CN113201681B - Oxide-reinforced austenitic stainless steel and preparation method thereof - Google Patents

Oxide-reinforced austenitic stainless steel and preparation method thereof Download PDF

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CN113201681B
CN113201681B CN202110477902.4A CN202110477902A CN113201681B CN 113201681 B CN113201681 B CN 113201681B CN 202110477902 A CN202110477902 A CN 202110477902A CN 113201681 B CN113201681 B CN 113201681B
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oxide
stainless steel
ball milling
austenitic stainless
powder
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CN113201681A (en
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邱国兴
李小明
贺芸
韦旭立
白冲
李林波
梁李斯
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Xian University of Architecture and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0207—Using a mixture of prealloyed powders or a master alloy
    • C22C33/0228—Using a mixture of prealloyed powders or a master alloy comprising other non-metallic compounds or more than 5% of graphite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

Abstract

The invention discloses an oxide-strengthened austenitic stainless steel and a preparation method thereof, wherein the oxide-strengthened austenitic stainless steel comprises an austenitic stainless steel matrix and micron oxides, submicron oxides and nanometer oxides which are dispersed and uniformly distributed in the austenitic stainless steel matrix; wherein the micron oxide is Ti2O3、TiO2Or ZrO2The submicron oxide is Y2O3The nano oxide is Y-Zr-O. The preparation process comprises the following steps: carrying out hot isostatic pressing on the powder A to obtain a forming body; carrying out heat treatment on the formed body to release the thermal stress in the formed body; wherein the powder A is obtained by ball milling and mixing the micron oxide and the powder B; the powder B is obtained by ball milling and solid dissolving the submicron oxide and the powder C; powder C is nanometer Y2O3And carrying out ball milling and solid solution on the nano Zr powder and the austenitic stainless steel powder to obtain the zirconium-based alloy. The invention utilizes the oxide metallurgy technology and the dispersion strengthening theory to introduce various oxide particles with different sizes into the steel to strengthen the austenitic stainless steel.

Description

Oxide-reinforced austenitic stainless steel and preparation method thereof
Technical Field
The invention belongs to the technical field of ferrous metallurgy, and particularly relates to oxide-reinforced austenitic stainless steel and a preparation method thereof.
Background
The austenitic stainless steel is a stainless steel having an austenitic structure at normal temperature. The steel has a stable austenitic structure when it contains about 18% Cr, about 8-25% Ni, and about 0.1% C. The austenitic chromium nickel stainless steel comprises famous 18Cr-8Ni steel and high Cr-Ni series steel developed by increasing the contents of Cr and Ni and adding elements such as Mo, Cu, Si, Nb, Ti and the like on the basis of the steel. Austenitic stainless steels are non-magnetic and have high toughness and plasticity, but low strength, and due to the phase composition characteristics of austenitic stainless steels, they cannot be strengthened by phase transformation.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide oxide-reinforced austenitic stainless steel and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
an oxide-strengthened austenitic stainless steel comprises an austenitic stainless steel matrix and micron oxides, submicron oxides and nanometer oxides which are dispersed and uniformly distributed in the austenitic stainless steel matrix; wherein the micron oxide is Ti2O3、TiO2Or ZrO2The submicron oxide is Y2O3The nano oxide is Y-Zr-O.
Preferably, in the oxide-reinforced austenitic stainless steel, the mass content of the micro-oxides is 0.0005-0.001%, the size is 0.5-1.0 μm, and the number is 1015～1016Per m3(ii) a The mass content of the submicron oxide is 0.002% -0.003%, the size is 0.1-0.5 mu m, and the number is 1018～1019Per m3(ii) a The mass content of the nano oxide is 0.2-0.3%, the particle size is 10-20 nm, and the number is 1023～1024Per m3。
Preferably, the micron oxide, the submicron oxide and the nanometer oxide are all spherical oxide particles.
Preferably, the austenitic stainless steel matrix is 304 austenitic stainless steel, 304L austenitic stainless steel, 304N austenitic stainless steel, 309 austenitic stainless steel, 316L austenitic stainless steel, or 317 austenitic stainless steel.
The invention also provides a method for preparing the oxide reinforced austenitic stainless steel, which comprises the following steps:
carrying out hot isostatic pressing on the powder A to obtain a forming body;
carrying out heat treatment on the formed body to release the thermal stress in the formed body;
wherein the powder A is obtained by ball milling and mixing the micron oxide and the powder B;
the powder B is obtained by performing ball milling and solid solution on the submicron oxide and the powder C;
the powder C is nano Y2O3And carrying out ball milling and solid solution on the nano Zr powder and the austenitic stainless steel powder to obtain the zirconium-based alloy.
Preferably, when the powder C is prepared, the nano Y with the size of 15-30 nm is used2O3Carrying out ball milling and solid solution on nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m, wherein in the ball milling and solid solution process, the ball-material ratio is 10-15: 1, the ball milling rotating speed is 450-500 r/min, the ball milling time is 45-50 h, and argon protection is adopted in the ball milling process.
Preferably, when the powder B is prepared, the powder C and the submicron oxide with the size of 0.1-0.5 mu m are subjected to ball milling and solid solution, in the ball milling and solid solution process, the ball-material ratio is 5-6: 1, the ball milling rotation speed is 400-450 r/min, the ball milling time is 5-8 h, and the ball milling process adopts argon protection.
Preferably, when the powder A is prepared, the powder B and micron oxide with the size of 0.5-1 mu m are subjected to ball milling, the ball-material ratio is 5-6: 1, the ball milling rotation speed is 350-400 r/min, the ball milling time is 2-3 h, and argon protection is adopted in the ball milling process.
Preferably, in the hot isostatic pressing forming process of the powder A, the pressure is 200-250 MPa, the forming temperature is 1150-1200 ℃, and the heat preservation time is 3-4 h.
Preferably, the heat treatment process of the formed body comprises the steps of heating the formed body to 950-1000 ℃, preserving heat for 2.5-3 hours and then cooling in air.
The invention has the following beneficial effects:
in the oxide-reinforced austenitic stainless steel, micron oxides, submicron oxides and nanometer oxides are uniformly dispersed in an austenitic stainless steel matrix, wherein the micron oxides Ti2O3、TiO2And ZrO2The crystal lattice matching degree with austenitic stainless steel is higher, and the function of pinning a crystal boundary can be achieved; submicron oxide Y2O3And aoThe steel has certain lattice matching degree and certain solid solubility, and plays a role in pinning grain boundary and dislocation; Y-Zr-O has a high solid solubility in austenitic steels and therefore can act as strengthening phase particles for pinning dislocations. In conclusion, the invention solves the defect that the austenitic stainless steel cannot be subjected to phase transformation in the hot working process and is difficult to be strengthened by a heat treatment mode.
In the method for preparing the oxide reinforced austenitic stainless steel, the powder A can be sintered and densified by using a hot isostatic pressing forming process, so that micron oxides, submicron oxides and nanometer oxides are uniformly distributed in an austenitic stainless steel matrix, and the aim of reinforcing the austenitic stainless steel is fulfilled. The formed body obtained by hot isostatic pressing is subjected to heat treatment, so that the thermal stress accumulated in the hot isostatic pressing process can be released. Nanometer Y2O3When the nano Zr powder and the austenitic stainless steel powder are subjected to ball milling and solid solution, the nano Y2O3Can react with nano Zr powder to generate Y-Zr-O and partially dissolve into the matrix of austenitic stainless steel powder, and the addition of Zr can improve Y2O3Solid solubility of (d); when the submicron oxide and the powder C are subjected to ball milling and solid solution, the submicron Y is formed2O3The particles do not react with residual Zr in the steel, but submicron Y2O3The particles are mechanically mixed with the austenitic stainless steel to partially form a solid solution, and Y is dissolved in the steel2O3The particles can act as barriers to dislocation movement, and submicron Y particles not dissolved in steel2O3The particles may act to pin the grain boundaries. When the micron oxide and the powder B are mixed by ball milling, the micron oxide and the austenitic stainless steel are mechanically mixed without solid solution, and the micron oxide which is not dissolved in the steel can play a role in pinning a grain boundary.
Further, when preparing the powder C, the nano Y with the size of 15-30 nm is used2O3Carrying out ball milling and solid solution on nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m, wherein the powder is subjected to ball milling for multiple times, the granularity is reduced once every time the powder is milled, and a larger powder is adoptedThe grain size of the final product is favorably controlled, the ball-material ratio is 10-15: 1, the ball milling rotating speed is 450-500 r/min, the ball milling time is 45-50 h, and under the high ball-material ratio and high-speed long-time ball milling, the nano Y can be obtained2O3Reacting with nano Zr powder to generate Y-Zr-O, and partially dissolving the Y-Zr-O into an austenitic stainless steel matrix, wherein the powder can be prevented from being oxidized by adopting argon protection in the ball milling process.
Furthermore, when the powder B is prepared, the ball-material ratio is 5-6: 1, the ball milling rotating speed is 400-450 r/min, the ball milling time is 5-8 h, and the added submicron Y can be ensured at the short-time medium speed2O3The particles do not react with residual Zr in the steel, and the medium-speed ball milling can lead the submicron Y2O3The particles are mechanically mixed with the austenitic stainless steel and partially solid-solubilized.
Further, when the powder A is prepared, the ball-material ratio is 5-6: 1, the ball milling rotation speed is 350-400 r/min, and the ball milling time is 2-3 h, so that under the condition of short-time low-speed ball milling, the micron oxide and the austenitic stainless steel can be mechanically mixed without solid solution, and meanwhile, the short-time low-speed ball milling can also prevent the ball milling and crushing of the micron oxide.
Detailed Description
The present invention will be further described with reference to the following examples.
The oxide-strengthened austenitic stainless steel comprises an austenitic stainless steel matrix and micron oxides, submicron oxides and nanometer oxides which are dispersed and distributed in the austenitic stainless steel matrix, wherein the austenitic stainless steel matrix comprises the following components in parts by weight: 304 austenitic stainless steel, 304L austenitic stainless steel, 304N austenitic stainless steel, 309 austenitic stainless steel, 316L austenitic stainless steel or 317 austenitic stainless steel, wherein the micro-oxide is Ti2O3、TiO2Or ZrO2The submicron oxide is Y2O3The nano oxide is Y-Zr-O. The micron oxide, the submicron oxide and the nanometer oxide are all spherical particles. In the oxide reinforced austenitic stainless steel, the mass content of the micron oxide particles is0.0005% -0.001%, the size is 0.5-1.0 μm, and the number is 1015～1016Per m3(ii) a The mass content of the submicron oxide particles is 0.002% -0.003%, the size is 0.1-0.5 mu m, and the number is 1018～1019Per m3(ii) a The mass content of the nano oxide particles is 0.2-0.3%, the size is 10-20 nm, and the number is 1023～1024Per m3。
The preparation method of the oxide reinforced austenitic stainless steel comprises the following steps:
(1) subjecting nano-Y with the size of 15-30 nm to2O3Placing nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m into a ball mill for high-speed ball milling and solid solution; in the ball milling and solid solution process, the ball-material ratio is 10-15: 1, the ball milling rotation speed is 450-500 r/min, the ball milling time is 45-50 h, and the ball milling process adopts argon protection.
(2) Carrying out medium-speed ball milling and mixing on the submicron oxide with the size of 0.1-0.5 mu m and the powder prepared in the step (1) according to steel components; in the ball milling process, the ball-material ratio is 5-6: 1, the ball milling rotation speed is 400-450 r/min, the ball milling time is 5-8 h, and argon protection is adopted in the ball milling process.
(3) Carrying out low-speed ball milling and mixing on the micron oxide with the size of 0.5-1 mu m and the powder prepared in the step (2) according to steel components; in the ball milling process, the ball-material ratio is 5-6: 1, the ball milling rotation speed is 350-400 r/min, the ball milling time is 2-3 h, and argon protection is adopted in the ball milling process.
(4) Performing hot isostatic pressing on the powder obtained in the step (3), wherein the forming temperature is 1150-1200 ℃, the pressure is 200-250 MPa, and the heat preservation time is 3-4 h;
(5) regulating and controlling the structure performance of the formed body obtained in the step (4): and heating the formed steel sample to 950-1000 ℃, preserving heat for 2.5-3 hours, and carrying out air cooling after the heat preservation is finished.
Example 1
In the oxide-strengthened austenitic stainless steel of the present example, the austenitic stainless steel matrix is: 304 austenitic stainless steel, wherein the micron oxide is Ti2O3The submicron oxide is Y2O3The nano oxide is Y-Zr-O. The micron oxide, the submicron oxide and the nanometer oxide are all spherical particles. In the oxide-strengthened austenitic stainless steel of the present example, the content of the fine oxide particles is 0.0005% by mass, the size is 0.5 to 1.0 μm, and the number is 1.2 × 10 in terms of mass percentage15Per m3(ii) a The submicron oxide particles have a mass content of 0.002%, a size of 0.1-0.5 μm, and a number of 1.1 × 1018Per m3(ii) a The nano oxide particles have a mass content of 0.2%, a size of 10-20 nm and a number of 2.2 × 1023Per m3。
The preparation method of the oxide reinforced austenitic stainless steel comprises the following steps:
(1) subjecting nano-Y with the size of 15-30 nm to2O3Placing nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m into a ball mill for high-speed ball milling and solid solution; in the ball milling and solid solution process, the ball-material ratio is 10:1, the ball milling rotation speed is 450 r/min, the ball milling time is 50h, and the ball milling process adopts argon protection.
(2) Carrying out medium-speed ball milling and mixing on the submicron oxide with the size of 0.1-0.5 mu m and the powder prepared in the step (1) according to steel components; in the ball milling process, the ball-material ratio is 5:1, the ball milling rotation speed is 400 r/min, the ball milling time is 8h, and the ball milling process adopts argon protection.
(3) Carrying out low-speed ball milling and mixing on the micron oxide with the size of 0.5-1 mu m and the powder prepared in the step (2) according to steel components; in the ball milling process, the ball-material ratio is 5:1, the ball milling rotation speed is 350 r/min, the ball milling time is 3h, and the ball milling process adopts argon protection.
(4) Carrying out hot isostatic pressing on the powder obtained in the step (3), wherein the forming temperature is 1150 ℃, the pressure is 200MPa, and the heat preservation time is 4 h;
(5) regulating and controlling the structure performance of the formed body obtained in the step (4): and (3) placing the formed steel sample at 950 ℃ for heat preservation for 3 hours.
The table of the performance test of the oxide-reinforced austenitic stainless steel manufactured in this example is shown in table 1.
Example 2
In the oxide-strengthened austenitic stainless steel of the present example, the austenitic stainless steel matrix is: 304 austenitic stainless steel, wherein the micron oxide is Ti2O3The submicron oxide is Y2O3The nano oxide is Y-Zr-O. The micron oxide, the submicron oxide and the nanometer oxide are all spherical particles. In the oxide-strengthened austenitic stainless steel of the present embodiment, the content of the micro oxide particles is 0.001% by mass, the size is 0.5 to 1.0 μm, and the number is 8.9 × 1016Per m3(ii) a The submicron oxide particles have a mass content of 0.003%, a size of 0.1 to 0.5 μm and a number of 9.1 × 1018Per m3(ii) a The nano oxide particles have a mass content of 0.3%, a size of 10-20 nm and a number of 8.6 × 1023Per m3。
The preparation method of the oxide reinforced austenitic stainless steel comprises the following steps:
(1) subjecting nano-Y with the size of 15-30 nm to2O3Placing nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m into a ball mill for high-speed ball milling and solid solution; in the ball milling and solid solution process, the ball-material ratio is 15:1, the ball milling rotation speed is 500 r/min, the ball milling time is 45h, and the ball milling process adopts argon protection.
(2) Carrying out medium-speed ball milling and mixing on the submicron oxide with the size of 0.1-0.5 mu m and the powder prepared in the step (1) according to steel components; in the ball milling process, the ball-material ratio is 6:1, the ball milling rotation speed is 450 r/min, the ball milling time is 5h, and the ball milling process adopts argon protection.
(3) Carrying out low-speed ball milling and mixing on the micron oxide with the size of 0.5-1 mu m and the powder prepared in the step (2) according to steel components; in the ball milling process, the ball-material ratio is 6:1, the ball milling rotation speed is 400 r/min, the ball milling time is 3h, and the ball milling process adopts argon protection.
(4) Carrying out hot isostatic pressing on the powder obtained in the step (3), wherein the forming temperature is 1200 ℃, the pressure is 250MPa, and the heat preservation time is 3 h;
(5) regulating and controlling the structure performance of the formed body obtained in the step (4): the shaped bodies were heated to 1000 ℃ and held for 2.5h and then air-cooled.
The table of the performance test of the oxide-reinforced austenitic stainless steel manufactured in this example is shown in table 1.
Example 3
In the oxide-strengthened austenitic stainless steel of the present example, the austenitic stainless steel matrix is: 304 austenitic stainless steel, wherein the micron oxide is Ti2O3The submicron oxide is Y2O3The nano oxide is Y-Zr-O. The micron oxide, the submicron oxide and the nanometer oxide are all spherical particles. In the oxide-strengthened austenitic stainless steel of the present embodiment, the content of the micro oxide particles is 0.0007% by mass, the size is 0.5 to 1.0 μm, and the number is 5.6 × 1015Per m3(ii) a The submicron oxide particles have a mass content of 0.0026%, a size of 0.1-0.5 μm, and a number of 6.3 × 1018Per m3(ii) a The mass content of the nano oxide particles is 0.24-0.3%, the size is 10-20 nm, and the number is 7.0 multiplied by 1023Per m3。
The preparation method of the oxide reinforced austenitic stainless steel comprises the following steps:
(1) subjecting nano-Y with the size of 15-30 nm to2O3Placing nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m into a ball mill for high-speed ball milling and solid solution; in the ball milling and solid solution process, the ball-material ratio is 13:1, the ball milling rotation speed is 480 r/min, the ball milling time is 47h, and the ball milling process adopts argon protection.
(2) Carrying out medium-speed ball milling and mixing on the submicron oxide with the size of 0.1-0.5 mu m and the powder prepared in the step (1) according to steel components; in the ball milling process, the ball-material ratio is 6:1, the ball milling rotation speed is 430 r/min, the ball milling time is 7h, and the ball milling process adopts argon protection.
(3) Carrying out low-speed ball milling and mixing on the micron oxide with the size of 0.5-1 mu m and the powder prepared in the step (2) according to steel components; in the ball milling process, the ball-material ratio is 5:1, the ball milling rotation speed is 380 r/min, the ball milling time is 2.5h, and the ball milling process adopts argon protection.
(4) Carrying out hot isostatic pressing on the powder obtained in the step (3), wherein the forming temperature is 1180 ℃, the pressure is 230MPa, and the heat preservation time is 3.5 h;
(5) regulating and controlling the structure performance of the formed body obtained in the step (4): the molded body is heated to 980 ℃, kept warm for 2.7h and then cooled in air.
The table of the performance test of the oxide-reinforced austenitic stainless steel manufactured in this example is shown in table 1.
Example 4
In the oxide-strengthened austenitic stainless steel of the present example, the austenitic stainless steel matrix is: 304L austenitic stainless steel, wherein the micron oxide is TiO2The submicron oxide is Y2O3The nano oxide is Y-Zr-O. The micron oxide, the submicron oxide and the nanometer oxide are all spherical particles. In the oxide-reinforced austenitic stainless steel of the present embodiment, the mass content of the micro oxide particles is 0.007%, the size is 0.5 to 1.0 μm, and the number is 5.8 × 1015～1016Per m3(ii) a The submicron oxide particles have a mass content of 0.0028%, a size of 0.1-0.5 μm, and a number of 6.1 × 1018Per m3(ii) a The nano oxide particles have a mass content of 0.26%, a size of 10-20 nm and a number of 6.8 × 1023Per m3。
The preparation method of the oxide reinforced austenitic stainless steel comprises the following steps:
(1) subjecting nano-Y with the size of 15-30 nm to2O3Placing nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m into a ball mill for high-speed ball milling and solid solution; in the ball milling and solid solution process, the ball-material ratio is 14:1, the ball milling rotation speed is 460 r/min, the ball milling time is 48h, and the ball milling process adopts argon protection.
(2) Carrying out medium-speed ball milling and mixing on the submicron oxide with the size of 0.1-0.5 mu m and the powder prepared in the step (1) according to steel components; in the ball milling process, the ball-material ratio is 5:1, the ball milling speed is 440 r/min, the ball milling time is 7h, and the ball milling process adopts argon protection.
(3) Carrying out low-speed ball milling and mixing on the micron oxide with the size of 0.5-1 mu m and the powder prepared in the step (2) according to steel components; in the ball milling process, the ball-material ratio is 6:1, the ball milling speed is 390 r/min, the ball milling time is 2.8h, and the ball milling process adopts argon protection.
(4) Carrying out hot isostatic pressing on the powder obtained in the step (3), wherein the forming temperature is 1190 ℃, the pressure is 240MPa, and the heat preservation time is 3.5 h;
(5) regulating and controlling the structure performance of the formed body obtained in the step (4): the molded body is heated to 980 ℃, kept warm for 2.7h and then cooled in air.
The table of the performance test of the oxide-reinforced austenitic stainless steel manufactured in this example is shown in table 1.
Example 5
In the oxide-strengthened austenitic stainless steel of the present example, the austenitic stainless steel matrix is: 304N austenitic stainless steel, wherein the micro oxide is ZrO2The submicron oxide is Y2O3The nano oxide is Y-Zr-O. The micron oxide, the submicron oxide and the nanometer oxide are all spherical particles. In the oxide-strengthened austenitic stainless steel of the present embodiment, the content of the micro oxide particles is 0.001% by mass, the size is 0.5 to 1.0 μm, and the number is 3.5 × 1015Per m3(ii) a The submicron oxide particles have a mass content of 0.0024%, a size of 0.1-0.5 μm, and a number of 4.2 × 1018Per m3(ii) a The nano oxide particles have a mass content of 0.26%, a size of 10-20 nm and a number of 5.8 × 1023Per m3。
The preparation method of the oxide reinforced austenitic stainless steel comprises the following steps:
(1) subjecting nano-Y with the size of 15-30 nm to2O3Placing nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m into a ball mill for high-speed ball milling and solid solution; in the ball milling and solid solution process, the ball-material ratio is 13:1, the ball milling rotation speed is 470 r/min, the ball milling time is 46h, and the ball milling process adopts argon protection.
(2) Carrying out medium-speed ball milling and mixing on the submicron oxide with the size of 0.1-0.5 mu m and the powder prepared in the step (1) according to steel components; in the ball milling process, the ball-material ratio is 5:1, the ball milling rotation speed is 430 r/min, the ball milling time is 7h, and the ball milling process adopts argon protection.
(3) Carrying out low-speed ball milling and mixing on the micron oxide with the size of 0.5-1 mu m and the powder prepared in the step (2) according to steel components; in the ball milling process, the ball-material ratio is 6:1, the ball milling speed is 360 r/min, the ball milling time is 2.5h, and the ball milling process adopts argon protection.
(4) Carrying out hot isostatic pressing on the powder obtained in the step (3), wherein the forming temperature is 1170 ℃, the pressure is 230MPa, and the heat preservation time is 3.5 h;
(5) regulating and controlling the structure performance of the formed body obtained in the step (4): the molded body was heated to 960 ℃ and kept warm for 2.8h, and then air-cooled.
The table of the performance test of the oxide-reinforced austenitic stainless steel manufactured in this example is shown in table 1.
Example 6
In the oxide-strengthened austenitic stainless steel of the present example, the austenitic stainless steel matrix is: 309 austenitic stainless steel, wherein the micro oxide is TiO2The submicron oxide is Y2O3The nano oxide is Y-Zr-O. The micron oxide, the submicron oxide and the nanometer oxide are all spherical particles. In the oxide-strengthened austenitic stainless steel of the present example, the content of the fine oxide particles is 0.0005% by mass, the size is 0.5 to 1.0 μm, and the number is 2.6 × 1015Per m3(ii) a The submicron oxide particles have a mass content of 0.003%, a size of 0.1 to 0.5 μm and a number of 7.7 × 1018Per m3(ii) a The nano oxide particles have a mass content of 0.27%, a size of 10-20 nm and a number of 8.9 × 1023Per m3。
The preparation method of the oxide reinforced austenitic stainless steel comprises the following steps:
(1) subjecting nano-Y with the size of 15-30 nm to2O310-20 nm in size and 40 ℃in sizePutting 50 mu m austenitic stainless steel powder into a ball mill for high-speed ball milling and solid solution; in the ball milling and solid solution process, the ball-material ratio is 13:1, the ball milling rotation speed is 480 r/min, the ball milling time is 47h, and the ball milling process adopts argon protection.
(2) Carrying out medium-speed ball milling and mixing on the submicron oxide with the size of 0.1-0.5 mu m and the powder prepared in the step (1) according to steel components; in the ball milling process, the ball-material ratio is 6:1, the ball milling speed is 440 r/min, the ball milling time is 7h, and the ball milling process adopts argon protection.
(3) Carrying out low-speed ball milling and mixing on the micron oxide with the size of 0.5-1 mu m and the powder prepared in the step (2) according to steel components; in the ball milling process, the ball-material ratio is 5:1, the ball milling speed is 360 r/min, the ball milling time is 2.5h, and the ball milling process adopts argon protection.
(4) Carrying out hot isostatic pressing on the powder obtained in the step (3), wherein the forming temperature is 1190 ℃, the pressure is 220MPa, and the heat preservation time is 3.5 h;
(5) regulating and controlling the structure performance of the formed body obtained in the step (4): the molded body was heated to 970 ℃, heat-preserved for 2.7h, and then air-cooled.
The table of the performance test of the oxide-reinforced austenitic stainless steel manufactured in this example is shown in table 1.
Example 7
In the oxide-strengthened austenitic stainless steel of the present example, the austenitic stainless steel matrix is: 316 austenitic stainless steel, wherein the micro oxide is TiO2The submicron oxide is Y2O3The nano oxide is Y-Zr-O. The micron oxide, the submicron oxide and the nanometer oxide are all spherical particles. In the oxide-strengthened austenitic stainless steel of the present embodiment, the content of the micro oxide particles is 0.0008% by mass, the size is 0.5 to 1.0 μm, and the number is 6.9 × 1015Per m3(ii) a The submicron oxide particles have a mass content of 0.003%, a size of 0.1 to 0.5 μm and a number of 8.6 × 1018Per m3(ii) a The nano oxide particles have a mass content of 0.3%, a size of 10-20 nm and a number of 8.7 × 1023Per m3。
The preparation method of the oxide reinforced austenitic stainless steel comprises the following steps:
(1) subjecting nano-Y with the size of 15-30 nm to2O3Placing nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m into a ball mill for high-speed ball milling and solid solution; in the ball milling and solid solution process, the ball-material ratio is 13:1, the ball milling rotation speed is 470 r/min, the ball milling time is 48h, and the ball milling process adopts argon protection.
(2) Carrying out medium-speed ball milling and mixing on the submicron oxide with the size of 0.1-0.5 mu m and the powder prepared in the step (1) according to steel components; in the ball milling process, the ball-material ratio is 5:1, the ball milling rotation speed is 410 r/min, the ball milling time is 7h, and the ball milling process adopts argon protection.
(3) Carrying out low-speed ball milling and mixing on the micron oxide with the size of 0.5-1 mu m and the powder prepared in the step (2) according to steel components; in the ball milling process, the ball-material ratio is 6:1, the ball milling rotation speed is 380 r/min, the ball milling time is 2.6h, and the ball milling process adopts argon protection.
(4) Carrying out hot isostatic pressing on the powder obtained in the step (3), wherein the forming temperature is 1180 ℃, the pressure is 235MPa, and the heat preservation time is 3.6 h;
(5) regulating and controlling the structure performance of the formed body obtained in the step (4): the molded body is heated to 980 ℃, kept warm for 2.8h and then cooled in air.
The table of the performance test of the oxide-reinforced austenitic stainless steel manufactured in this example is shown in table 1.
Example 8
In the oxide-strengthened austenitic stainless steel of the present example, the austenitic stainless steel matrix is: 316L austenitic stainless steel, wherein the micron oxide is Ti2O3The submicron oxide is Y2O3The nano oxide is Y-Zr-O. The micron oxide, the submicron oxide and the nanometer oxide are all spherical particles. In the oxide-strengthened austenitic stainless steel of the present embodiment, the content of the micro oxide particles is 0.0009% by mass, the size is 0.5 to 1.0 μm, and the number is 7.9 × 1015Per m3(ii) a The mass content of the submicron oxide particles is 0.0027%, size of 0.1-0.5 μm, and number of 6.8 × 1018～1019Per m3(ii) a The nano oxide particles have a mass content of 0.27%, a size of 10-20 nm and a number of 7.9 × 1023Per m3。
The preparation method of the oxide reinforced austenitic stainless steel comprises the following steps:
(1) subjecting nano-Y with the size of 15-30 nm to2O3Placing nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m into a ball mill for high-speed ball milling and solid solution; in the ball milling and solid solution process, the ball-material ratio is 12:1, the ball milling speed is 490 r/min, the ball milling time is 48h, and the ball milling process adopts argon protection.
(2) Carrying out medium-speed ball milling and mixing on the submicron oxide with the size of 0.1-0.5 mu m and the powder prepared in the step (1) according to steel components; in the ball milling process, the ball-material ratio is 6:1, the ball milling rotation speed is 410 r/min, the ball milling time is 7h, and the ball milling process adopts argon protection.
(3) Carrying out low-speed ball milling and mixing on the micron oxide with the size of 0.5-1 mu m and the powder prepared in the step (2) according to steel components; in the ball milling process, the ball-material ratio is 6:1, the ball milling speed is 370 r/min, the ball milling time is 2.6h, and the ball milling process adopts argon protection.
(4) Carrying out hot isostatic pressing on the powder obtained in the step (3), wherein the forming temperature is 1160 ℃, the pressure is 230MPa, and the heat preservation time is 3.5 h;
(5) regulating and controlling the structure performance of the formed body obtained in the step (4): the molded body was heated to 960 ℃ and kept warm for 2.7h, and then air-cooled.
The table of the performance test of the oxide-reinforced austenitic stainless steel manufactured in this example is shown in table 1.
Example 9
In the oxide-strengthened austenitic stainless steel of the present example, the austenitic stainless steel matrix is: 317 austenitic stainless steel, wherein the micron oxide is TiO2The submicron oxide is Y2O3The nano oxide is Y-Zr-O. The micron oxide, the submicron oxide and the nanometer oxide are all spherical particles. To be provided withIn the oxide-strengthened austenitic stainless steel of the present example, the mass content of the micro oxide particles is 0.0006%, the size is 0.5 to 1.0 μm, and the number is 4.7 × 1015Per m3(ii) a The submicron oxide particles have a mass content of 0.0022%, a size of 0.1-0.5 μm, and a number of 3.2 × 1018Per m3(ii) a The nano oxide particles have a mass content of 0.27%, a size of 10-20 nm and a number of 7.3 × 1023Per m3。
The preparation method of the oxide reinforced austenitic stainless steel comprises the following steps:
(1) subjecting nano-Y with the size of 15-30 nm to2O3Placing nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m into a ball mill for high-speed ball milling and solid solution; in the ball milling and solid solution process, the ball-material ratio is 13:1, the ball milling rotation speed is 480 r/min, the ball milling time is 47h, and the ball milling process adopts argon protection.
(2) Carrying out medium-speed ball milling and mixing on the submicron oxide with the size of 0.1-0.5 mu m and the powder prepared in the step (1) according to steel components; in the ball milling process, the ball-material ratio is 5:1, the ball milling speed is 440 r/min, the ball milling time is 7.5h, and the ball milling process adopts argon protection.
(3) Carrying out low-speed ball milling and mixing on the micron oxide with the size of 0.5-1 mu m and the powder prepared in the step (2) according to steel components; in the ball milling process, the ball-material ratio is 5:1, the ball milling rotation speed is 380 r/min, the ball milling time is 2.5h, and the ball milling process adopts argon protection.
(4) Carrying out hot isostatic pressing on the powder obtained in the step (3), wherein the forming temperature is 1170 ℃, the pressure is 235MPa, and the heat preservation time is 3.5 h;
(5) regulating and controlling the structure performance of the formed body obtained in the step (4): the molded body is heated to 980 ℃, kept warm for 2.7h and then cooled in air.
The table of the performance test of the oxide-reinforced austenitic stainless steel manufactured in this example is shown in table 1.
TABLE 1
Figure BDA0003047750310000141
The invention can be seen from the above, different particles are introduced through different short-time ball milling processes, the dosage and the size of each scale particle are optimized, and the multi-scale particles are uniformly distributed in the low-activation steel matrix through hot isostatic pressing forming, so that the strength of the low-activation steel is obviously improved.

Claims (9)

1. The oxide-reinforced austenitic stainless steel is characterized by comprising an austenitic stainless steel matrix and micron oxides, submicron oxides and nanometer oxides which are dispersed and uniformly distributed in the austenitic stainless steel matrix; wherein the micron oxide is Ti2O3、TiO2Or ZrO2The submicron oxide is Y2O3The nano oxide is Y-Zr-O;
in the oxide-reinforced austenitic stainless steel, the mass content of the micron oxide is 0.0005-0.001%, the size is 0.5-1.0 mu m, and the number is 1015~1016Per m3(ii) a The mass content of the submicron oxide is 0.002% -0.003%, the size is 0.1-0.5 mu m, and the number is 1018~1019Per m3(ii) a The mass content of the nano oxide is 0.2-0.3%, the particle size is 10-20 nm, and the number is 1023~1024Per m3。
2. The oxide-strengthened austenitic stainless steel of claim 1, wherein the micro, sub-micro and nano-oxides are spherical oxide particles.
3. The oxide-strengthened austenitic stainless steel of any of claims 1-2, wherein the austenitic stainless steel matrix is 304 austenitic stainless steel, 304L austenitic stainless steel, 304N austenitic stainless steel, 309 austenitic stainless steel, 316L austenitic stainless steel, or 317 austenitic stainless steel.
4. A method of manufacturing the oxide-strengthened austenitic stainless steel of any of claims 1 to 3, comprising the steps of:
carrying out hot isostatic pressing on the powder A to obtain a forming body;
carrying out heat treatment on the formed body to release the thermal stress in the formed body;
wherein the powder A is obtained by ball milling and mixing the micron oxide and the powder B;
the powder B is obtained by performing ball milling and solid solution on the submicron oxide and the powder C;
the powder C is nano Y2O3And carrying out ball milling and solid solution on the nano Zr powder and the austenitic stainless steel powder to obtain the zirconium-based alloy.
5. The method according to claim 4, wherein the powder C is prepared by mixing nano-Y particles having a size of 15 to 30nm2O3Carrying out ball milling and solid solution on nano Zr powder with the size of 10-20 nm and austenitic stainless steel powder with the size of 40-50 mu m, wherein in the ball milling and solid solution process, the ball-material ratio is 10-15: 1, the ball milling rotating speed is 450-500 r/min, the ball milling time is 45-50 h, and argon protection is adopted in the ball milling process.
6. The method as claimed in claim 4, wherein when preparing the powder B, the powder C and the submicron oxide with the size of 0.1-0.5 μm are subjected to ball milling and solid solution, the ball-material ratio in the ball milling and solid solution process is 5-6: 1, the ball milling rotation speed is 400-450 r/min, the ball milling time is 5-8 h, and the ball milling process adopts argon protection.
7. The method as claimed in claim 4, wherein when preparing the powder A, the powder B is ball-milled with micron oxides with the size of 0.5-1 μm, the ball-to-material ratio in the ball-milling process is 5-6: 1, the ball-milling rotation speed is 350-400 r/min, the ball-milling time is 2-3 h, and argon gas is adopted for protection in the ball-milling process.
8. The method according to any one of claims 4 to 7, wherein the powder A is subjected to hot isostatic pressing at a pressure of 200 to 250MPa, a forming temperature of 1150 to 1200 ℃ and a holding time of 3 to 4 hours.
9. The method according to any one of claims 4 to 7, wherein the heat treatment of the shaped body comprises heating the shaped body to 950 to 1000 ℃, holding the temperature for 2.5 to 3 hours, and then cooling the heated shaped body with air.
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