CN113308644B - Iron-chromium-aluminum alloy material for improving high-temperature comprehensive performance by using vanadium-rare earth synergy and preparation method thereof - Google Patents
Iron-chromium-aluminum alloy material for improving high-temperature comprehensive performance by using vanadium-rare earth synergy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an iron-chromium-aluminum alloy material for improving high-temperature comprehensive performance by using vanadium-rare earth synergy and a preparation method thereof, wherein the iron-chromium-aluminum alloy material has excellent high-temperature strength and high-temperature oxidation resistance, and comprises the following components in percentage by mass: less than or equal to 0.05 percent of C, less than or equal to 0.14 percent of Si, less than or equal to 0.2 percent of Mn, less than or equal to 0.06 percent of S, less than or equal to 0.01 percent of P, V: 0.5-0.8%, La: 0.1-0.15%, Cr: 21-23%, Al: 5-6% and the balance of Fe. The manufacturing method comprises the following steps: and preparing the element powder according to the mass percentage, performing ball milling in a high-energy ball mill under the protection of argon to obtain mixed powder, then putting the mixed powder into a graphite die, and performing hot-pressing sintering molding in a vacuum hot-pressing furnace to obtain the FeCrAl-V-La alloy with excellent high-temperature comprehensive performance. The high-temperature strength and the high-temperature oxidation resistance of the FeCrAl-V-La alloy prepared by the invention are obviously improved, and particularly, the high-temperature yield strength of the FeCrAl-V-La alloy is 135.8MPa, and the rapid oxidation life value of the FeCrAl-V-La alloy at 1350 ℃ is 83 h. Compared with the similar iron-chromium-aluminum alloy, the material prepared by the invention has the advantages of lower production cost, longer service life, less environmental pollution and good economic benefit.
Description
Technical Field
The invention belongs to the technical field of iron-chromium-aluminum alloy materials, and particularly relates to an iron-chromium-aluminum alloy material for improving high-temperature comprehensive performance by using vanadium and rare earth in a synergistic manner and a preparation method thereof.
Background
The FeCrAl alloy is an important electrothermal alloy, has the advantages of high heat resistance, thermal conductivity, excellent high-temperature oxidation resistance and the like, and is lower in price by 20-30% than Ni-Cr electrothermal alloy materials. Therefore, the excellent performance and the low price of the FeCrAl alloy provide favorable conditions for market demands, and the FeCrAl alloy is widely applied to industries such as electric heating elements, precision instruments, chemical containers and the like.
At present, the preparation of FeCrAl alloy generally adopts an electroslag remelting or vacuum induction melting method. The process control difficulty in the electroslag remelting process is high, cracks are easily generated in the cast ingot, the mechanical property of the material is seriously influenced, the power consumption of the method is high, the cost is high, and the slag is easy to pollute the environment in the remelting process. The cast ingot prepared by vacuum induction melting is easy to have the defects of looseness, shrinkage cavity and the like, and is not beneficial to the subsequent hot working. Therefore, the development of a preparation process which is efficient, low-cost and meets the material uniformity becomes a hot point of research. The FeCrAl electrothermal alloy prepared by powder metallurgy makes up the defect that the traditional process cannot eliminate, and as one of advanced manufacturing processes, the FeCrAl electrothermal alloy not only enhances the high-temperature strength, the high-temperature oxidation resistance and the medium corrosion resistance, but also can obtain better processing performance and reduce the possibility of coarse grains. The powder metallurgy method is the focus of the research of the FeCrAl alloy at present, is one of the development directions of the preparation of the electrothermal alloy, and is very likely to replace the current smelting method.
The FeCrAl alloy has excellent high-temperature oxidation resistance mainly because Al can be selectively formed on the surface2O3The film, however, gradually peels off and fails as the Al content in the matrix is consumed. The addition of a proper amount of rare earth elements La, Ce and Y into the FeCrAl alloy can reduce the growth rate of the oxide film, improve the strength and plasticity of the oxide film and enhance the compactness and adhesive force of the oxide film, thereby improving the oxidation resistance of the alloy. In addition, the FeCrAl alloy has low high-temperature strength, is easy to generate creep deformation, has poor plastic toughness, and is easy to coarsen crystal grains during high-temperature work and brittle fracture under the action of stress. By adding Nb, Mo, V, Ti and other refractory metal elements into the FeCrAl alloy, the high-temperature strength of the alloy can be improved, and the processing performance is improved. Thus, FeCrAl alloy is consideredThe rare earth element and the refractory metal element with proper content are simultaneously added into the gold, so that under the complex service working condition, the high-temperature oxidation resistance and the high-temperature strength performance of the FeCrAl alloy are simultaneously improved, the service life of the alloy is prolonged, and the rare earth value is more effectively exerted.
The domestic research on the rare earth FeCrAl alloy mainly focuses on the aspects of the action and mechanism of La, Ce, Y and mixed rare earth in cast iron alloy, and the research on the action and mechanism of rare earth elements in powder metallurgy FeCrAl alloy is less. Moreover, the research on the action rules of the rare earth elements and the refractory metals in the powder metallurgy technology is less, and the powder metallurgy has wide application prospects in specific fields, so that the research on the action of the rare earth elements and the refractory metals in the powder metallurgy FeCrAl alloy is necessary.
Disclosure of Invention
The invention aims to provide a FeCrAl alloy material with excellent high-temperature comprehensive performance and high economy, which improves the high-temperature oxidation resistance of the alloy by adding a proper amount of La and improves the high-temperature strength performance of the alloy by adding a proper amount of V.
The FeCrAl alloy comprises the following chemical components in percentage by mass: less than or equal to 0.05 percent of C, less than or equal to 0.14 percent of Si, less than or equal to 0.2 percent of Mn, less than or equal to 0.06 percent of S, less than or equal to 0.01 percent of P, V: 0.5-0.8%, La: 0.1-0.15%, Cr: 21-23%, Al: 5-6% and the balance Fe.
The original powder adopts vanadium powder, lanthanum powder, chromium powder, aluminum powder and iron powder, and the purity of each metal powder is higher than 99%.
The effects of V and La are as follows:
v: can form fine and dispersed carbide in the FeCrAl alloy, plays a role in precipitation strengthening on a matrix, simultaneously prevents the growth of crystal grains, plays a role in refining the crystal grains, and improves the high-temperature strength of the FeCrAl alloy. However, since excessive V coarsens carbide, the content is preferably 0.5 to 0.8%.
La: the trace addition of La can refine the crystal grains by 1-2 levels, reduce the inclusion by 0.5-1 level, improve the yield by more than 10%, has a quick service life value 1 time higher than that of the alloy without rare earth, can capture carbon and nitride particles, reduce the precipitation of carbonitride, improve the binding force of an oxide film and an alloy matrix, and enhance the high-temperature oxidation resistance of the FeCrAl alloy.
In order to solve the problems existing in the prior art for smelting FeCrAl-V-La alloy, the invention also provides a method for preparing the alloy material, which comprises the following steps:
1) preparing materials: weighing vanadium powder, lanthanum powder, chromium powder, aluminum powder and iron powder according to corresponding mass percentages to prepare a mixture;
2) sealing: in a vacuum glove box, putting the mixture and the grinding balls in the step 1) into a ball milling tank, adding absolute ethyl alcohol as a process control agent, and sealing the ball milling tank;
3) ball milling: putting the ball milling tank obtained in the step 2) into a high-energy ball mill for ball milling;
4) and (3) screen granulation: adding a paraffin forming agent into the ball-milling mixture obtained in the step 3), and then wiping and screening the mixture by using a screen to prepare particles;
5) and (3) green pressing: cleaning the mold by using acetone, coating a proper amount of mold release agent, putting the mixed powder obtained in the step 4) into a graphite mold, and keeping the pressure at 150-200 MPa for 15 min;
6) and (3) sintering: sintering the graphite mold in a vacuum hot pressing furnace to obtain FeCrAl-V-La alloy, wherein the sintering process in the vacuum hot pressing furnace comprises the following steps: opening a vacuum pump for vacuumizing, performing pre-sintering when the vacuum degree is reduced to below 10Pa, increasing the temperature to 300-400 ℃ at a heating rate of 1-10 ℃/min, and then preserving the heat for 30-40 min; then high-temperature sintering is carried out, the temperature is increased to 1180-1220 ℃ at the temperature rise rate of 4-8 ℃/min, and the pressure is uniformly increased to 50-70 Mpa within 5-10 min; and (4) maintaining the pressure for 15-25 min, unloading, keeping the temperature for 3-4 h, and cooling to room temperature along with the furnace.
Further, in step 1), the Fe powder consists of two particle sizes: 12-15 μm and 8-10 μm, and the weight percentages are respectively: 60-75% of water and 25-40% of water; the particle diameters of vanadium powder, lanthanum powder, chromium powder and aluminum powder are all 30 micrometers;
further, in the step 1), polyoxyethylene dodecyl ether is further added as a dispersing agent in the process of proportioning the metal powder to reduce the agglomeration phenomenon of the powder and the viscosity of slurry in the process of ball milling, and the addition amount of the dispersing agent is as follows: 1 to 3ml/100 g.
Further, in the step 2), the mass ratio of the grinding balls to the mixture is (7-8): 1; the grinding balls are composed of stainless steel grinding balls with the diameters of 10mm, 6mm and 4mm respectively, and the mass ratio is 1:5: 1;
further, in the step 2), the total volume of the mixture and the grinding balls accounts for 20-40% of the volume of the ball milling tank; the using amount of the absolute ethyl alcohol is 5-6% of the total mass of the mixture;
further, in the step 2), introducing high-purity argon gas into the sealing tank to serve as protective gas;
further, in the step 3), the ball milling tank is placed into a high-energy ball mill for ball milling for 15-20 hours;
further, in the step 4), the addition amount of the paraffin is 6-10% of the mass of the ball-milling mixture; the screen is 400 meshes so as to improve the formability of the pressed compact in the compression molding process and the compactness of the pressed compact.
Compared with the prior art, the invention has the following beneficial effects:
(1) the high-temperature strength of the alloy is improved by adding a proper amount of V and La elements, the high-temperature strength of the alloy is improved by precipitation strengthening of V, La can reduce the generation rate of an oxide film of the FeCrAl alloy and enhance the binding force between the oxide film and a matrix, and La can reduce impurities causing alloy embrittlement and promote the fine dispersion distribution of V (C, N) while improving the high-temperature oxidation resistance of the alloy, so that the high-temperature comprehensive performance of the FeCrAl-V-La alloy is synergistically improved.
(2) The FeCrAl-V-La alloy is prepared by adopting a powder metallurgy method, and the prepared alloy material has uniform components and fine granularity, so that the problem of traditional smelting is avoided.
(3) The method has the advantages of simple process, easy realization, safe, environment-friendly and pollution-free raw materials and process, high efficiency and further reduction of the production cost. The obtained FeCrAl alloy material has high-temperature strength, excellent high-temperature oxidation resistance, long service life and strong practicability.
Drawings
FIG. 1 is a graph showing the oxidation kinetics of example 1 at 1250 ℃ for 300h, and example 2 at 1100 ℃ for 300 h.
Detailed Description
The described embodiments of the invention are only some of the embodiments of the invention and the scope of protection is not limited thereto.
Example 1:
(1) preparing materials: v is as follows according to the mass percent: 0.6%, La: 0.12%, Cr: 21%, Al: 5%, Fe: 73.28%, weighing vanadium powder, lanthanum powder, chromium powder, aluminum powder and iron powder with the purity higher than 99%, and preparing into a mixture; adding polyoxyethylene dodecyl ether according to the proportion of 1-3 ml/100 g;
(2) sealing: in a vacuum glove box, filling grinding balls and a mixture into a ball milling tank according to a ball-to-material ratio of 8:1, wherein the total volume of the grinding balls and the mixture accounts for 20-40% of the volume of the ball milling tank, adding absolute ethyl alcohol accounting for 5% of the total mass of the mixture into the ball milling tank as a process control agent, sealing the ball milling tank, and introducing high-purity argon as a protective gas;
(3) ball milling: putting the ball milling tank into a high-energy ball mill for ball milling for 15-20 h;
(4) and (3) granulating by using a screen: adding a paraffin forming agent into the mixture subjected to ball milling, wherein the addition amount (mass percentage) of paraffin is 6-10%, and then performing friction screening and granulation by using a 400-mesh screen;
(5) pressing: cleaning the mold by using acetone, coating a proper amount of mold release agent, putting the mixed powder into a graphite mold, and keeping the pressure at 150-200 MPa for 15 min;
(6) and (3) sintering: and (4) placing the graphite mold into a vacuum hot pressing furnace for sintering to obtain FeCrAl alloy. The sintering process in a vacuum hot pressing furnace comprises the following steps: opening a vacuum pump for vacuumizing, performing pre-sintering when the vacuum degree is reduced to below 10Pa, increasing the temperature to 300-400 ℃ at a heating rate of 1-10 ℃/min, and then preserving the heat for 30-40 min; then high-temperature sintering is carried out, the sintering temperature of the iron-based powder metallurgy material is TBaking＝(0.7～0.8)TmNamely 1100-1230 ℃, continuously increasing the temperature to 1180-1220 ℃ by adopting the heating rate of 4-8 ℃/min, pressurizing to 50-70 Mpa within 5-10 min, unloading after maintaining the pressure for 15-25 min, continuously preserving the heat for 3-4 h, and cooling along with the furnaceAnd (4) cooling to room temperature. This sample was designated as sample No. A1 obtained in example 1. A1 sample is cut into 30X 10X 5mm sample, and the weight of the sample after being oxidized in air at 1250 ℃ for 300h is 1.01mg/cm2。
Example 2:
the same as example 1 except that: vanadium powder is not added, but the vanadium powder comprises the following components in percentage by mass: la: 0.12%, Cr: 21%, Al: 5%, Fe: 73.88% lanthanum powder, chromium powder, aluminum powder and iron powder are weighed to prepare a mixture. This sample was designated as sample No. A2 obtained in example 2. A2 sample is cut into 30X 10X 5mm sample, and the weight of the sample after being oxidized in air at 1100 ℃ for 300h is 1.58mg/cm2。
The performance results for the samples prepared in examples 1 and 2 are shown in table 1 and fig. 1.
TABLE 1 basic Performance data for the samples obtained in examples 1 and 2, such as yield strength at elevated temperature, oxidation behavior, etc
FIG. 1 is a graph showing the oxidation kinetics of example 1 at 1250 ℃ for 300h, and example 2 at 1100 ℃ for 300 h. As can be seen from FIG. 1, the oxidation kinetics curves of the alloy all conform to the parabolic law, but the addition of V, La can further improve the high-temperature oxidation performance of the alloy.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (9)
1. The iron-chromium-aluminum alloy material for improving the high-temperature comprehensive performance by using the vanadium-rare earth synergy is characterized by comprising the following chemical components in percentage by mass: less than or equal to 0.05 percent of C, less than or equal to 0.14 percent of Si, less than or equal to 0.2 percent of Mn, less than or equal to 0.06 percent of S, less than or equal to 0.01 percent of P, V: 0.5-0.8%, La: 0.1-0.15%, Cr: 21-23%, Al: 5-6% of Fe, and the balance of Fe; is prepared by the following steps:
1) preparing materials: weighing vanadium powder, lanthanum powder, chromium powder, aluminum powder and iron powder according to corresponding mass percentages to prepare a mixture;
2) sealing: in a vacuum glove box, filling the mixture and the grinding balls in the step 1) into a ball milling tank, adding absolute ethyl alcohol as a process control agent, and sealing the ball milling tank;
3) ball milling: putting the ball milling tank obtained in the step 2) into a high-energy ball mill for ball milling;
4) and (3) granulating by using a screen: adding a paraffin forming agent into the ball-milling mixture obtained in the step 3), and then wiping and screening the mixture by using a screen to prepare particles;
5) pressing: cleaning the mold by using acetone, coating a proper amount of release agent, putting the mixed powder obtained in the step 4) into a graphite mold, pressing under the pressure of 150-200 MPa, and maintaining the pressure for a certain time;
6) and (3) sintering: the graphite mould is placed into a vacuum hot-pressing furnace for sintering to obtain FeCrAl-V-La alloy, and the sintering process in the vacuum hot-pressing furnace comprises the following steps: opening a vacuum pump for vacuumizing, performing pre-sintering when the vacuum degree is reduced to below 10Pa, increasing the temperature to 300-400 ℃ at a heating rate of 1-10 ℃/min, and then preserving the heat for 30-40 min; then high-temperature sintering is carried out, the temperature is raised to 1180-1220 ℃ at the temperature rise rate of 4-8 ℃/min, and the pressure is uniformly increased to 50-70 Mpa within 5-10 min; and (4) maintaining the pressure for 15-25 min, unloading, keeping the temperature for 3-4 h, and cooling to room temperature along with the furnace.
2. The ferrochromium-aluminum alloy material for improving high-temperature combination property by synergy of vanadium and rare earth as claimed in claim 1, wherein the original powder is vanadium powder, lanthanum powder, chromium powder, aluminum powder and iron powder, and the purity of each metal powder is higher than 99%.
3. The ferrochromium-aluminum alloy material for synergistically improving the high-temperature comprehensive performance by using the vanadium-rare earth as claimed in claim 1, wherein the fast oxidation life value is 83 hours, and the high-temperature strength is 135.8 MPa.
4. The preparation method of the ferrochromium-aluminum alloy material for synergistically improving the high-temperature comprehensive performance by using the vanadium-rare earth as claimed in claim 1, wherein the ferrochromium-aluminum alloy material comprises the following chemical components in percentage by mass: less than or equal to 0.05 percent of C, less than or equal to 0.14 percent of Si, less than or equal to 0.2 percent of Mn, less than or equal to 0.06 percent of S, less than or equal to 0.01 percent of P, V: 0.5-0.8%, La: 0.1-0.15%, Cr: 21-23%, Al: 5-6% of Fe, and the balance of Fe; the method is characterized by comprising the following steps:
1) preparing materials: weighing vanadium powder, lanthanum powder, chromium powder, aluminum powder and iron powder according to corresponding mass percentages to prepare a mixture;
in the process of proportioning the metal powder, a dispersing agent polyoxyethylene dodecyl ether is also added, wherein the addition amount of the dispersing agent is as follows: 1-3 ml/100 g;
2) sealing: in a vacuum glove box, putting the mixture and the grinding balls in the step 1) into a ball milling tank, adding absolute ethyl alcohol as a process control agent, and sealing the ball milling tank;
3) ball milling: putting the ball milling tank obtained in the step 2) into a high-energy ball mill for ball milling;
4) and (3) granulating by using a screen: adding a paraffin forming agent into the ball-milling mixture obtained in the step 3), and then wiping and screening the mixture by using a screen to prepare particles; the addition amount of the paraffin is 6-10% of the mass of the ball-milling mixture;
5) pressing: cleaning the mold by using acetone, coating a proper amount of mold release agent, putting the mixed powder obtained in the step 4) into a graphite mold, pressing at 150-200 MPa, and maintaining the pressure for a certain time;
6) and (3) sintering: sintering the graphite mold in a vacuum hot pressing furnace to obtain FeCrAl-V-La alloy, wherein the sintering process in the vacuum hot pressing furnace comprises the following steps: opening a vacuum pump for vacuumizing, performing pre-sintering when the vacuum degree is reduced to below 10Pa, increasing the temperature to 300-400 ℃ at a heating rate of 1-10 ℃/min, and then preserving the heat for 30-40 min; then high-temperature sintering is carried out, the temperature is raised to 1180-1220 ℃ at the temperature rise rate of 4-8 ℃/min, and the pressure is uniformly increased to 50-70 Mpa within 5-10 min; and (4) maintaining the pressure for 15-25 min, unloading, keeping the temperature for 3-4 h, and cooling to room temperature along with the furnace.
5. The method of claim 4, wherein in step 1), the Fe powder consists of two particle sizes: 12-15 μm and 8-10 μm, and the mass percentages are respectively: 60-75% of water and 25-40% of water; the particle diameters of the vanadium powder, the lanthanum powder, the chromium powder and the aluminum powder are all 30 mu m.
6. The preparation method according to claim 4, wherein in the step 2), the mass ratio of the grinding balls to the mixture is (7-8): 1; the grinding balls are composed of stainless steel grinding balls with the diameters of 10mm, 6mm and 4mm respectively, and the mass ratio is 1:5: 1; the total volume of the mixture and the grinding balls accounts for 20-40% of the volume of the ball milling tank; the using amount of the absolute ethyl alcohol is 5-6% of the total mass of the mixture; high-purity argon is introduced into the sealed ball milling tank to be used as protective gas.
7. The preparation method of claim 4, wherein in the step 3), the ball milling tank is placed in a high-energy ball mill for ball milling for 15-20 hours.
8. The method of claim 4, wherein in step 4), the screen is selected to be 400 mesh.
9. The method according to claim 4, wherein the dwell time in step 5) is 15 min.
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