CN112593161A - High-strength Sc composite nano oxide dispersion strengthening Fe-based alloy and preparation method thereof - Google Patents
High-strength Sc composite nano oxide dispersion strengthening Fe-based alloy and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-strength Sc composite nano oxide dispersion strengthening Fe-based alloy and a preparation method thereof, wherein an oxide playing a strengthening role in the alloy is Sc-Al-O or Sc-Ti-O composite nano oxide. The alloy comprises the following components in percentage by mass: 0.1-1.5% of Sc, 0.0-10.0% of Al, 9.0-25.0% of Cr, 0.0-0.6% of Ti, 0.05-0.35% of O, 0.0-4.0% of W and the balance of Fe. The preparation method comprises the following steps: (1) atomizing to prepare Fe-based alloy powder according to the alloy components; (2) mixing Fe-based alloy powder with a proper amount of oxide or mixed powder of oxide and hydride, and carrying out ball milling under the protection of high-purity argon or hydrogen to obtain mechanical alloying powder; (3) and (3) carrying out vacuum packaging on the ball-milled alloy powder, and solidifying the powder into the alloy by hot isostatic pressing or hot extrusion. By using the method, the oxygen content of the alloy can be effectively controlled, and the Sc-Al-O or Sc-Ti-O nano oxide with fine particle size, uniform distribution and stable structure is obtained, so that the alloy has excellent mechanical properties at room temperature and high temperature.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, and particularly provides a novel high-strength nano-oxide dispersion-strengthened Fe-based alloy and a preparation method thereof.
Background
With the rapid development of aviation, aerospace, nuclear energy and civil industries, the requirements on the high-temperature mechanical property and the high-temperature corrosion resistance of the material are higher and higher. The conventional high-temperature alloy adopts M23X6Precipitation hardening with MX precipitate phase as the main strengthening means, but M at high temperature23C6And MX is converged to grow or be dissolved into the matrix again, so that the alloy loses the strengthening effect, and the service temperature of the high-temperature alloy is limited. Dispersion strengthening, achieved by incorporating oxide ceramic particles with high stability in the alloy, has proven to be an effective way to achieve excellent high temperature strength. The Oxide Dispersion Strengthened (ODS) alloy can generate Y-rich Oxide particles with stable chemical structures in a matrix by adding a proper amount of elements such as Y, Al, Ti, oxygen and the like, plays a role in enhancing the mechanical strength of the alloy, and has the strengthening effect of maintaining the temperature close to the melting point temperature (1400 ℃) of the alloy and high-temperature oxidation resistance. ODS alloys are a new field of superalloy development.
The oxygen content in the ODS alloy is the main factor influencing the microstructure and macroscopic performance of the alloy, the alloy is prepared by adopting a powder metallurgy method, and Y is added2O3The powder becomes the main source of the precipitated phases of the nano Y-Al-O and Y-Ti-O. Pre-alloyed powder or simple substance element powder containing matrix components is mixed with yttrium oxide powder, ball milling is carried out under the protection of inert gas, the alloy powder after ball milling is solidified under high temperature and high pressure, and Y, Al, Ti and other elements in the matrix are re-precipitated under the assistance of oxygenAnd become Y-rich composite nano-oxides, and these nano-oxides are not easily changed under high temperature conditions, thus playing a role in strengthening the alloy. However, when the process is adopted, O, C, N pollution in the powder ball milling process cannot be avoided, and the Y and O contents of the alloy cannot be regulated and controlled simultaneously, so that the comprehensive performance of the alloy is influenced. In order to further improve the preparation process of the oxide dispersion strengthened Fe-based alloy and improve the mechanical property of the alloy, the research and development of new components, new processes and high-performance alloys are necessary to meet the requirements of modern industrial production.
Disclosure of Invention
The invention relates to the technical field of powder metallurgy, provides a high-strength oxide dispersion strengthened Fe-based alloy taking Sc-Al-O or Sc-Ti-O nano oxides as precipitated phases and a preparation method thereof, and realizes effective control of oxygen content in the alloy. The Sc-containing composite nano oxide particles obtained by the method have smaller sizes and more uniform distribution, so that the alloy has excellent room-temperature and high-temperature mechanical properties.
The technical scheme of the invention is as follows:
the high-strength Sc composite nano oxide dispersion strengthened Fe-based alloy is characterized by comprising the following components in percentage by mass: 0.1-1.5% of Sc, 0.0-10.0% of Al, 9.0-25.0% of Cr, 0.0-0.6% of Ti, 0.05-0.35% of O, 0.0-4.0% of W and the balance of Fe. The precipitated phase of the alloy is Sc-Al-O or Sc-Ti-O nano particles, and further preferable alloy components are as follows: 0.15-0.65% of Sc, 0.0-6.5% of Al, 9.0-16.0% of Cr, 0.2-0.5% of Ti, 0.10-0.35% of O, 0.0-2.0% of W and the balance of Fe.
A preparation method of a high-strength Sc composite nano oxide dispersion-strengthened Fe-based alloy comprises the following steps:
step one, according to the alloy components, smelting an alloy mother ingot by using a vacuum induction furnace, and atomizing to prepare powder to obtain Fe-based alloy powder containing active elements;
mixing Fe-based alloy powder with a proper amount of oxide powder or mixed powder of oxide and hydride, and carrying out ball milling under the protection of gas to obtain mechanical alloying powder;
and step three, carrying out vacuum packaging on the ball-milled alloy powder, and solidifying the powder to the alloy through hot isostatic pressing or hot extrusion.
By the method, the ODS-Fe-based alloy with a precipitated phase of Sc-Al-O or Sc-Ti-O composite nano-oxidation phase can be prepared.
As a preferred technical scheme:
and in the second step, Fe-based alloy powder with the particle diameter smaller than 100 mu m is selected during ball milling.
In the second step, the oxide powder used for mixing is one or more of ferric oxide, chromium oxide and scandium oxide, the hydride powder is titanium hydride, and the powder can be used for adjusting the oxygen content of Sc, Ti, Al and alloy in the matrix by controlling the dosage of single or combined powder. The addition amount of the powder for mixing is 0.20 to 1 weight percent.
And in the second step, the protective gas for ball milling is high-purity argon or hydrogen (more than or equal to 99.9%).
The technological parameters of ball milling in the second step are as follows: the ball milling speed is 180-350 r/min, and the ball milling time is 20-50 hours.
And in the third step, the temperature used in the hot isostatic pressing and hot extrusion process is 1050-1250 ℃, the applied pressure is 130-200 MPa, and the hot isostatic pressing time is maintained for 2-5 hours, so that the Sc-Al-O or Sc-Ti-O composite nano oxide can be dispersed and precipitated in the matrix.
The invention has the advantages that:
1) in terms of the preparation method, the invention realizes the effective control of the oxygen content in the ODS iron-based alloy through the adjustment of the oxide and hydride powder containing matrix components.
2) The invention realizes the dispersion and precipitation of Sc-Al-O and Sc-Ti-O composite nano oxides in the alloy, has small particle size and uniform distribution, and obtains the strong plasticity matching alloy.
Drawings
FIG. 1 is a transmission electron microscope picture and energy spectrum analysis result of the Sc-Al-O nano oxide distribution in the oxide dispersion strengthened FeCrAl alloy in example 1.
FIG. 2 is a metallographic comparison of the oxide dispersion strengthened FeCrAl alloy of example 2 with a smelted FeCrAl alloy, and (a) Sc composite nano-oxide strengthened FeCrAl alloy, and (b) smelted FeCrAl alloy.
FIG. 3 is a transmission electron microscope picture of the distribution of Sc-Ti-O nano oxides in the oxide dispersion strengthened FeCr alloy in example 3.
FIG. 4 is the mechanical properties of the oxide dispersion strengthened FeCr alloy of example 4 after forging.
Detailed Description
Example 1
The Sc composite nano oxide reinforced FeCrAl alloy is prepared, and the alloy comprises the following components in percentage by mass: fe-13Cr-6.0Al-0.3Ti-0.25 Sc-0.20O.
And smelting the alloy master ingot by using a kilogram-level vacuum induction furnace, and spraying by using a powder making device to obtain iron-based powder Fe-13Cr-6.0 Al. After the alloy powder is sieved, 1 kilogram of alloy powder with the particle size of less than 100 microns and 3.9 grams of high-purity Sc are mixed2O3Mixing the powder, and ball-milling for 40 hours by using high-energy ball-milling equipment under the conditions of high-purity Ar gas protection and rotating speed of 320 r/min. Then the powder is packaged in vacuum, and is pressed for 4 hours at 1150 ℃/160MPa by adopting a hot isostatic pressing process to prepare ODS-FeCrAl alloy, and the oxygen content is measured to be 0.20 wt%.
FIG. 1 is a transmission electron microscope photograph of the dispersion distribution of nano oxides in an ODS-FeCrAl alloy after hot isostatic pressing, wherein oxides with the average size of 10nm are dispersed and distributed in an alloy matrix, and the oxides are subjected to component analysis, and an energy spectrum shows that precipitated phase particles are mainly Sc-Al-O phase, so that the method can be used for effectively preparing the Sc-Al-O nano oxide dispersion strengthened FeCrAl alloy.
Example 2
Preparing a Sc composite nano oxide reinforced FeCrAl alloy, wherein the alloy comprises the following components: fe-20Cr-3.5Al-2W-0.25Ti-0.6 Sc-0.32O.
And smelting an alloy mother ingot by using a vacuum induction furnace, and atomizing by using a powder making device to obtain alloy powder with the components of Fe-20Cr-3.5Al-0.25Ti-0.2 Sc. After the alloy powder was sieved, 4 kg of the alloy powder having particles smaller than 100 μm were mixed with 20 g of iron oxide, 3.6 g of titanium hydride and 6.5 g of scandium oxide powder in a sieveRotating speed of 240r/min and high purity H2Ball milling is carried out for 50 hours under the protection of gas. And (3) carrying out vacuum packaging on the mechanical alloying powder, and pressing for 2 hours at 1200 ℃/150MPa by adopting a hot isostatic pressing process to prepare the ODS-FeCrAl alloy, wherein the oxygen content is about 0.32 wt%.
FIG. 2 is a photograph of the microstructure of an ODS alloy after hot isostatic pressing at 1200 ℃ while the metallographic microstructure of a molten FeCrAl alloy of similar composition is given for comparison. In the example, the alloy pressed at the high temperature of 1200 ℃ still has very fine grain size, a part of areas show obvious grain size bimodal distribution, and nano-scale grains surround the micron-scale grains, which mainly results from that Sc-Al-O nano-particles generated in the thermocuring process have strong pinning effect on the grain boundary of the alloy and have obvious inhibition on the growth of the grain boundary, thereby playing a role in strengthening the alloy. The hot isostatic pressed alloy of this example was tested for hardness, which was 291.6Hv0.5。
Example 3
The preparation method of the Sc composite nano oxide reinforced FeCr alloy comprises the following steps: fe-10Cr-0.30Ti-1.0W-0.35 Sc-0.22O.
Smelting an alloy mother ingot by using a vacuum induction furnace, atomizing by using a powder making device to obtain alloy powder with the components of Fe-10Cr-0.30Ti-1.0W-0.35Sc, and screening the alloy powder. 2 kg of iron-based alloy powder with the size less than 100 microns is mixed with 4.0 g of chromium oxide powder, and the mixture is ball-milled for 48 hours by using a high-energy ball mill under the protection of high-purity Ar gas at the rotating speed of 280 r/min. And (3) carrying out vacuum packaging on the alloyed powder after ball milling, completing the thermosetting of the alloy by adopting a hot extrusion mode, and preparing an ODS-FeCr alloy bar at 1050 ℃/150MPa, wherein the oxygen content of the alloy is about 0.22 wt%.
FIG. 3 is a distribution diagram of nano-oxide obtained after ODS-FeCr hot extrusion in alloy, and the composition shows that precipitated phases are mainly Sc-Ti-O phases, the particle size is concentrated between 2 nm and 6nm, and compared with the existing Y-Ti-O phase particles, the nano-oxide has smaller size, more uniform distribution and higher expected mechanical strength.
Example 4
The preparation method of the Sc composite nano oxide reinforced FeCr alloy comprises the following steps: fe-10Cr-0.30Ti-1.0W-0.35 Sc-0.22O.
The preparation process of the Sc composite nano-oxide reinforced FeCr alloy is consistent with that of the embodiment 3.
The bar stock obtained by hot extrusion is subjected to subsequent machining to obtain a bar with the diameter of 12.5mm, and after the bar is subjected to heat treatment at the temperature of 800 ℃/1 hour, the room-temperature and high-temperature mechanical strength of the alloy bar is tested, and the obtained result is shown in fig. 4. The ODS-FeCrAl alloy of this example had a room temperature tensile strength of 1291MPa, a yield strength of 1254MPa and an elongation of 13.5%; the tensile strength at the high temperature of 1000 ℃ is 188MPa, the yield strength is 148MPa, and the elongation is 14.5 percent. The alloy has excellent mechanical properties at room temperature and high temperature.
Example 5
Preparing a Sc composite nano oxide reinforced FeCrAl alloy, wherein the alloy comprises the following components: fe-13Cr-5.0Al-0.25 Sc-0.19O.
And smelting the alloy master ingot by using a kilogram-level vacuum induction furnace, and spraying by using a powder making device to obtain iron-based powder Fe-13Cr-5.0 Al. After the alloy powder is sieved, 1 kilogram of alloy powder with the particle size less than 100 microns and about 4 grams of high-purity Sc are mixed2O3Mixing the powder, and ball-milling for 48 hours by using high-energy ball-milling equipment under the conditions of high-purity Ar gas protection and the rotating speed of 300 r/min. And (3) carrying out vacuum packaging on the alloyed powder, and pressing for 4 hours at 1150 ℃/160MPa by adopting a hot isostatic pressing process to prepare the ODS-FeCrAl alloy, wherein the measured oxygen content is 0.19 wt%. The transmission electron microscope analysis obtains oxides with the particle size of 5-10 nm uniformly distributed in the alloy, the energy spectrum analysis obtains nano-oxide particles mainly composed of Sc-Al-O, and mechanical tests show that the alloy strength is similar to that of the alloy in the embodiment 1.
The above-mentioned embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and to implement the present invention, and therefore, the scope of the present invention should not be limited thereto, and all equivalent changes and modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (10)
1. The high-strength Sc composite nano oxide dispersion strengthened Fe-based alloy is characterized by comprising the following components in percentage by mass: 0.1-1.5% of Sc, 0.0-10.0% of Al, 9.0-25.0% of Cr, 0.0-0.6% of Ti, 0.05-0.35% of O, 0.0-4.0% of W and the balance of Fe.
2. The high-strength Sc composite nano oxide dispersion-strengthened Fe-based alloy as claimed in claim 1, wherein the alloy comprises, by mass: 0.15-0.65% of Sc, 0.0-6.5% of Al, 9.0-20.0% of Cr, 0.2-0.5% of Ti, 0.10-0.35% of O, 0.0-2.0% of W and the balance of Fe.
3. A method for preparing the high-strength Sc composite nano oxide dispersion-strengthened Fe-based alloy according to claim 1 or 2, characterized by comprising the steps of:
step one, according to alloy components, smelting an alloy mother ingot by using a vacuum induction furnace, and atomizing to prepare Fe-based alloy powder;
mixing Fe-based alloy powder and oxide powder or mixed powder of oxide and hydride, and carrying out ball milling under the protection of gas to obtain mechanical alloying powder;
and step three, carrying out vacuum packaging on the ball-milled alloy powder, and solidifying the powder to the alloy through hot isostatic pressing or hot extrusion.
4. The method for preparing the high-strength Sc composite nano oxide dispersion-strengthened Fe-based alloy according to claim 3, wherein the method comprises the following steps: the diameter of the Fe-based alloy powder used in the second step is less than 100 mu m.
5. The method for preparing the high-strength Sc composite nano oxide dispersion-strengthened Fe-based alloy according to claim 3, wherein the method comprises the following steps: in the second step, the oxide powder is one or more of ferric oxide, chromium oxide and scandium oxide, and the hydride powder is titanium hydride.
6. The method for preparing a high-strength Sc composite nano-oxide dispersion-strengthened Fe-based alloy according to claim 3 or 5, wherein the method comprises the following steps: in the second step, the addition amount of the oxide powder or the mixed powder of the oxide and the hydride is 0.20 to 1 weight percent.
7. The method for preparing the high-strength Sc composite nano oxide dispersion-strengthened Fe-based alloy according to claim 3, wherein the method comprises the following steps: and in the second step, the protective gas used for ball milling is high-purity argon or hydrogen.
8. The method for preparing the high-strength Sc composite nano oxide dispersion-strengthened Fe-based alloy according to claim 3, wherein the method comprises the following steps: and the technological parameters of ball milling in the second step are ball milling rotating speed of 180-350 r/min, and ball milling time is 20-50 hours.
9. The method for preparing the high-strength Sc composite nano oxide dispersion-strengthened Fe-based alloy as claimed in claim 3, wherein the process requirements of hot isostatic pressing and hot extrusion in step three are as follows: the curing temperature is 1050-1250 ℃, the applied pressure is 130-200 MPa, and the hot isostatic pressing needs to be kept for 2-5 hours.
10. The method for preparing the high-strength Sc composite nano oxide dispersion-strengthened Fe-based alloy according to claim 3, wherein the method comprises the following steps: the nano oxide precipitated from the prepared alloy is Sc-Al-O or Sc-Ti-O particles.
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