CN113278895A - High-strength FeCrAl-based alloy - Google Patents
High-strength FeCrAl-based alloy Download PDFInfo
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- CN113278895A CN113278895A CN202110491841.7A CN202110491841A CN113278895A CN 113278895 A CN113278895 A CN 113278895A CN 202110491841 A CN202110491841 A CN 202110491841A CN 113278895 A CN113278895 A CN 113278895A
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- 239000000956 alloy Substances 0.000 title claims abstract description 41
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000001125 extrusion Methods 0.000 claims abstract description 23
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 229910000568 zirconium hydride Inorganic materials 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000003825 pressing Methods 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000005551 mechanical alloying Methods 0.000 claims abstract description 4
- 238000000137 annealing Methods 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 238000009837 dry grinding Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 238000005253 cladding Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 3
- 238000005728 strengthening Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 239000003758 nuclear fuel Substances 0.000 abstract description 2
- 150000003755 zirconium compounds Chemical class 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 4
- 239000002245 particle Substances 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910001093 Zr alloy Inorganic materials 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
- C22C33/0228—Using a mixture of prealloyed powders or a master alloy comprising other non-metallic compounds or more than 5% of graphite
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/28—Ferrous alloys, e.g. steel alloys containing chromium with titanium or zirconium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention discloses a high-strength FeCrAl-based alloy, relates to the technical field of nuclear fuel cladding materials, and relates to FeCrAl alloy powder, nano ZrC and nano ZrH2The powder is firstly subjected to mechanical alloying ball milling treatment, then is subjected to discharge plasma sintering forming to obtain an ingot, and finally the ingot is fed intoThe equal channel angular pressing treatment is carried out. According to the principle of the effect of dispersion strengthening and crystal boundary purification on the improvement of the performance of a metal material, in order to improve the comprehensive performance, particularly the elongation and the strength of FeCrAl, a nano-sized high-hardness phase ZrC is dispersed and distributed at the crystal boundary and in the crystal grain of FeCrAl, and the strength of FeCrAl is improved through the regulation and control of the phase boundary and the crystal boundary; meanwhile, in order to improve the plastic deformation capability of FeCrAl-ZrC, ZrH is utilized2The grain boundary purification effect during the formation of metal Zr and zirconium compounds is used for improving the elongation. In addition, an equal channel angular extrusion process is introduced after spark plasma sintering, and high-density dislocation is introduced through large plastic deformation to further improve FeCrAl-ZrC-ZrH2The comprehensive mechanical property of (2).
Description
Technical Field
The invention relates to the technical field of nuclear fuel cladding materials, in particular to a high-strength FeCrAl-based alloy.
Background
The urgent need for clean energy makes the development of nuclear energy increasingly necessary, and nuclear energy safety is the central importance of the continued development of nuclear energy. To further increase the safety threshold of nuclear energy, accident-resistant fuel concepts have been proposed, and the most critical of these is the development of accident-resistant fuel cladding to replace the zirconium alloy cladding currently in use. As a material for the accident-resistant cladding, in addition to properties similar to those of zirconium alloy, such as high strength, low neutron absorption, radiation resistance, high thermal conductivity, etc., a high resistance to water vapor oxidation is required. The FeCrAl alloy has good comprehensive performance and extremely excellent steam oxidation resistance, so that the FeCrAl alloy is separated from other candidate accident-resistant cladding materials. At present, the preparation processes of FeCrAl-based alloy are mostly reported to be a vacuum melting-forging-hot rolling-normalizing-tempering process and a ball-milling powder mixing-SPS sintering (-forging) process, and although the preparation processes are mature, the mechanical properties of the prepared alloy need to be further improved. For example, the invention patent CN111809119A discloses a dispersion strengthening FeCrAl alloy material, which utilizes the ball-milling powder mixing-SPS sintering-forging process to prepare FeCrAl alloy with good processing property and stable structure, but the mechanical property of the FeCrAl alloy is required to be further improved.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a high-strength FeCrAl-based alloy which is prepared by adopting a process of mechanical alloying ball-milling powder mixing, discharge plasma sintering, equal channel angular extrusion, and has the advantages of simple preparation process, low cost and excellent comprehensive mechanical property.
A high-strength FeCrAl-base alloy is prepared from FeCrAl alloy powder, nano-ZrC and nano-ZrH2The powder is firstly subjected to mechanical alloying ball milling treatment, then is subjected to discharge plasma sintering forming to obtain an ingot, and finally is subjected to equal channel angular pressing treatment to obtain the product.
Preferably, the annealing treatment is carried out after 1 pass of equal channel angular pressing is carried out on the cast ingot.
In the invention, the sample after extrusion is annealed to reduce the internal stress caused by large extrusion deformation.
Preferably, the process parameters of the annealing treatment are as follows: annealing at 600-750 deg.C for 40-80 min.
Preferably, the equal channel angular pressing treatment is pressing by adopting a C path; the extrusion was carried out using extrusion dies having an intersection angle of 90 °.
The C path refers to that the sample rotates 180 degrees around the extrusion direction after each extrusion and then carries out the next extrusion.
Preferably, the chemical composition of the FeCrAl alloy powder comprises the following components in percentage by weight: 12.5-13% of Cr, 3.6-4.0% of Al, 1.5-1.7% of Mo, less than or equal to 0.015% of P, less than or equal to 0.015% of S, less than or equal to 0.02% of O, less than or equal to 0.015% of N, and the balance of iron and impurities.
Preferably, the addition amount m of the nano ZrC powderZrCAnd weight m of FeCrAl alloy powderFeCrAlThe relationship between them is: m isZrC/mFeCrAl＝0.5～1.0wt.％。
Preferably, the nano ZrH2Amount of powder added mZrH2And weight m of FeCrAl alloy powderFeCrAlThe relationship between them is: m isZrH2/mFeCrAl≤1.0wt.％。
Preferably, the ball milling treatment is dry milling in an inert atmosphere; the ball milling time is 18-22 h, and the ball-to-material ratio is 11-13: 1, the ball milling speed is 250-350 r/min.
Preferably, the spark plasma sintering is sintering in an argon atmosphere containing a small amount of hydrogen, and the volume percentage of hydrogen to argon is 3: 97.
has the advantages that: according to the principle of the effect of dispersion strengthening and grain boundary purification on the improvement of the performance of a metal material, in order to improve the comprehensive performance, particularly the elongation and the strength of FeCrAl, a nano-sized high-hardness phase ZrC is dispersed and distributed at the grain boundary and in the grain of FeCrAl, and the strength of FeCrAl is improved through the regulation and control of the phase boundary and the grain boundary; meanwhile, in order to improve the plastic deformation capability of FeCrAl-ZrC, ZrH is utilized2The grain boundary purification effect during the formation of metal Zr and zirconium compounds is used for improving the elongation. In addition, an Equal Channel Angular Pressing (ECAP) process is introduced after spark plasma sintering, and FeCrAl-ZrC-ZrH is further improved through large plastic deformation2The comprehensive mechanical property of (2); and annealing the extruded sample to reduce the internal stress caused by large extrusion deformation.
Drawings
FIG. 1 is a SEM of raw material powder and the corresponding size fraction in the example of the present inventionLaying out a layout; wherein, (a) FeCrAl, (b) ZrC and (c) ZrH2；
FIG. 2 is a representation of FeCrAl +1 wt.% ZrC +0.2 wt.% ZrH prepared in an example of the present invention2A comparison graph of mechanical properties of the alloy before and after equal channel angular extrusion treatment; wherein (a) ultimate tensile strength at room temperature, and (b) elongation.
Detailed Description
The chemical components of the FeCrAl alloy powder used in the following examples were Cr 12.71%, Al 3.7%, Mo 1.63%, P0.01%, S0.003%, O0.019%, N0.005%, and the balance iron and impurities; the average size of the particles was about 16.5um, and the morphology of the particles was as shown in FIG. 1 (a).
The average particle size of the nano ZrC powder used in the following examples is about 20.1nm, and the morphology of the particles is shown in FIG. 1 (b); nanometer ZrH2The particle size of the powder is bimodal, the large particle size is mainly 4-6 μm, the small particle size is mainly 0.5-1 μm, and the particle morphology is shown in FIG. 1 (c).
The technical solution of the present invention will be described in detail below with reference to specific examples.
Examples
Preparation of FeCrAl +1 wt.% ZrC +0.2 wt.% ZrH2Alloy (I)
S1, weighing 79.04g of FeCrAl alloy powder, 0.8g of nano ZrC powder and 0.16g of ZrH2Adding the mixture into a ball milling tank, carrying out 3 times of gas washing on the ball milling tank by using Ar gas, finally filling the ball milling tank with the Ar gas and keeping micro-positive pressure, and then carrying out dry milling in a horizontal planetary ball mill, wherein the ball milling parameters are set as ball-material ratio of 12: 1, the rotating speed is 300r/min, the ball milling is stopped for 20min after 60min, the ball milling time is 20h, and the nano ZrH is obtained2Fully and uniformly mechanically alloying ZrC and FeCrAl alloy powder, and taking out mixed powder in a ball milling tank after ball milling; the spherical FeCrAl is seriously deformed, ZrC and ZrH after the mechanized ball milling2The particles are embedded in the FeCrAl or attached to the surface of the FeCrAl.
S2, pouring the mixed powder into a graphite mold with the diameter of phi 90mm (the size of the graphite mold can be designed according to the requirement in the specific implementation), and discharging in a discharge plasma sintering devicePlasma sintering to obtain FeCrAl alloy powder and ZrH2Further alloying the nano ZrC powder to obtain an ingot;
FeCrAl +1 wt.% ZrC +0.2 wt.% ZrH formed by spark plasma sintering in S2 was measured2The alloy had a hardness of 296.1Hv, an Ultimate Tensile Strength (UTS) of about 850MPa at room temperature, and an Elongation (Elongation) of about 18%.
S3, cutting the cast ingot into round bars with the diameter of 10 x 60mm, then carrying out ECAP extrusion treatment on an equal channel angular extrusion die according to a route C (namely, after each extrusion, the sample rotates 180 degrees around the extrusion direction and then carries out the next extrusion), wherein the intersection angle of the extrusion die is 90 degrees, the extruded sample is annealed at 700 ℃ for 1h in a heating furnace to reduce the internal stress caused by large extrusion deformation, the annealing treatment is carried out after each 1-time equal channel angular extrusion of the cast ingot, the extrusion-annealing operation is repeated, and the equal channel angular extrusion treatment is carried out on the cast ingot for 2 times.
FeCrAl +1 wt.% ZrC +0.2 wt.% ZrH after equal channel angular pressing in S3 was measured2The hardness of the alloy is about 350Hv, the Ultimate Tensile Strength (UTS) at room temperature is about 1250MPa, and the Elongation (Elongation) is about 12%. The mechanical properties of the alloys obtained in S2 and S3 are compared with those of FIG. 2, and the data show that the tensile strength of the alloy is remarkably increased by introducing an ECAP or other channel angular pressing process after SPS sintering.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A high-strength FeCrAl-base alloy is prepared from FeCrAl alloy powder, nano-ZrC and nano-ZrH2The powder is firstly subjected to mechanical alloying ball milling treatment, then is subjected to discharge plasma sintering forming to obtain an ingot, and finally is subjected to equal channel angular pressing treatment to obtain the product.
2. The high strength FeCrAl-based alloy of claim 1, wherein the ingot is annealed after each 1 pass of equal channel angular extrusion.
3. A high strength FeCrAl-based alloy according to claim 2, wherein the process parameters of the annealing treatment are: annealing at 600-750 deg.C for 40-80 min.
4. A high strength FeCrAl-based alloy according to any of claims 1-3, wherein the equal channel angular pressing process is pressing using a C-path; the extrusion was carried out using extrusion dies having an intersection angle of 90 °.
5. A high strength FeCrAl-based alloy according to claim 1, characterized in that the chemical composition of the FeCrAl alloy powder comprises, in weight percent: 12.5-13% of Cr, 3.6-4.0% of Al, 1.5-1.7% of Mo, less than or equal to 0.015% of P, less than or equal to 0.015% of S, less than or equal to 0.02% of O, less than or equal to 0.015% of N, and the balance of iron and impurities.
6. The high strength FeCrAl-based alloy as claimed in claim 1, wherein the nano ZrC powder is added in an amount mZrCAnd weight m of FeCrAl alloy powderFeCrAlThe relationship between them is: m isZrC/mFeCrAl＝0.5～1.0％。
7. The high strength FeCrAl-based alloy of claim 1, wherein the nano ZrH2Amount of powder added mZrH2And weight m of FeCrAl alloy powderFeCrAlThe relationship between them is: m isZrH2/mFeCrAl≤1.0％。
8. The high strength FeCrAl-based alloy of claim 1 wherein the ball milling process is dry milling in an inert atmosphere; the ball milling time is 18-22 h, and the ball-to-material ratio is 11-13: 1, the ball milling speed is 250-350 r/min.
9. A high strength FeCrAl-based alloy according to claim 1, wherein the spark plasma sintering is sintering in an argon atmosphere containing a small amount of hydrogen, the volume percentage of hydrogen and argon being 3: 97.
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| CN115896589A (en) * | 2022-11-04 | 2023-04-04 | 苏州热工研究院有限公司 | Oxide dispersion strengthening FeCrAl alloy and preparation method and application thereof |
| CN115971011A (en) * | 2022-11-28 | 2023-04-18 | 中国科学院合肥物质科学研究院 | High-entropy composite oxide hydrogen-resistant coating and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114951691A (en) * | 2022-03-28 | 2022-08-30 | 上海大学 | Laser additive manufacturing method of ZrC particle reinforced FeCrAl metal matrix composite material for nuclear fuel cladding |
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| CN115896589B (en) * | 2022-11-04 | 2024-04-05 | 苏州热工研究院有限公司 | Oxide dispersion strengthening FeCrAl alloy and preparation method and application thereof |
| CN115971011A (en) * | 2022-11-28 | 2023-04-18 | 中国科学院合肥物质科学研究院 | High-entropy composite oxide hydrogen-resistant coating and preparation method thereof |
| CN115971011B (en) * | 2022-11-28 | 2023-12-08 | 中国科学院合肥物质科学研究院 | High-entropy composite oxide hydrogen-resistant coating and preparation method thereof |
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