wherein the heat treatment temperature is 1170+/-30 ℃, and the treatment time is 10-20 min; when the thickness of the plate is below 7mm, hot rolling is carried out with the pressing amount of 0.5 mm/pass, and furnace returning heat treatment is carried out after two passes of hot rolling, wherein the heat treatment temperature is 1170+/-30 ℃, and the treatment time is 10-20 min; finally, the cast ingot is rolled into a plate with the thickness of 5mm.
Step 4, finally carrying out heat treatment at 1170-1200 ℃ for 30min plus or minus 10min on the gadolinium-enriched nickel-based alloy plate after hot forging and hot rolling; in the implementation, the gadolinium-enriched nickel-based alloy plate with the thickness of 300mm multiplied by 5mm is finally obtained.
The gadolinium-enriched nickel-based alloy plate with the thickness of 300mm multiplied by 5mm prepared by the embodiment has good appearance and no obvious crack; further mechanical property test results show that the gadolinium-enriched nickel-based superalloy plate prepared by the embodiment has room-temperature tensile strength of more than 775Mpa and elongation of more than 49.0%, and the mechanical property and corrosion resistance of the gadolinium-enriched nickel-based superalloy plate are far superior to those of the traditional boron steel, B 4 C/Al-based composite material and gadolinium-containing stainless steel.
Example 2:
The gadolinium-enriched nickel-based superalloy sheet is prepared by adopting the substantially same formula and process as in the embodiment 1, and the only difference is that: in the hot rolling process, when the thickness of the plate is 40-10 mm, hot rolling is carried out with the pressing amount of 3 mm/pass; when the thickness of the plate is 11-7 mm, hot rolling is carried out by the pressing amount of 1 mm/pass; when the thickness of the plate is below 7mm, hot rolling is carried out with the pressing amount of 0.5 mm/pass; and the rest process parameters are the same, and finally the long-strip gadolinium-enriched nickel-based alloy plate with the length of 820mm multiplied by 120mm multiplied by 5mm is obtained.
The gadolinium-enriched nickel-based alloy plate with the thickness of 820mm multiplied by 120mm multiplied by 5mm prepared by the embodiment has good appearance and no obvious crack; further mechanical property test results show that the gadolinium-enriched nickel-based superalloy plate prepared by the embodiment has room-temperature tensile strength of more than 775Mpa and elongation of more than 49.0%, and the mechanical property and corrosion resistance of the gadolinium-enriched nickel-based superalloy plate are far superior to those of the traditional boron steel, B 4 C/Al-based composite material and gadolinium-containing stainless steel.
Comparative example 1:
The gadolinium-enriched nickel-based superalloy sheet was prepared by using substantially the same formulation and process as in example 1, with the only difference that the hot forging was performed using a 1000 ton air hammer, and the surface cracking of the sheet finally obtained was severe.
Comparative example 2:
the gadolinium-enriched nickel-based superalloy sheet was prepared by using substantially the same formulation and process as in example 1, with the only difference that the hot forging was performed using a1 ton air hammer, and the surface cracking of the sheet finally obtained was severe.
Comparative examples 1 and 2 show that qualified gadolinium-rich nickel-based superalloy plates cannot be obtained by hot forging with an air hammer of more than 750kg, and the influence of the hot forging process on the quality of the final plates is proved.
Example 3:
the gadolinium-rich nickel-base alloy in this example uses the same composition as the existing American ASTM B-932-04 material; the components of the composition in percentage by mass are as follows: c is less than or equal to 0.01, mn is less than or equal to 0.5, si is less than or equal to 0.08, fe is less than or equal to 1, co is less than or equal to 2, cr:14.5 to 17.1, mo:13.1 to 16.0, gd:1.9 to 2.1 percent, and the balance of nickel and unavoidable impurities.
The same gadolinium-enriched nickel-based alloy sheet preparation process as in example 2 was used for sheet preparation, wherein the gadolinium-enriched nickel-based alloy ingot had a weight of 5kg, and the final sheet size was 800mm×100mm×5mm.
The gadolinium-enriched nickel-based alloy plate prepared by the embodiment has good appearance and no obvious cracks; the test result of the further transverse mechanical property is as follows: yield strength: 462MPa; tensile strength: 778MPa; elongation percentage: 26%, the longitudinal tensile properties are: yield strength: 474MPa; tensile strength: 861MPa; elongation percentage: 55%. And the ASTM B-932-04 board mechanical property test result produced by the United states former factory is: yield strength: 400MPa; tensile strength: 701MPa; elongation percentage: 23.4% of the material, the longitudinal tensile properties are: yield strength: 404MPa; tensile strength: 785MPa; elongation percentage: 42.9%. As can be seen by comparison, the ASTM B-932-04 board prepared by the preparation process of the invention has greatly improved mechanical properties.
Comparative example 3:
200g small ingots of six different Gd contents (Gd contents 0, 0.25%, 0.5%, 1.0%, 1.5% and 2%, respectively) were prepared according to the gadolinium-enriched nickel-base alloy formulation of example 1 and using the same ingot manufacturing process as in example 1; the sheet was then prepared without hot forging, but by direct hot rolling, with the same process parameters as in example 1. Among the six finally obtained plate samples, the mechanical properties of the five gadolinium-containing samples are lower than those of the Gd-free sample and are further lower than those of the example 1, so that the necessity of combining hot forging and hot rolling processes is verified.
The preparation method of the gadolinium-enriched nickel-based alloy plate can effectively avoid the problems of cracking and mechanical property deterioration in the processing process, can be used for preparing large plates which are difficult to prepare in the prior art, and has better comprehensive performance. The gadolinium-enriched nickel-based alloy plate prepared by the invention can further obtain various components in various forms, which are suitable for various processes such as spent fuel treatment, transportation, treatment and storage, through processing means such as rolling, cutting, welding and the like.
Claims (9)
1. A preparation method of a gadolinium-enriched nickel-based alloy plate, wherein the gadolinium-enriched nickel-based alloy is used for thermal neutron absorption and comprises an austenite matrix and a second-phase compound Ni 5 Gd distributed among dendrites of the austenite matrix; the preparation method of the gadolinium-enriched nickel-based alloy plate is characterized by comprising the following steps of:
Step 1, preparing Ni 87Gd13 binary alloy with corresponding mass according to the mass ratio of the gadolinium-enriched nickel-based alloy;
step 2, weighing other raw materials according to the mass ratio of the gadolinium-enriched nickel-based alloy, and carrying out vacuum induction smelting by using the following method:
Step 2.1, firstly, vacuum induction smelting nickel and other main component raw materials to alloying, and then vacuum degassing to obtain a molten alloy solution;
Step 2.2, adding Ni 87Gd13 binary alloy into the alloy solution and melting;
step 2.3, adding the rest raw materials into the alloy solution and melting;
Step 2.4, pouring to obtain a gadolinium-enriched nickel-based alloy cast ingot;
Step 3, hot forging the gadolinium-enriched nickel-base alloy cast ingot by using an air hammer of not more than 750kg, and hot rolling the gadolinium-enriched nickel-base alloy cast ingot with a reduction of not more than 3 mm/pass; the intermediate furnace return heat treatment temperature in the hot forging and hot rolling process is 1170+/-30 ℃;
And step 4, finally, carrying out heat treatment at 1170-1200 ℃ for 30 min+/-10 min on the gadolinium-enriched nickel-based alloy plate after hot forging and hot rolling.
2. The method of manufacturing gadolinium-enriched nickel-based alloy sheet material according to claim 1, wherein in step 2.1, nickel raw materials are placed on the upper and lower layers of a vacuum induction melting apparatus, other main component raw materials are placed between two layers of nickel raw materials, and then vacuum induction melting is performed.
3. The method for preparing gadolinium-enriched nickel-base alloy sheet material according to claim 1, wherein the vacuum electromagnetic suspension smelting method is used to prepare the Ni 87Gd13 binary alloy with corresponding mass in step 1.
4. The method for preparing gadolinium-enriched nickel-base alloy sheet according to claim 1, wherein during the hot rolling, the hot rolling is performed with a pressing amount of 2 mm/pass at a sheet thickness of 40-20 mm; when the thickness of the plate is 20-12 mm, hot rolling is carried out by the pressing amount of 1.5 mm/pass; when the thickness of the plate is 12-7 mm, hot rolling is carried out by the pressing amount of 1.0 mm/pass; when the thickness of the sheet is 7mm or less, hot rolling is performed at a reduction of 0.5 mm/pass.
5. The method for preparing gadolinium-enriched nickel-base alloy sheet according to claim 1, wherein during the hot rolling, the hot rolling is performed with a reduction of 3 mm/pass at a sheet thickness of 40 to 10 mm; when the thickness of the plate is 11-7 mm, hot rolling is carried out by the pressing amount of 1 mm/pass; when the thickness of the sheet is 7mm or less, hot rolling is performed at a reduction of 0.5 mm/pass.
6. The method for preparing the gadolinium-enriched nickel-based alloy plate according to claim 1, wherein the gadolinium-enriched nickel-based alloy comprises the following components in percentage by mass: c is less than or equal to 0.05, mn is less than or equal to 0.5, si is less than or equal to 0.5, fe is less than or equal to 5, cr: 6-8, mo: 16-18, gd less than or equal to 3.0, and the balance of Ni and unavoidable impurities.
7. The method of preparing a gadolinium-enriched nickel-based alloy sheet material according to claim 1, wherein the casting process of power failure before live casting is used in step 2.4.
8. A gadolinium-enriched nickel-base alloy sheet material, characterized in that it is produced by the method according to any one of claims 1 to 7.
9. A gadolinium-rich nickel-base alloy component, characterized in that it is manufactured by using the gadolinium-rich nickel-base alloy sheet material according to claim 8.
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