CN111041381B - Method for increasing content of solid solution oxygen in alloy - Google Patents
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Abstract
The invention provides a method for improving the content of solid solution oxygen in an alloy, which comprises the following steps: (1) mechanically alloying the main alloy element with 10-50% oxide powder to prepare oxygen supersaturated alloy powder; (2) adding oxygen supersaturated alloy powder into the alloy liquid, and stirring to realize uniform dispersion of the alloy powder in the alloy liquid; wherein the density of the oxygen supersaturated alloy powder is 90-120% of the density of the alloy liquid, the oxygen content of the oxygen supersaturated alloy powder is 3-10% by weight, and the melting point of the oxygen supersaturated alloy powder is 30-50 ℃ higher than the temperature of the alloy liquid. The invention has the advantages that: the problems of cavities and inclusions caused by directly filling oxygen into the alloy in the traditional smelting method are solved, the solid solution oxygen content in the alloy is greatly improved on the premise of ensuring the strength and toughness of the alloy, and a foundation is laid for preparing the oxide reinforced alloy by the smelting method; in addition, the method has simple process and high efficiency, and is suitable for industrial production.
Description
Technical Field
The invention relates to the field of alloy material preparation, in particular to a method for improving the content of solid solution oxygen in an alloy.
Background
Dispersion strengthening is one way of strengthening materials. Compared with the strengthening modes such as fine crystal strengthening, solid solution strengthening, precipitation strengthening and the like, the dispersion strengthening breaks through the limit of recrystallization of the material, and still has the strengthening effect under the condition of being close to the melting point. The oxide dispersion strengthening material is the most important one of the dispersion strengthening materials, and is characterized in that stable, uniform and fine second-phase oxides are introduced into a metal matrix, and dislocation movement is pinned so as to improve the strength of the material; meanwhile, the oxide has higher high-temperature thermal stability, so that the material can be prevented from generating grain boundary sliding at higher temperature, and the creep resistance of the material can be effectively improved; under the irradiation condition, the nanometer oxide is used as a nucleation site of the helium bubble, and the problems of helium brittleness and swelling under the irradiation of high-energy neutrons are solved to a great extent. Therefore, oxide strengthening is a desirable means to improve material performance. In recent years, research on dispersion-strengthened high-performance nickel-based, iron-based, and aluminum-based materials has attracted more and more attention.
At present, the method for preparing the oxide dispersion strengthening alloy mainly comprises a mechanical alloying method. However, the mechanical alloying method consumes time and energy, is easy to introduce impurities in the ball milling process, is not easy to prepare in large batch, and is difficult to realize engineering application. Thus, the "smelting process" is beginning to be an effective way to achieve large-scale production of oxide-dispersed alloys.
In order to obtain a high number density of oxides in the alloy, it is generally required that the solid solution oxygen content in the steel reaches 1000 ppm. However, in the conventional process for preparing oxide dispersion strengthened alloy by the "smelting method", although the oxygen content in the molten alloy liquid can reach 2000ppm, the oxygen concentration in the solidified alloy does not exceed 30ppm, and during the solidification process, too high dissolved oxygen can become gas to escape or be combined with elements in the molten steel to form inclusions, thereby obviously reducing the performance of the alloy. Therefore, in order to realize the smelting efficient preparation of the oxide dispersion strengthened alloy, a method capable of effectively increasing the content of the solid solution oxygen in the alloy is needed.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for improving the content of solid-solution oxygen in an alloy, which solves the problems of cavities and inclusions caused by directly filling oxygen into the alloy in the traditional smelting method, greatly improves the content of the solid-solution oxygen in the alloy on the premise of ensuring the strength and the toughness of the alloy, has simple process and high efficiency, and is suitable for industrial production.
The invention adopts the following technical scheme to solve the technical problems:
a method for increasing the content of solid solution oxygen in an alloy comprises the following steps:
(1) mechanically alloying the main alloy element with 10-50% oxide powder to prepare oxygen supersaturated alloy powder;
(2) adding the oxygen supersaturated alloy powder prepared in the step (1) into the alloy liquid, and stirring to realize uniform dispersion of the alloy powder in the alloy liquid;
wherein the density of the oxygen supersaturated alloy powder is 90-120% of the density of the alloy liquid, the oxygen content of the oxygen supersaturated alloy powder is 3-10% by weight, and the melting point of the oxygen supersaturated alloy powder is 30-50 ℃ higher than the temperature of the alloy liquid.
In a preferred embodiment of the present invention, in the step (1), the main alloy element and 10% to 50% of the oxide powder are added to a ball mill under the protection of an argon or nitrogen atmosphere to perform mechanical alloying, so as to achieve solid solution of oxygen in the matrix, thereby obtaining the oxygen supersaturated alloy powder.
In a preferred embodiment of the present invention, in the step (1), the oxide powder is specifically Y2O3、Fe2O3、Fe3O4、Gd2O3、NiO、ZrO2One kind of (1).
In a preferred embodiment of the present invention, in the step (2), the oxygen supersaturated alloy powder is added to the molten alloy liquid, and the alloy powder is uniformly dispersed in the alloy liquid by stirring; wherein the supercooling degree of the alloy liquid is 20-50 ℃, the alloy liquid is stirred and mixed for 5-10 min, and then the mixture is solidified at the speed of 60-400 ℃/min.
In a preferred embodiment of the present invention, in the step (2), the alloy liquid is specifically molten steel.
In a preferred embodiment of the present invention, the melting point of the oxygen-supersaturated alloy powder is controlled to be higher than the alloy liquid temperature by 30 to 50 ℃ by adjusting the composition.
As the inventionIn a preferred embodiment, the oxygen supersaturated alloy powder comprises the following components: 78% Fe, 10% Ti, 2% W and 10% Y2O3。
In a preferred embodiment of the present invention, the oxygen supersaturated alloy powder comprises the following components: 80% Ni and 20% Fe2O3。
Compared with the prior art, the invention has the advantages that: the invention utilizes mechanical alloying to prepare supersaturated oxide alloy powder which has the density similar to that of alloy and the melting point higher than the temperature of alloy liquid by 30-50 ℃, and then the supersaturated oxide alloy powder is added into the alloy liquid and is uniformly distributed in the alloy liquid in a solid phase particle state by rapid stirring, thereby achieving the purpose that supersaturated oxygen exists in the solid phase particles in a solid solution state; when the oxygen supersaturated alloy powder is solidified in the alloy, the concentration of solid solution oxygen in the alloy can reach more than 1000 ppm; the method avoids the problems of cavities and inclusions caused by directly filling oxygen into the alloy in the traditional smelting method, greatly improves the content of solid solution oxygen in the alloy on the premise of ensuring the strength and toughness of the alloy, and lays a foundation for preparing the oxide reinforced alloy by the smelting method; in addition, the method has simple process and high efficiency, and is suitable for industrial production.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
The method for increasing the content of solid solution oxygen in the alloy comprises the following steps:
(1) under the protection of argon atmosphere, mixing Fe 78%, Ti 10%, W2% and Y according to mass percentage2O3Adding 10 percent of the mixed solution into a ball mill for mechanical alloying to realize the solid solution of oxygen in a matrix so as to obtain oxygen supersaturated alloy powder;
(2) the method comprises the following steps of smelting Chinese low-activation anti-radiation structural steel (CLAM) molten steel by using a vacuum induction furnace, wherein the CLAM molten steel comprises, by mass, 0.1% of C, 9.0% of Cr, 1.5% of W, 0.20% of V, 0.19% of Ta, 0.45% of Mn, 0.05% of Si and the balance of Fe, wherein the total mass of the CLAM molten steel is 100%;
(3) adding the oxygen supersaturated alloy powder prepared in the step (1) into molten steel with the supercooling degree of 20 ℃ at the temperature of 1550 ℃, stirring for 5min, and then rapidly solidifying at the speed of 60 ℃/min;
wherein the density of the oxygen supersaturated alloy powder is 90 percent of the density of the molten steel, the oxygen content of the oxygen supersaturated alloy powder is 3 wt percent, and the melting point of the oxygen supersaturated alloy powder is higher than the temperature of the molten steel by 30 ℃.
The irradiation-resistant low-activation steel prepared by the method has no shrinkage cavity, inclusion and other macroscopic defects in the macroscopic structure after solidification according to the macroscopic structure analysis, and A, B, C, D-class nonmetallic inclusions in the macroscopic structure are not more than 0.5 grade according to the ASTM analysis. The solid solution oxygen content in the steel was about 1000 ppm. Therefore, the CLAM-ODS steel prepared by the embodiment has the advantages that the solid solution oxygen content is obviously improved, and the microstructure has no micro defects such as cavities, segregation and the like.
Example 2
The method for increasing the content of solid solution oxygen in the alloy comprises the following steps:
(1) under the protection of nitrogen atmosphere, mixing Ni 80% and Fe2O3Adding 20% of the alloy powder into a ball mill for mechanical alloying to realize the solid solution of oxygen in a matrix so as to obtain oxygen supersaturated alloy powder;
(2) smelting nickel-based alloy molten steel by using a vacuum induction furnace, wherein the total mass of the alloy molten steel is 100%, and the components and mass percentages of the alloy molten steel are Ni 52%, Cr 19%, Mo 3.0%, Nb 5.0%, Y6.0% and the balance of Fe;
(3) adding the oxygen supersaturated alloy powder prepared in the step (1) into alloy molten steel with the supercooling degree of 50 ℃ at the temperature of 1550 ℃, stirring for 8min, and then rapidly solidifying at the speed of 100 ℃/min;
wherein the density of the oxygen supersaturated alloy powder is 120 percent of the density of the alloy steel liquid, the oxygen content of the oxygen supersaturated alloy powder is 6 percent by weight, and the melting point of the oxygen supersaturated alloy powder is 50 ℃ higher than the temperature of the alloy steel liquid.
The nickel-based alloy prepared by the method has no shrinkage cavity, inclusion and other macroscopic defects in the macroscopic structure after solidification, and the A, B, C, D-type nonmetallic inclusion in the macroscopic structure is not more than 0.5 grade according to ASTM analysis. The solid solution oxygen content in the alloy was about 1200 ppm. Therefore, the content of solid solution oxygen in the nickel-based alloy is greatly improved, and a foundation is laid for realizing the ODS nickel-based alloy.
Example 3
The method for increasing the content of solid solution oxygen in the alloy comprises the following steps:
(1) under the protection of argon atmosphere, Fe 40%, W10%, Y10% and Fe3O4Adding 40% of the alloy powder into a ball mill for mechanical alloying to realize the solid solution of oxygen in a matrix so as to obtain oxygen supersaturated alloy powder;
(2) smelting Chinese low-activation anti-radiation structural steel (CLAM) molten steel by using a vacuum induction furnace, wherein the CLAM molten steel comprises, by mass, 0.1% of C, 90% of Cr, 1.5% of W, 0.20% of V, 0.19% of Ta0.19% of Mn, 0.45% of Si, and the balance of Fe, wherein the total mass of the CLAM molten steel is 100%; (ii) a
(3) Adding the oxygen supersaturated alloy powder prepared in the step (1) into molten alloy liquid with the supercooling degree of 40 ℃ at the temperature of 1550 ℃, stirring for 10min, and then rapidly solidifying at the speed of 400 ℃/min;
wherein the density of the oxygen supersaturated alloy powder is 96% of the density of the alloy liquid, the oxygen content of the oxygen supersaturated alloy powder is 10% by weight, and the melting point of the oxygen supersaturated alloy powder is higher than the temperature of the alloy liquid by 40 ℃.
The irradiation-resistant activated steel prepared by the method has no macroscopic defects such as shrinkage cavities, inclusion and the like in the macroscopic structure after solidification, and A, B, C, D-type nonmetallic inclusions in the macroscopic structure are not more than 0.5 grade according to ASTM analysis. The solid solution oxygen content in the steel was about 1000 ppm. Therefore, the CLAM-DOS steel prepared by the embodiment has the advantages that the solid solution oxygen content is obviously improved, and the microstructure has no micro defects such as cavities, segregation and the like.
In addition, it should be noted that the above embodiment 1The oxide powder in-3 can also be replaced by Gd2O3、NiO、ZrO2Any one of the above-mentioned alloys can be used as long as the melting point of the corresponding oxygen supersaturated alloy powder is maintained to be 30-50 ℃ higher than the temperature of the alloy liquid.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. A method for increasing the content of solid solution oxygen in an alloy is characterized by comprising the following steps:
(1) mechanically alloying the main alloy element with 10-50% oxide powder to prepare oxygen supersaturated alloy powder;
(2) adding the oxygen supersaturated alloy powder prepared in the step (1) into the alloy liquid, and stirring to realize uniform dispersion of the alloy powder in the alloy liquid; the supercooling degree of the alloy liquid is 20-50 ℃, the alloy liquid is stirred and mixed for 5-10 min, and then the mixture is solidified at the speed of 60-400 ℃/min;
wherein the oxide powder is specifically one of Y2O3, Fe2O3, Fe3O4, Gd2O3, NiO and ZrO 2; the density of the oxygen supersaturated alloy powder is 90-120% of the density of the alloy liquid, the oxygen content of the oxygen supersaturated alloy powder is 3-10% by weight, and the melting point of the oxygen supersaturated alloy powder is 30-50 ℃ higher than the temperature of the alloy liquid.
2. The method for increasing the content of solid-solution oxygen in the alloy according to claim 1, wherein in the step (1), under the protection of an argon or nitrogen atmosphere, the main alloy element and 10% -50% of oxide powder are added into a ball mill for mechanical alloying, so as to realize the solid solution of the oxygen element in the matrix, and obtain the oxygen supersaturated alloy powder.
3. The method for increasing the content of solid solution oxygen in the alloy according to claim 1, wherein in the step (2), the alloy liquid is specifically molten steel.
4. A method for increasing the solid solution oxygen content in an alloy as claimed in any one of claims 1 to 3, wherein the melting point of the oxygen supersaturated alloy powder is controlled to be 30 to 50 ℃ higher than the temperature of the alloy liquid by adjusting the composition.
5. The method for increasing the solid solution oxygen content in the alloy according to claim 4, wherein the oxygen supersaturated alloy powder comprises the following specific components: 78% Fe, 10% Ti, 2% W and 10% Y2O 3.
6. The method for increasing the solid solution oxygen content in the alloy according to claim 4, wherein the oxygen supersaturated alloy powder comprises the following specific components: 80% Ni and 20% Fe2O 3.
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| CN107541666A (en) * | 2017-09-08 | 2018-01-05 | 中国科学院合肥物质科学研究院 | A kind of preparation method of oxide dispersion intensifying steel |
| CN110181009A (en) * | 2019-06-26 | 2019-08-30 | 中国科学院合肥物质科学研究院 | Alloy powder Quick uniform decentralized control method in a kind of melt |
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| CN107541666A (en) * | 2017-09-08 | 2018-01-05 | 中国科学院合肥物质科学研究院 | A kind of preparation method of oxide dispersion intensifying steel |
| CN110181009A (en) * | 2019-06-26 | 2019-08-30 | 中国科学院合肥物质科学研究院 | Alloy powder Quick uniform decentralized control method in a kind of melt |
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