CN115074601A - Method for preparing high volume fraction B2 strengthened ferrite alloy - Google Patents
Method for preparing high volume fraction B2 strengthened ferrite alloy Download PDFInfo
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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
- C22C33/04—Making ferrous alloys by melting
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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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/18—Hardening; Quenching with or without subsequent tempering
-
- 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
- C21D8/005—Modifying the physical properties by deformation combined with, or followed by, heat treatment of ferrous alloys
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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
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/005—Ferrite
Abstract
The invention belongs to the field of preparation research of high-performance metal materials, and particularly provides a method for preparing a high-volume-fraction B2 strengthened ferrite alloy. The method comprises the following steps: s1) obtaining an alloy ingot by adopting a vacuum melting mode; s2) carrying out homogenization heat treatment on the alloy ingot obtained in the step S1); s3) carrying out thermal deformation treatment on the alloy ingot processed by the S2); to regulate the grain structure and induce the formation of B2 phase partially unqualified with ferrite matrix; s4) carrying out solution and aging heat treatment on the deformation sample obtained in S3) to obtain a ferrite alloy with the volume fraction of B2 phase in the alloy being more than 30%. The elongation before room temperature tensile fracture is more than 15 percent. The method has the advantages of simple process and low cost, and is a method for efficiently preparing the B2 reinforced ferrite alloy with good plasticity.
Description
Technical Field
The invention belongs to the field of preparation research of high-performance metal materials, and particularly provides a method for preparing a high-volume-fraction B2 strengthened ferrite alloy.
Background
The ferrite alloy has lower density, excellent mechanical property, good oxidation resistance, higher heat conductivity coefficient and lower cost, so the ferrite alloy is widely applied to the fields of automobile industry, electric power industry, aerospace, nuclear industry and the like. Precipitation strengthening is the most important strengthening mechanism of high-strength alloy, is realized by particle dispersion generating dislocation movement disorder, and the size and volume fraction of grains of precipitated phases and the size and distribution of gaps among precipitated phases have important influence on the performance of the alloy in the aging process. Generally, the higher the volume fraction of the precipitation strengthening phase, the more uniform the particle size distribution, and the better the strengthening effect. The precipitation of the precipitated phase belongs to a solid phase change process, the precipitated phase and a matrix can generate new interface energy of the interface lifting material in the nucleation process, meanwhile, the precipitated phase and the matrix generally have structural difference, and the nucleation process can improve the strain energy of the material. The greater the interfacial energy and strain energy increases, meaning the greater the resistance of the precipitate phase during nucleation. Too much resistance to precipitate phase precipitation leads to difficult nucleation, and finally leads to low volume fraction of the precipitated phase and large particle size. Therefore, in order to obtain a further enhanced effect, a precipitated phase having the same structure as the matrix and a similar lattice constant is generally selected for enhancement. The ferrite matrix is of a body-centered cubic (bcc) structure, the lattice structure constant is 0.28665nm, the B2 phase is a CsCl type crystal structure, the structure is similar to that of ferrite, the lattice structure constant is 0.28864nm, and the lattice mismatching degree of the two phases is 0.69%, which means that the B2 phase can be uniformly and dispersedly precipitated in the alpha-Fe in a manner of coherent precipitation.
The development of modern industry places higher demands on the performance of ferritic alloys, and particularly the introduction of a high volume fraction of B2 strengthening phase into ferritic alloys used under extreme conditions such as high temperature. However, the introduction of the high volume fraction of the B2 strengthening phase results in a ferritic alloy susceptible to brittle fracture at room temperature. A series of B2 strengthened ferritic alloys (designated FBB series alloys) were developed by p.k.liaw of tennessee university, m.e.fine and g.ghosh of northwestern university, m.d.asta of california university and c.t.liu of hong kong city university. The development of such alloys has been aimed at obtaining ferritic based superalloys with a similar microstructure to nickel based superalloys, which can be used at medium and high temperatures. However, the results of the research show that the bending plasticity of the alloy is lower than 1% when the volume fraction of the B2 strengthening phase is more than 15%, which greatly limits the application of the high volume fraction B2 strengthening ferrite alloy.
Disclosure of Invention
In view of the above problems, the present invention provides a method for manufacturing a high volume fraction B2 phase content ferritic alloy, which solves any of the above and other potential problems of the prior art.
In order to achieve the purpose, the technical scheme of the invention is as follows: a method for processing and preparing a high volume fraction B2 phase content ferrite alloy comprises the following steps:
s1) obtaining an alloy ingot by adopting a vacuum melting mode;
s2) carrying out homogenization heat treatment on the alloy ingot obtained in the step S1);
s3) carrying out thermal deformation treatment on the alloy ingot processed by the S2); to regulate the grain structure and induce the formation of B2 phase partially unqualified with ferrite matrix;
s4) carrying out solution and aging heat treatment on the deformation sample obtained in S3) to obtain a ferrite alloy with the volume fraction of B2 phase in the alloy being more than 30%.
Furthermore, the B2 phase in the alloy is uniformly dispersed in a ferrite matrix, and the elongation before room temperature stretch breaking is more than 15%.
Further, the specific steps of S1) are:
s1.1) weighing each metal raw material with the purity of 99.99% according to a design group for later use;
s1.2) placing the metal raw materials weighed in the S1.2) into a copper crucible of a vacuum smelting furnace, placing pure Ti particles into the copper crucible to serve as an oxygen absorbent in the smelting process, and smelting for 5-7 times to obtain an alloy ingot.
Further, the alloy ingot in the step S1) comprises the following components in percentage by mass: cr 9-16 wt.%, Ni10-14 wt.%, Co10-14 wt.%, Al4-8 wt.%, Mo 0-2 wt.%, Zr 0-2 wt.%, Hf 0-2 wt.%, the balance being Fe and unavoidable impurities.
Further, the mass percentages of the components of the alloy ingot in the S1) are as follows: 10-12% of Cr, 78-13% of Ni11, 11.5-13% of Co11, 4.5-6% of Al4, 0-2.0% of Mo, 0-1.5% of Zr, 0-1.5% of Hf, and the balance of Fe element and inevitable impurities.
Further, the specific process parameters of the homogenization treatment in S2) are as follows:
the homogenization temperature is 1100-.
Further, the process parameters of the thermal deformation treatment in S3) are:
when the thermal deformation adopts rolling, the rolling temperature is 600-1000 ℃, the heat preservation time before rolling is 0.5-2 hours, the single deformation is 10-20%, the annealing is carried out for 5-20 minutes after the single rolling deformation, the total deformation is 30-80%, and the cooling mode after rolling is air cooling.
Further, the process parameters of the thermal deformation treatment in S3) are:
when the thermal deformation is extrusion, the extrusion temperature is 600-1000 ℃, the heat preservation time before extrusion is 0.5-2 hours, and the extrusion ratio is 16-50.
Further, the technological parameters of the solution and aging heat treatment in the step S4) are as follows:
the temperature of the solution heat treatment is 850-1200 ℃, the heat preservation time is 0.5-2 hours, and the cooling medium is air;
the ageing heat treatment temperature is 500-800 ℃, the heat preservation time is 0.5-480 hours, and the cooling medium is air.
A high-volume-fraction B2 reinforced ferrite alloy is prepared by the method.
The invention provides a processing and preparation method of a high volume fraction B2 phase content ferrite alloy, wherein the volume fraction of a B2 phase in the alloy is more than 30%, and the elongation before room temperature tensile fracture resistance is more than 15%.
The vacuum melting mode specifically comprises the following steps: preparing metal raw materials with the purity of 99.9 percent or more, scrubbing a copper crucible and a tungsten electrode tip of a vacuum smelting furnace, weighing the metal raw materials according to alloy components, putting the metal raw materials into a water-cooled copper crucible, and putting pure Ti particles into an empty copper crucible to be used as an oxygen absorbent in the smelting process. The working cavity of the vacuum melting furnace is vacuumized to 5 multiplied by 10 -1 Pa to form low vacuum, and continuously vacuumizing the molecular pump to make the pressure reach 5 × 10 -3 And Pa, closing the molecular pump, and repeatedly washing the furnace chamber with argon for three times to ensure that the sample melting is carried out under the conditions of high vacuum and argon protection. After the arc is started, the tungsten electrode head is aligned with pure Ti particles for smelting for 1min, oxygen in a hearth is consumed, and the vacuum degree is improved. And aligning the tungsten electrode head to the center of the sample, adjusting the current in the process to control the smelting state of the sample, moving the tungsten electrode to the next copper crucible for smelting after the smelting is finished, turning the sample by using a mechanical arm after all the samples are subjected to initial smelting for 5min, smelting again, and obtaining the alloy ingot after ensuring that the smelting is carried out for 5-7 times. b. Homogenizing an alloy sample: cutting the obtained alloy cast ingot into a required shape according to requirements, polishing the surface of a cut sample, cleaning to remove impurities, heating the metal piece with the treated surface to a certain temperature, preserving the temperature for a period of time, carrying out homogenization heat treatment, polishing the surface of the sample to be bright after the homogenization treatment, and cleaning.
The invention has the advantages that:
1. the volume fraction of the ferrite alloy B2 phase obtained in the invention is more than 30%, and the phase is uniformly dispersed in a ferrite matrix.
2. The B2 reinforced ferrite alloy prepared by the invention has excellent room temperature tensile plasticity, the elongation before fracture exceeds 15%, and the strength and the plasticity can be adjusted by a heat treatment process.
3. The method has simple process and low cost, and is a method for preparing the B2 phase reinforced ferrite alloy with high volume fraction by high-efficiency processing.
Description of the drawings:
FIG. 1 is a flow chart of the present invention.
Fig. 2 is an XRD pattern of a typical ferritic alloy obtained in accordance with the present invention, showing only ferritic and B2 phases in the alloy.
Fig. 3 is an SEM image of precipitated phases of a typical ferritic alloy obtained according to the present invention, and it can be seen that a large amount of nano-sized B2 precipitated phases are present in the matrix, and combined with the XRD refinement results, the volume fraction of B2 phase is confirmed to be greater than 35%.
FIG. 4 is a room temperature tensile curve of a typical ferritic alloy obtained in accordance with the present invention, from which it can be seen that the alloy has good room temperature tensile plasticity with a pre-fracture elongation of more than 25%.
The specific implementation mode is as follows:
the technical solution of the present invention is further explained with reference to the accompanying drawings and specific embodiments.
As shown in FIG. 1, the invention relates to a method for processing and preparing a high volume fraction B2 phase content ferrite alloy, which comprises the following steps:
s1) obtaining an alloy ingot by adopting a vacuum melting mode;
s2) carrying out homogenization heat treatment on the alloy ingot obtained in the step S1), and cooling to room temperature;
s3) carrying out thermal deformation treatment on the alloy ingot processed by the S2), cooling to obtain a deformation sample so as to regulate and control the crystal grain structure and induce to form a B2 phase partially unqualified with the ferrite matrix;
s4) carrying out solution and aging heat treatment on the deformation sample obtained in S3) to obtain a ferrite alloy with the volume fraction of B2 phase in the alloy being more than 30%.
The B2 phase in the alloy is uniformly dispersed in a ferrite matrix, and the elongation before room temperature stretch-breaking resistance is more than 15%.
The S1) comprises the following specific steps:
s1.1) weighing each metal raw material with the purity of 99.99% according to a design group for later use;
s1.2) placing the metal raw materials weighed in the S1.2) into a copper crucible of a vacuum smelting furnace, placing pure Ti particles into the copper crucible to serve as an oxygen absorbent in the smelting process, and smelting for 5-7 times to obtain an alloy ingot.
The alloy ingot in the S1) comprises the following components in percentage by mass: 9-16% of Cr, 78-14% of Ni10, 10-14% of Co, 4-8% of Al, 0-2% of Mo, 0-2% of Zr, 0-2% of Hf, and the balance of Fe and inevitable impurities.
The mass percentages of the components of the alloy ingot in the S1) are as follows: 10-12% of Cr, 78-13% of Ni11, 5-13% of Co11.5, 4.5-6% of Al, 0-2.0% of Mo, 0-1.5% of Zr, 0-1.5% of Hf, and the balance of Fe element and inevitable impurities.
The specific process parameters of the homogenizing treatment of S2) are as follows:
the homogenization temperature is 1100-1250 ℃, the heat preservation time is 1-4 hours, and the cooling medium is air.
The process parameters of the thermal deformation treatment in S3) are as follows:
when the thermal deformation adopts rolling, the rolling temperature is 600-1000 ℃, the heat preservation time before rolling is 0.5-2 hours, the single deformation is 10-20%, the annealing is carried out for 5-20 minutes after the single rolling deformation, the total deformation is 30-80%, and the cooling mode after rolling is air cooling.
The process parameters of the thermal deformation treatment in S3) are as follows:
when the thermal deformation is extrusion, the extrusion temperature is 600-1000 ℃, the heat preservation time before extrusion is 0.5-2 hours, and the extrusion ratio is 16-50.
The technological parameters of the solid solution and aging heat treatment in the S4) are as follows:
the temperature of the solution heat treatment is 850-;
the temperature of the aging heat treatment is 500-.
A high-volume-fraction B2 reinforced ferrite alloy is prepared by the method.
Example 1: preparation of an alloy with the composition of Fe-12 wt.% Cr-4 wt.% Al-12 wt.% Co-10 wt.% Ni-1.5 wt.% Mo
Preparing high-purity metal raw materials, putting the high-purity metal raw materials into a vacuum smelting furnace for smelting, and repeatedly smelting for 5 times to obtain an alloy ingot, wherein the alloy comprises the components of Fe, 12 wt.% of Cr, 4 wt.% of Al, 12 wt.% of Co, 10 wt.% of Ni and 1.5 wt.% of Mo. And (3) preserving the temperature of the alloy ingot at 1100 ℃ for 2 hours, and cooling the alloy ingot in air to finish homogenization treatment. And (3) carrying out hot rolling treatment on the homogenized sample, wherein the rolling temperature is 800 ℃, the heat preservation time before rolling is 1 hour, the single deformation amount of rolling is 10%, annealing is carried out for 5 minutes after the single rolling deformation, the total deformation amount is 50%, and air cooling is carried out after the rolling is finished to obtain the deformed sample. The deformed sample was solution treated at 870 ℃ for 0.5 hour for air cooling and then aged at 550 ℃ for 128 hours to obtain an alloy with the composition Fe-12 wt.% Cr-4 wt.% Al-12 wt.% Co-10 wt.% Ni-1.5 wt.% Mo.
Example 2: preparation of an alloy with the composition of Fe-11 wt.% Cr-5 wt.% Al-12 wt.% Co-12 wt.% Ni-2 wt.% Mo
Preparing a high-purity metal raw material, putting the high-purity metal raw material into a vacuum smelting furnace for smelting, and repeatedly smelting for 7 times to obtain an alloy ingot, wherein the alloy comprises the components of Fe, 11 wt.% Cr, 5 wt.% Al, 12 wt.% Co, 12 wt.% Ni and 2 wt.% Mo. And (3) preserving the heat of the alloy ingot at 1150 ℃ for 2 hours, and cooling the alloy ingot in air to finish homogenization treatment. And (3) carrying out hot rolling treatment on the homogenized sample, wherein the rolling temperature is 900 ℃, the heat preservation time before rolling is 1 hour, the single deformation amount of rolling is 20%, annealing is carried out for 10 minutes after the single rolling deformation, the total deformation amount is 80%, and air cooling is carried out after the rolling is finished to obtain a deformed sample. The deformed sample was solution treated at 900 ℃ for 0.5 hour of air cooling and then aged at 700 ℃ for 480 hours to obtain an alloy with the composition Fe-11 wt.% Cr-5 wt.% Al-12 wt.% Co-12 wt.% Ni-2 wt.% Mo. The X-ray diffraction analysis chart of the alloy is shown in fig. 2, the SEM chart of the precipitated phase is shown in fig. 3, and the room temperature tensile curve is shown in fig. 4.
Example 3: preparation of an alloy with the composition Fe-14 wt.% Cr-6 wt.% Al-14 wt.% Co-14 wt.% Ni-2 wt.% Mo-0.1Zr
Preparing a high-purity metal raw material, putting the high-purity metal raw material into a vacuum smelting furnace for smelting, and repeatedly smelting for 5 times to obtain an alloy ingot, wherein the alloy comprises the components of Fe, 10 wt.% of Cr, 4 wt.% of Al, 10 wt.% of Co, 13 wt.% of Ni, 2 wt.% of Mo and 0.1 Zr. And (3) preserving the heat of the alloy cast ingot for 3 hours at 1200 ℃, and cooling in air to finish homogenization treatment. And (3) carrying out hot extrusion treatment on the homogenized sample, wherein the hot extrusion temperature is 1000 ℃, the heat preservation time before extrusion is 2 hours, the extrusion ratio is 32, and air cooling is carried out after extrusion to obtain a deformed sample. The deformed sample was solution treated at 950 ℃ for 1 hour for air cooling and then aged at 700 ℃ for 64 hours to obtain an alloy with the composition Fe-14 wt.% Cr-6 wt.% Al-14 wt.% Co-14 wt.% Ni-2 wt.% Mo-0.1 Zr.
Example 4: preparation of an alloy with the composition of Fe-10 wt.% Cr-6 wt.% Al-12.5 wt.% Co-12.5 wt.% Ni-1 wt.% Mo
Preparing high-purity metal raw materials, putting the high-purity metal raw materials into a vacuum smelting furnace for smelting, and repeatedly smelting for 5 times to obtain an alloy ingot, wherein the alloy comprises the components of Fe, 10 wt.% of Cr, 6 wt.% of Al, 12.5 wt.% of Co, 12.5 wt.% of Ni and 1 wt.% of Mo. And (3) preserving the heat of the alloy cast ingot for 1 hour at 1050 ℃, and cooling in air to finish homogenization treatment. And (3) carrying out hot rolling treatment on the homogenized sample, wherein the rolling temperature is 700 ℃, the heat preservation time before rolling is 0.5 hour, the single deformation amount of rolling is 15%, annealing is carried out for 5 minutes after single rolling deformation, the total deformation amount is 60%, and air cooling is carried out after rolling is finished to obtain the deformed sample. The deformed sample was solution treated at 800 ℃ for 1 hour for air cooling and then aged at 750 ℃ for 32 hours to obtain an alloy with the composition Fe-10 wt.% Cr-6 wt.% Al-12.5 wt.% Co-12.5 wt.% Ni-1 wt.% Mo.
The inventor proposes a method for processing and preparing a high volume fraction B2 reinforced ferrite alloy. The method mainly comprises the steps of obtaining an as-cast alloy by vacuum melting, carrying out thermal deformation processing on the as-cast alloy under certain process conditions after carrying out homogenization treatment, carrying out solid solution aging heat treatment on the alloy after thermal deformation treatment to finally obtain a ferrite alloy with the phase volume fraction of B2 being more than 30% and the elongation percentage being more than 15% before room temperature stretch breaking, and regulating the phase composition and the phase transition temperature of the alloy by controlling the distribution ratio of a control group.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions and substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (10)
1. A method of making a high volume fraction B2 phase strengthened ferritic alloy, characterized in that the method comprises the steps of, in order:
s1) obtaining an alloy ingot by adopting a vacuum melting mode;
s2) carrying out homogenization heat treatment on the alloy ingot obtained in the step S1), and cooling to room temperature;
s3) carrying out thermal deformation treatment on the alloy ingot processed by the S2) to obtain a deformation sample;
s4) carrying out solution and aging heat treatment on the deformation sample obtained in S3) to obtain a ferrite alloy with the volume fraction of B2 phase in the alloy being more than 30%.
2. The method of claim 1, wherein the alloy has B2 phase uniformly dispersed in a ferritic matrix and a room temperature elongation before stretch-breaking of greater than 15%.
3. The method as claimed in claim 1, wherein the specific steps of S1) are:
s1.1) weighing each metal raw material with the purity of 99.99% according to a design group for later use;
s1.2) placing the metal raw materials weighed in the S1.2) into a copper crucible of a vacuum smelting furnace, placing pure Ti particles into the copper crucible to serve as an oxygen absorbent in the smelting process, and smelting for 5-7 times to obtain an alloy ingot.
4. The method as claimed in claim 1, wherein the alloy ingot in S1) comprises the following components in percentage by mass: 9-16% of Cr, 10-14% of Ni, 10-14% of Co, 4-8% of Al, 0-2.0% of Mo, 0-2.0% of Zr, 0-2.0% of Hf, and the balance of Fe and inevitable impurities.
5. The method as claimed in claim 1, wherein the alloy ingot in S1) comprises the following components in percentage by mass: 10-12% of Cr, 11-13% of Ni, 11.5-13% of Co, 4.5-6% of Al, 0-2.0% of Mo, 0-1.5% of Zr, 0-1.5% of Hf, and the balance of Fe element and inevitable impurities.
6. The method as claimed in claim 1, wherein the specific process parameters of the homogenization treatment in the step S2) are as follows:
the homogenization temperature is 1100-.
7. The method as claimed in claim 1, wherein the process parameters of the hot deformation process in S3) are:
when the thermal deformation adopts rolling, the rolling temperature is 600-1000 ℃, the heat preservation time before rolling is 0.5-2 hours, the single deformation is 10-20%, the annealing is carried out for 5-20 minutes after the single rolling deformation, the total deformation is 30-80%, and the cooling mode after rolling is air cooling.
8. The method as claimed in claim 1, wherein the process parameters of the hot deformation process in S3) are:
when the thermal deformation is extrusion, the extrusion temperature is 600-1000 ℃, the heat preservation time before extrusion is 0.5-2 hours, and the extrusion ratio is 16-50.
9. The method according to claim 1, wherein the process parameters of the solution and aging heat treatment in S4) are:
the temperature of the solution heat treatment is 850-;
the temperature of the aging heat treatment is 500-.
10. A high volume fraction B2 strengthened ferritic alloy, characterized in that the high volume fraction B2 strengthened ferritic alloy is produced with the method according to any of claims 1-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202210571161.0A CN115074601B (en) | 2022-05-24 | 2022-05-24 | Method for preparing high volume fraction B2 reinforced ferrite alloy |
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| CN115627405A (en) * | 2022-10-21 | 2023-01-20 | 中国科学院金属研究所 | High-entropy alloy resistant to liquid lead and bismuth corrosion and preparation method thereof |
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