CN112647012A - Fe-Cr-Al-Nb-Ti-RE alloy material for catalyst carrier of exhaust gas purifier and preparation method thereof - Google Patents
Fe-Cr-Al-Nb-Ti-RE alloy material for catalyst carrier of exhaust gas purifier and preparation method thereof Download PDFInfo
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- C22C38/00—Ferrous alloys, e.g. steel alloys
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/002—Hybrid process, e.g. forging following casting
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/26—Ferrous alloys, e.g. steel alloys containing chromium with niobium or tantalum
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
Abstract
The invention belongs to the field of steel materials, and discloses a Fe-Cr-Al-Nb-Ti-RE alloy material for a catalyst carrier of an exhaust gas purifier and a preparation method thereof. The invention is based on commercial Fe25Cr5Al (wt%) alloy, optimizes the component proportion, and greatly improves the high-temperature corrosion resistance by adding lanthanum, cerium and yttrium mixed rare earth, titanium, niobium and other elements. Under severe conditions of extremely high temperature, thermal fatigue, thermal shock and the like, the rare earth elements La, Ce and Y obviously improve the adhesion of an alloy matrix and an oxide film and improve the high-temperature oxidation resistance of the iron-chromium-aluminum alloy. Meanwhile, the interaction of elements formed by the rare earth and strong carbonitrides such as Ti, Nb and the like promotes fine precipitated phases to disperse and separate out refined grains, and improves the toughness of the iron-chromium-aluminum alloy. The material is suitable for the field of catalyst carriers of exhaust purifiers of internal combustion engines.
Description
Technical Field
The invention relates to a catalyst carrier of an automobile exhaust purifier, in particular to an iron-chromium-aluminum alloy material and a preparation method thereof, belonging to the field of steel materials.
Background
The adoption of the high-efficiency tail gas purifier becomes a necessary measure for reducing the tail gas emission of the internal combustion engine and controlling air pollution. The quality and performance of the catalyst carrier material play an important role in the exhaust gas purification effect. The catalyst carrier material applied to the tail gas purifier mainly comprises a honeycomb ceramic carrier and a metal carrier, and compared with the ceramic carrier, the metal carrier has the advantages of small heat capacity, high heat conductivity and good high-temperature oxidation resistance, and is an important development direction for purifying the tail gas of the internal combustion engine.
The Fe-Cr-Al high-temperature alloy has relatively low thermal expansion coefficient, strong high-temperature oxidation resistance and low production cost, and has wide application prospect in comprehensive consideration of processability, economic value and the like. Because the service environment of the carrier material is under the test conditions of severe conditions such as thermal cycle with temperature difference of hundreds of degrees, thermal fatigue, thermal shock and the like for a long time, the protective oxide film layer formed on the surface of the Fe-Cr-Al alloy is easy to peel off and becomes a main factor causing the failure of a material system. The high-temperature oxidation resistance of the alloy can be obviously improved by coating technology, oxide dispersion strengthening, active element adding and the like, and the Fe-Cr-Al alloy with the high-temperature oxidation resistance improved by adding the active element Hf and the like is widely applied so far.
With the rapid development of automobile manufacturing technology, the quality requirement of the purifier catalyst carrier material is continuously higher. The high-temperature service life of the iron-chromium-aluminum alloy can be obviously prolonged by adding the active elements such as the mixed rare earth La, Ce, Y and the like, and the alloy with excellent high-temperature oxidation resistance and comprehensive mechanical property is prepared by adopting commercial mixed rare earth, ferrotitanium and ferroniobium through the process of a vacuum induction smelting furnace and can be used as a catalyst carrier material of a purifier and other electric heating alloy devices.
Disclosure of Invention
The invention provides a preparation method of a low-cost catalyst carrier material for an automobile exhaust purifier, which has excellent high-temperature oxidation resistance and mechanical property and can be used as a catalyst carrier of the exhaust purifier and an electric heating alloy element.
The carrier material of the tail gas purifier comprises the following components in percentage by mass: cr: 23-25 wt%, Al: 4.5-5.5 wt%, Ti: 0.1-0.5 wt%, Nb: 0.5-1.5 wt%, RE: 0.1 to 0.25 wt%, less than or equal to 0.002 wt% of C, less than or equal to 0.003 wt% of S, less than 0.03 wt% of N, less than 0.2 wt% of Si, less than 0.02 wt% of P, and the balance of Fe and inevitable impurities.
A preparation method of Fe-Cr-Al-Nb-Ti-RE alloy material for a catalyst carrier of an exhaust purifier adopts a vacuum induction furnace smelting process, and comprises the following specific steps:
(1) pretreatment of raw materials: before smelting, putting ferrochromium, aluminum, industrial pure iron, ferrotitanium and ferroniobium into a drying box for drying, wherein the raw material is industrial pure iron containing carbon and ultralow sulfur, and the temperature is 100-150 ℃;
(2) melting: charging in a crucible, selecting an electric smelting magnesia crucible as a smelting crucible, and adding dried ferrochromium, ferrocolumbium and industrial pure iron rods to ensure that the later furnace burden melting stage is smoothly carried out, wherein the charging is tight and loose;
(3) melting and refining:
vacuumizing after charging is finished, keeping the vacuum degree for 3-8 min after the vacuum degree reaches 0.12Pa, starting cooling water, and preparing for power transmission and heating;
the melting time is shortened by keeping larger power in the early stage of melting, and the power is properly reduced when the furnace burden starts to melt, so that the furnace burden is prevented from bridging smoothly by melting;
when furnace burden is completely melted, no bubbles are emitted from the surface of molten steel, heating to 1600-1650 ℃, preserving heat for 10-15 min, and refining alloy;
taking a 50Kg vacuum induction furnace as an example, the power is kept between 80 and 90KW in the early stage of melting so as to shorten the melting time, and when the furnace burden starts to melt, the power is kept between 30 and 40KW so as to ensure that the melting is smoothly carried out and prevent the furnace burden from bridging;
(4) adding ferrotitanium, pure aluminum and rare earth:
titanium is prevented from being oxidized, ferrotitanium is added within 15-20 min before tapping, and stirring is carried out, so that the titanium is uniformly distributed in the molten steel;
protective gas is filled, aluminum is added in batches, and the aluminum is uniformly distributed in the steel through stirring;
adding rare earth Re under the heat preservation power, stirring for 1-2 min, adjusting the temperature of the molten steel to 1600-1650 ℃, and preparing for tapping;
(5) tapping and pouring: pouring under argon, paying attention to the fact that an oxide film enters molten steel, stopping power supply after pouring, and preparing for breaking vacuum;
(6) breaking vacuum: before breaking vacuum, in order to prevent the molten steel from being oxidized and polluted, the molten steel is cooled for 10-15 min in a vacuum environment and then broken vacuum;
(7) hot forging: and (3) carrying out heat preservation on the steel ingot at 1050 ℃ for 30min, then carrying out open forging, wherein the finish forging temperature is 750 ℃.
In the step (4), the protective gas is argon.
The invention has the beneficial effects that:
the alloy material prepared by the invention has lower cost and excellent comprehensive performance. Compared with the traditional Fe-Cr-Al alloy, the addition of the RE, Ti and Nb elements obviously improves the high-temperature resistance, oxidation resistance and processability.
Drawings
FIG. 1 is a graph showing the oxidation kinetics of Fe-Cr-Al alloy and Fe-Cr-Al-Nb-Ti-RE alloy.
FIG. 2 shows the surface morphology of Fe-Cr-Al alloy after the material is oxidized in air for 300h at 1100 ℃.
FIG. 3 shows the surface morphology of the material after oxidation in air for 300h at 1100 ℃ for Fe-Cr-Al-Nb-Ti-RE alloy.
FIG. 4 shows the cross-sectional morphology of the Fe-Cr-Al alloy oxide film after the material is oxidized in air for 300h at 1100 ℃.
FIG. 5 shows the cross-sectional morphology of an oxide film of Fe-Cr-Al-Nb-Ti-RE alloy after the material is oxidized in air for 300h at 1100 ℃.
Detailed Description
Comparative example 1
The composition ratio is optimized based on the existing commercial Fe25Cr5Al (wt%) alloy material. The weight percentage of the components is as follows: cr: 23-25, Al: 4.5-5.5, less than 0.0015 of C, less than 0.0031 of P, less than 0.0041 of S, less than 0.12 of Si, and the balance of Fe.
The raw materials are dried and weighed, then the industrial pure iron, the metal chromium and the pure aluminum are added into a furnace for smelting in batches, and the hot forging forming is carried out after pouring and demoulding. The wrought alloy is processed into a 30 multiplied by 10 multiplied by 5mm sample by cutting, and the weight of the sample is increased to 4.4mg/cm after being oxidized in the air at 1100 ℃ for 300h2. After the oxide film is oxidized for 300 hours at 1100 ℃, the oxide film cracks and peels off.
Example 1
Based on the component proportion of the embodiment 1, materials such as lanthanum-cerium-yttrium mixed rare earth, titanium, niobium and the like are added. The weight percentages of the specific components are as follows: cr: 23-25, Al: 4.5-5.5, Ti: 0.1 to 0.5, Nb: 0.5 to 1.5, RE: 0.1-0.25 percent, less than or equal to 0.002 percent of C, less than or equal to 0.003 percent of S, less than 0.03 percent of N, less than 0.2 percent of Si, less than 0.02 percent of P, and the balance of Fe.
The smelting process of the vacuum induction furnace comprises the following specific steps:
(1) pretreatment of raw materials: before smelting, putting ferrochromium, aluminum, industrial pure iron, ferrotitanium and ferroniobium into a drying oven for drying at 100-150 ℃;
(2) melting: charging materials into a crucible, selecting an electric smelting magnesia crucible as a smelting crucible, and adding dried ferrochromium, ferrocolumbium and industrial pure iron rods;
(3) melting and refining:
vacuumizing after charging is finished, keeping the vacuum degree for 3-8 min after the vacuum degree reaches 0.12Pa, starting cooling water, and preparing for power transmission and heating;
the higher power is kept for supplying power in the early stage of melting to shorten the melting time, and the heating power is properly reduced when the furnace burden begins to melt;
when furnace burden is completely melted, no bubbles are emitted from the surface of molten steel, heating to 1600-1650 ℃, and keeping the temperature for 10-15 min for alloy refining;
(4) adding ferrotitanium, pure aluminum and rare earth:
adding ferrotitanium in batches within 15-20 min before tapping, and stirring to uniformly distribute the titanium element in the molten steel;
argon is filled, aluminum is added in batches, and the aluminum is uniformly distributed in the steel through stirring;
adding rare earth Re under the heat preservation power, stirring for 1-2 min, adjusting the temperature of the molten steel to 1600-1650 ℃, and preparing for tapping;
(5) tapping and pouring: pouring under argon, paying attention to the fact that an oxide film enters molten steel, stopping power supply after pouring, and preparing for breaking vacuum;
(6) breaking vacuum: cooling for 10-15 min in a vacuum environment and then breaking vacuum;
(7) hot forging: and (3) carrying out heat preservation on the steel ingot at 1050 ℃ for 30min, then carrying out open forging, wherein the finish forging temperature is 750 ℃.
The wrought alloy is processed into a 30 multiplied by 10 multiplied by 5mm sample by cutting, and the weight of the sample is increased to 0.83mg/cm after being oxidized in the air at 1100 ℃ for 300h2. The oxidation kinetics curve follows a parabolic law, which shows that a perfect oxidation film has been formed, effectively preventing further oxidation of the alloy. The result shows that the alloy material has excellent high-temperature oxidation resistance and can be applied to the fields of catalyst carrier materials of exhaust gas purifiers of internal combustion engines and the like.
FIG. 1 is a graph showing the oxidation kinetics of Fe-Cr-Al alloy and Fe-Cr-Al-Nb-Ti-RE alloy. As can be seen from FIG. 1, the high temperature oxidation resistance of the Fe-Cr-Al alloy is remarkably improved after rare earth elements, Ti and Nb are added.
FIG. 2 shows the surface morphology of Fe-Cr-Al alloy after the material is oxidized in air for 300h at 1100 ℃.
FIG. 3 shows the surface morphology of the material after oxidation in air for 300h at 1100 ℃ for Fe-Cr-Al-Nb-Ti-RE alloy.
Comparing fig. 2 and 3 shows that the material added with lanthanum, cerium and yttrium mixed rare earth, titanium and niobium has flat and compact surface appearance after high-temperature oxidation. This type of oxidation has very excellent resistance to high temperature oxidation.
FIG. 4 shows the cross-sectional morphology of an oxide film of Fe-Cr-Al alloy, which is formed by oxidizing the material at 1100 ℃ in air for 300h, wherein the oxide film has delamination, undulation and a large number of voids.
FIG. 5 shows the cross-sectional morphology of the Fe-Cr-Al-Nb-Ti-RE alloy oxide film, which is continuously compact and flat, after the material is oxidized in air at 1100 ℃ for 300 h.
Comparing fig. 4 and 5 shows that after the material added with the lanthanum, cerium and yttrium mixed rare earth, titanium and niobium is oxidized at high temperature, the oxide film is more tightly combined with the matrix, and the high-temperature oxidation resistance is better.
The foregoing is only a preferred embodiment of the present invention and appropriate changes and modifications may be made by those skilled in the art without departing from the principles of the invention and these changes and modifications are to be considered as the protection of the present invention.
Claims (4)
1. The Fe-Cr-Al-Nb-Ti-RE alloy material for the catalyst carrier of the tail gas purifier is characterized by comprising the following components in percentage by mass: cr: 23-25 wt%, Al: 4.5-5.5 wt%, Ti: 0.1-0.5 wt%, Nb: 0.5-1.5 wt%, RE: 0.1 to 0.25 wt%, less than or equal to 0.002 wt% of C, less than or equal to 0.003 wt% of S, less than 0.03 wt% of N, less than 0.2 wt% of Si, less than 0.02 wt% of P, and the balance of Fe and inevitable impurities.
2. The preparation method of the Fe-Cr-Al-Nb-Ti-RE alloy material for the catalyst carrier of the exhaust gas purifier according to claim 1, which is characterized in that a vacuum induction electric furnace smelting process is adopted, and the method comprises the following specific steps:
(1) pretreatment of raw materials: before smelting, putting ferrochromium, aluminum, industrial pure iron, ferrotitanium and ferroniobium into a drying box for drying;
(2) melting: charging materials into a crucible, selecting an electric smelting magnesia crucible as a smelting crucible, and adding dried ferrochromium, ferrocolumbium and industrial pure iron rods;
(3) melting and refining:
vacuumizing after charging is finished, keeping the vacuum degree for 3-8 min after the vacuum degree reaches 0.12Pa, starting cooling water, and preparing for power transmission and heating;
the higher power is kept for supplying power in the early stage of melting to shorten the melting time, and the heating power is properly reduced when the furnace burden begins to melt;
when furnace burden is completely melted, no bubbles are emitted from the surface of molten steel, heating to 1600-1650 ℃, and keeping the temperature for 10-15 min for alloy refining;
(4) adding ferrotitanium, pure aluminum and rare earth:
adding ferrotitanium in batches within 15-20 min before tapping, and stirring to uniformly distribute the titanium element in the molten steel;
protective gas is filled, aluminum is added in batches, and the aluminum is uniformly distributed in the steel through stirring;
adding rare earth Re under the heat preservation power, stirring for 1-2 min, adjusting the temperature of the molten steel to 1600-1650 ℃, and preparing for tapping;
(5) tapping and pouring: pouring under argon, paying attention to the fact that an oxide film enters molten steel, stopping power supply after pouring, and preparing for breaking vacuum;
(6) breaking vacuum: cooling for 10-15 min in a vacuum environment and then breaking vacuum;
(7) hot forging: and (3) carrying out heat preservation on the steel ingot at 1050 ℃ for 30min, then carrying out open forging, wherein the finish forging temperature is 750 ℃.
3. The method according to claim 2, wherein the drying temperature in the step (1) is 100 to 150 ℃.
4. The method of claim 2, wherein in step (4), the protective gas is argon.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113308644A (en) * | 2021-05-10 | 2021-08-27 | 江苏大学 | Iron-chromium-aluminum alloy material for improving high-temperature comprehensive performance by using vanadium-rare earth synergy and preparation method thereof |
| CN114959435A (en) * | 2022-05-26 | 2022-08-30 | 中联先进钢铁材料技术有限责任公司 | Nb-Cr-Fe ternary intermediate alloy and preparation method and application thereof |
| CN115786636A (en) * | 2022-12-15 | 2023-03-14 | 河钢股份有限公司 | Method for smelting high-purity iron-chromium-aluminum alloy by vacuum induction furnace |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113308644A (en) * | 2021-05-10 | 2021-08-27 | 江苏大学 | Iron-chromium-aluminum alloy material for improving high-temperature comprehensive performance by using vanadium-rare earth synergy and preparation method thereof |
| CN114959435A (en) * | 2022-05-26 | 2022-08-30 | 中联先进钢铁材料技术有限责任公司 | Nb-Cr-Fe ternary intermediate alloy and preparation method and application thereof |
| CN115786636A (en) * | 2022-12-15 | 2023-03-14 | 河钢股份有限公司 | Method for smelting high-purity iron-chromium-aluminum alloy by vacuum induction furnace |
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