CN113215480B - Multi-scale particle reinforced low-activation steel and preparation method thereof - Google Patents

Multi-scale particle reinforced low-activation steel and preparation method thereof Download PDF

Info

Publication number
CN113215480B
CN113215480B CN202110475932.1A CN202110475932A CN113215480B CN 113215480 B CN113215480 B CN 113215480B CN 202110475932 A CN202110475932 A CN 202110475932A CN 113215480 B CN113215480 B CN 113215480B
Authority
CN
China
Prior art keywords
powder
ball milling
particles
low
nano
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110475932.1A
Other languages
Chinese (zh)
Other versions
CN113215480A (en
Inventor
邱国兴
李小明
韦旭立
贺芸
白冲
李林波
梁李斯
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian University of Architecture and Technology
Original Assignee
Xian University of Architecture and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian University of Architecture and Technology filed Critical Xian University of Architecture and Technology
Priority to CN202110475932.1A priority Critical patent/CN113215480B/en
Publication of CN113215480A publication Critical patent/CN113215480A/en
Application granted granted Critical
Publication of CN113215480B publication Critical patent/CN113215480B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/10—Pre-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/20—Post-treatment, e.g. curing, coating or polishing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00—Products made by additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D6/00—Heat treatment of ferrous alloys
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Civil Engineering (AREA)
  • Composite Materials (AREA)
  • Structural Engineering (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses multi-scale particle reinforced low-activation steel and a preparation method thereof2O3The submicron particle is Y2O3The nano particles are Y-Ti-O; in the multi-scale particle reinforced low-activation steel, the content of micron particles is 0.01-0.02 percent, the content of submicron particles is 0.01-0.02 percent, and the content of nano particles is 0.1-0.2 percent by mass percent; the size of the microparticles is greater than 0.5 μm and less than or equal to 1.5 μm, and the number of the microparticles is 1013~1014Per m3(ii) a The size of the sub-micrometer particles is 0.1 μm or more and 0.5 μm or less, and the number of the sub-micrometer particles is 1017~1018Per m3(ii) a The nanoparticles have a particle size of 10-20 nm and a number of 1023~1024Per m3。

Description

Multi-scale particle reinforced low-activation steel and preparation method thereof
Technical Field
The invention belongs to the technical field of ferrous metallurgy, and particularly relates to multi-scale particle reinforced low-activation steel and a preparation method thereof.
Background
The low-activation steel becomes a preferred structural material of the fusion reactor due to the excellent characteristics of the low-activation steel, and the materials have higher thermal conductivity and neutron irradiation damage resistance at 300-500 ℃. But the defects of insufficient high-temperature strength (the highest operation temperature can only reach 550 ℃), easy helium brittleness and the like greatly limit the use of the alloy in key parts such as the first wall of a fusion reactor, the fourth generation fission fast reactor cladding and the like. Because of the requirement of low activity, the addable alloy elements are limited, and the performance of the alloy is difficult to be greatly improved by a simple alloying method. There are two concepts at present: one is to introduce a dispersion phase of refractory oxide (Y) into the low activation steel2O3Y-Ti-O, etc.), and the mechanical property of the steel is improved by utilizing the dispersion strengthening effect of the second phase; secondly, the grain size of the low-activation steel is adjusted through a heat treatment process, and the mechanical property of the steel is improved by utilizing fine grain strengthening.
At present, the powder metallurgy process is generally adopted to introduce fine dispersed oxide particles into steel. But the powder is very easy to be polluted during mechanical alloying, the mechanical alloying time is more than 50-100 hours, and the production efficiency is low. The subsequent hot isostatic pressing process requires higher pressure and temperature, and the compactness of the product is difficult to ensure. The need for elevated temperatures and heat preservation to adjust the grain size of low activation steel through heat treatment processes increases manufacturing costs. Meanwhile, because the working temperature of the low-activation steel is higher, fine crystal grains adjusted by heat treatment are quickly coarsened at high temperature, and the strengthening effect is reduced.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide the multi-scale particle reinforced low-activation steel and the preparation method thereof.
The technical scheme adopted by the invention is as follows:
the multi-scale particle reinforced low-activation steel comprises a low-activation matrix and micro-particles, sub-micro-particles and nano-particles which are uniformly distributed in the low-activation matrix, wherein the micro-particles are TiN or Ti2O3The submicron particle is Y2O3The nano particles are Y-Ti-O;
in the multi-scale particle reinforced low-activation steel, the content of the micron particles is 0.01-0.02 percent, the content of the submicron particles is 0.01-0.02 percent, and the content of the nano particles is 0.1-0.2 percent by mass percent;
the size of the micro-particles is 0.5-1.5 μm, and the number of the micro-particles is 1013～1014Per m3(ii) a The sub-micron particles have a size of 0.1 to 0.5 μm and a number of 1017～1018Per m3(ii) a The particle size of the nano particles is 10-20 nm, and the number of the nano particles is 1023～1024Per m3。
Preferably, the low activation matrix is Eurofer97, 9Cr2WVTa, F82H, JLF-1, CLAM, CLF-1 or ARAA.
The invention also provides a method for preparing the multi-scale particle reinforced low-activation steel, which comprises the following steps:
performing laser printing forming in an inert gas atmosphere of powder C to obtain a forming body;
performing high-temperature stress regulation and control on the formed body;
wherein, the powder C is obtained by ball milling and mixing micron particles and the powder B; powder B is submicron Y2O3Performing ball milling and solid solution on the powder A to obtain the powder A; the powder A is nanometer Y2O3And the nano Ti powder and the low-activation steel powder are subjected to ball milling and solid solution to obtain the low-activation steel powder.
Preferably, the size of the low-activation steel powder is 50-100 mu m and the size of the low-activation steel powder is nanometer Y2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm.
Preferably, nano-Y2O3Nano Ti powder and low-activation steel powder ballIn the grinding process, the ball-material ratio is 10 (1-1.5), the ball-milling rotating speed is 500-550 r/min, the ball-milling time is 10-15 h, and the ball-milling atmosphere is inert atmosphere.
Preferably, nano-Y2O3Y is obtained by ball milling of nano Ti powder and low-activation steel powder2O3The mass ratio of the nano Ti powder to the low-activation steel powder is (0.5-1): (0.5-1): 100.
Preferably, submicron Y2O3In the process of carrying out ball milling and solid solution on the powder A, the ball-material ratio is 5 (1-1.5), the ball milling rotating speed is 300-350 r/min, the ball milling time is 2-3 h, and the ball milling atmosphere is inert atmosphere; submicron Y2O3The mass of (A) is 0.02-0.04% of the mass of the powder A.
Preferably, in the ball milling and mixing process of the micron particles and the powder B, the ball-material ratio is 5 (1-1.5), the ball milling speed is 100-150 r/min, the ball milling time is 2-3 h, and the ball milling atmosphere is inert atmosphere; the mass of the micron particles is 1-2% of the mass of the powder B.
Preferably, in the process of carrying out laser printing forming in the inert gas atmosphere of powder C, the laser power is 3.5-4 kW, the powder feeding speed is 1.2-1.5 kg/h, the scanning speed is 1000m/min, and argon protection is carried out in the whole printing process.
Preferably, the high-temperature stress control process for the molded body comprises: and heating the formed body to 950-980 ℃, preserving heat for 2-2.5 hours, and then cooling.
The invention has the following beneficial effects:
in the multi-scale particle reinforced low-activation steel, a plurality of particles with different sizes reinforce the low-activation steel, wherein the micron particles and the submicron particles can pin the grain boundary to play a role in fine crystal reinforcement, and the submicron particles and the nanoparticles pin the dislocation to play a role in second phase reinforcement. The strengthening effect of the second phase in the steel is directly related to its chemical composition, size, shape, amount and distribution. The invention controls the following components by content: the content of the micron particles is 0.01 to 0.02 percent, the content of the submicron particles is 0.01 to 0.02 percent, and the content of the nano particles is 0.1 to 0.2 percent; size and number control: micron meterThe particles have a size of 0.5 to 1.5 μm and a number of 1013～1014Per m3(ii) a The sub-micron particles have a size of 0.1 to 0.5 μm and a number of 1017～1018Per m3(ii) a The particle size of the nano particles is 10-20 nm, and the number of the nano particles is 1023～1024Per m3So that various particles have good strengthening effect on low-activation steel.
According to the method for preparing the multi-scale particle reinforced low-activation steel, different particles are introduced by using a ball milling process, the using amount and the size of each particle are optimized, and the multi-scale particles are uniformly distributed in a low-activation steel matrix through laser printing forming, so that the strength of the low-activation steel is obviously improved, and the method has an important significance for improving the safety of a fusion reactor. Wherein the powder A is nanometer Y2O3The powder obtained by ball milling and solid solution of the nano Ti powder and the low activation steel powder leads Y-Ti-O particles to be introduced into the low activation steel, and the Y-Ti-O particles have better wettability with the low activation steel, thereby being beneficial to the uniform distribution of subsequent strengthening phase particles and leading the particles to be uniformly dispersed and distributed in the low activation matrix.
Further, the size of the low-activation steel powder is 50-100 mu m, and the nano Y is2O3The size of the powder is 15-30 nm, the size of the nano Ti powder is 15-20 nm, the granularity is reduced once after the low-activation steel is subjected to multiple ball milling, and the powder with larger granularity is beneficial to saving the preparation cost.
Further, nano Y2O3In the ball milling process of the nano Ti powder and the low-activation steel powder, the ball-to-material ratio is 10 (1-1.5), and the ball-to-material ratio is high, so that the ball milling efficiency is improved. The ball milling speed is 500-550 r/min, and Y is obtained by high-speed ball milling2O3Reacting with Ti powder to generate Y-Ti-O and partially dissolving the Y-Ti-O into the low activation steel matrix, wherein the addition of the Ti powder can improve Y2O3The solid solubility of the titanium-containing alloy is 10-15 h, the solid solution reaction can be maximized, and the oxidation of Ti and steel powder can be prevented due to the fact that the ball milling atmosphere is inert.
Further, nano Y2O3Y is obtained by ball milling of nano Ti powder and low-activation steel powder2O3The mass ratio of the nano Ti powder to the low-activation steel powder is (0.5-1): (0.5-1): 100, at which ratio Y is favoured2O3And the powder is fed by gas in the subsequent laser printing forming process, so that the powder loss is caused, the ball milling is carried out according to the proportion, the mass fraction of the nano particles in the final forming body can be obtained, and the content of various particles is ensured.
Further, submicron Y2O3In the process of carrying out ball milling and solid solution on the powder A, the ball-material ratio is 5 (1-1.5), the ball milling rotating speed is 300-350 r/min, the ball milling time is 2-3 h, and the added submicron Y can be ensured under the short-time medium-speed ball milling2O3The particles do not react with the Ti remaining in the powder a. Because the powder is fed by gas in the subsequent powder feeding laser process, the loss of the powder is caused, under the preferable powder feeding process, the proportion which is 2 times higher than that of the target components is adopted for material mixing and ball milling, the mass fraction of the nano particles in the multi-scale particle reinforced low-activation steel can be finally obtained, and the ball milling atmosphere is inert atmosphere and can prevent the oxidation of Ti and steel powder.
Furthermore, in the process of ball milling and mixing the micron particles and the powder B, the ball-material ratio is 5 (1-1.5), the ball milling rotating speed is 100-150 r/min, the ball milling time is 2-3 h, and the added TiN or Ti can be ensured by ball milling at a short time and a medium speed2O3The particles do not react with other particles in the steel, the loss of powder can be caused because gas is adopted for powder feeding in the subsequent powder feeding laser process, and under the preferable powder feeding process, the mass fraction of the nano particles in the multi-scale particle reinforced low-activation steel can be finally obtained by adopting the proportion which is 100 times higher than that of the target components for material mixing and ball milling.
Furthermore, in the process of carrying out laser printing forming in the inert gas atmosphere of the powder C, the laser power is 3.5-4 kW, the powder feeding speed is 1.2-1.5 kg/h, and the scanning speed is 1000m/min, wherein the parameters are optimized in the invention, so that the uniform distribution of multi-scale particles in a low-activation steel matrix and the final content of various particles in steel can be ensured.
Furthermore, a large amount of thermal stress can remain in the printed steel sample and needs to be removed, so that the formed body is subjected to high-temperature stress regulation and control, the formed body is heated to 950-980 ℃ during regulation and control, the temperature is kept for 2-2.5 hours, and then cooling is performed, the thermal stress in the formed body can be removed under the process, and meanwhile, the growth of crystal grains is also avoided under the heat preservation system.
Detailed Description
The present invention will be further described with reference to the following examples.
The invention relates to multi-scale particle reinforced low-activation steel and a preparation method thereof, which comprises the following steps:
(1) ball-milling and solid-dissolving nano particles: nano Y2O3Placing the nano Ti powder and the low-activation steel powder in a ball mill for high-speed ball milling and solid solution; wherein the low-activation steel powder is Eurofer97 steel powder, 9Cr2WVTa steel powder, F82H steel powder, JLF-1 steel powder, CLAM steel powder, CLF-1 steel powder or ARAA steel powder, the size of the low-activation steel powder is 50-100 mu m, and the nano Y is2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm; nanometer Y2O3The mass ratio of the nano Ti powder to the low-activation steel powder is (0.5-1): (0.5-1) 100; the ball-material ratio of the high-speed ball milling is 10: 1-1.5, the rotating speed is 500-550 r/min, the ball milling time is 10-15 h, and the ball milling atmosphere is inert atmosphere;
(2) ball-milling and solid-dissolving submicron particles: mixing sub-micron Y2O3Carrying out medium-speed ball milling and solid solution on the powder prepared in the step 1, wherein the ball-material ratio of the medium-speed ball milling is 5 (1-1.5), the rotating speed is 300-350 r/min, the ball milling time is 2-3 h, and the ball milling atmosphere is inert atmosphere; submicron Y2O3The mass of the powder is 0.02-0.04% of the mass of the powder prepared in the step (1);
(3) and (3) carrying out ball milling and mixing on micron particles: mixing TiN particles or Ti2O3Performing low-speed ball milling and mixing on the powder prepared in the step 2 by particle neutralization, wherein the ball-material ratio of the low-speed ball milling is 5 (1-1.5), the rotating speed is 100-150 r/min, the ball milling time is 2-3 h, and the ball milling atmosphere is inert atmosphere; the addition amount of the micron particles is 1 to 2 percent of the mass of the powder prepared in the step (2);
(4) carrying out powder feeding laser printing molding on the powder obtained in the step (3): the laser power is 3.5-4 kW, the powder feeding speed is 1.2-1.5 kg/h, the scanning speed is 1000m/min, and argon protection is performed in the whole printing process;
(5) and (3) carrying out high-temperature stress regulation on the formed body obtained in the step (4): and (3) placing the formed steel sample at 950-980 ℃ for heat preservation for 2-2.5 h.
In the multi-scale particle reinforced low-activation steel prepared by the invention, the micron particles (namely TiN or Ti) are calculated by mass percent2O3Particles) of 0.01 to 0.02%, a particle size of 0.5 to 1.5 μm and a number of 1013～1014Per m3(ii) a Submicron particles (i.e. Y)2O3Particles) of 0.01 to 0.02%, a particle size of 0.1 to 0.5 μm and a number of 1017～1018Per m3(ii) a The content of the nano particles is 0.1-0.2%, the particle size is 10-20 nm, and the number is 1023～1024Per m3. Wherein, the micron and submicron particles mainly play a role in pinning austenite grain boundary refined grains and are used as nucleation particles of acicular ferrite to refine the grains, and the submicron and nano particles play a role in pinning dislocation to strengthen the second phase.
Example 1
(1) Ball-milling and solid-dissolving nano particles: nano Y2O3Placing the nano Ti powder and the low-activation steel powder in a ball mill for high-speed ball milling and solid solution; wherein the low-activation steel powder is Eurofer97 steel powder, the size of the low-activation steel powder is 50-100 mu m, and the nano Y is2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm; nanometer Y2O3The mass ratio of the nano Ti powder to the low-activation steel powder is 0.5: 1: 100; the ball-material ratio of the high-speed ball milling is 10:1, the rotating speed is 500 r/min, the ball milling time is 15h, and the ball milling atmosphere is inert atmosphere;
(2) ball-milling and solid-dissolving submicron particles: mixing sub-micron Y2O3Carrying out medium-speed ball milling and solid solution on the powder prepared in the step 1, wherein the ball-material ratio of the medium-speed ball milling is 5:1, the rotating speed is 300 r/min, the ball milling time is 3h, and the ball milling atmosphere is inert atmosphere; submicron Y2O3The mass of (2) is 0.02% of the mass of the powder prepared in the step (1);
(3) and (3) carrying out ball milling and mixing on micron particles: performing low-speed ball milling on the TiN particles and the powder prepared in the step 2 to mix the materials, wherein the ball-to-material ratio of the low-speed ball milling is 5:1, the rotating speed is 100 r/min, the ball milling time is 3 hours, and the ball milling atmosphere is inert atmosphere; the addition amount of the micron particles is 2 percent of the mass of the powder prepared in the step (2);
(4) carrying out powder feeding laser printing molding on the powder obtained in the step (3): the laser power is 3.5kW, the powder feeding speed is 1.2kg/h, the scanning speed is 1000m/min, and argon protection is carried out in the whole printing process;
(5) and (3) carrying out high-temperature stress regulation on the formed body obtained in the step (4): and (3) placing the formed steel sample at 950 ℃ for heat preservation for 2.5 h.
In the multi-scale particle reinforced low activation steel prepared by the embodiment, the content of the micron particles (namely TiN) is 0.016 percent by mass, the particle size is 0.5-1.5 mu m, and the number is 9.8 multiplied by 1013Per m3(ii) a Submicron particles (i.e. Y)2O3Particles) of 0.013%, the particle size of 0.1 to 0.5 μm, and the number of particles of 1.8X 1017Per m3(ii) a The content of the nano particles is 0.16 percent, the particle size is 10-20 nm, and the number is 4.9 multiplied by 1023Per m3。
The table for testing the properties of the multi-scale particle reinforced low activation steel prepared in this example is shown in table 1.
Example 2
(1) Ball-milling and solid-dissolving nano particles: nano Y2O3Placing the nano Ti powder and the low-activation steel powder in a ball mill for high-speed ball milling and solid solution; wherein the low-activation steel powder is Eurofer97 steel powder, the size of the low-activation steel powder is 50-100 mu m, and the nano Y is2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm; nanometer Y2O3The mass ratio of the nano Ti powder to the low-activation steel powder is 1: 0.5: 100; the ball-material ratio of the high-speed ball milling is 10:1.5, the rotating speed is 550 r/min, the ball milling time is 10, and the ball milling atmosphere is inert atmosphere;
(2) ball-milling and solid-dissolving submicron particles: mixing sub-micron Y2O3Carrying out medium-speed ball milling and solid solution on the powder prepared in the step 1, wherein the ball-material ratio of the medium-speed ball milling is 5:1.5, the rotating speed is 350 r/min, the ball milling time is 2h, and the ball milling atmosphere is inert atmosphere; submicron Y2O3The mass of (2) is 0.04% of the mass of the powder prepared in the step (1);
(3) and (3) carrying out ball milling and mixing on micron particles: performing low-speed ball milling on the TiN particles and the powder prepared in the step 2 to mix the materials, wherein the ball-to-material ratio of the low-speed ball milling is 5:1.5, the rotating speed is 150 r/min, the ball milling time is 2h, and the ball milling atmosphere is inert atmosphere; the addition amount of the micron particles is 1 percent of the mass of the powder prepared in the step (2);
(4) carrying out powder feeding laser printing molding on the powder obtained in the step (3): the laser power is 4kW, the powder feeding speed is 1.5kg/h, the scanning speed is 1000m/min, and argon protection is carried out in the whole printing process;
(5) and (3) carrying out high-temperature stress regulation on the formed body obtained in the step (4): and (3) placing the formed steel sample at 980 ℃ for heat preservation for 2 h.
In the multi-scale particle reinforced low activation steel prepared in the embodiment, the content of the micro particles (namely TiN particles) is 0.012 percent by mass, the particle size is 0.5-1.5 mu m, and the number is 1.2 multiplied by 1013Per m3(ii) a Submicron particles (i.e. Y)2O3Particles) of 0.019%, a particle size of 0.1 to 0.5 μm and a number of 8.6X 1017Per m3(ii) a The content of the nano particles is 0.14 percent, the particle size is 10-20 nm, and the number is 5.1 multiplied by 1023Per m3。
The table for testing the properties of the multi-scale particle reinforced low activation steel prepared in this example is shown in table 1.
Example 3
(1) Ball-milling and solid-dissolving nano particles: nano Y2O3Placing the nano Ti powder and the low-activation steel powder in a ball mill for high-speed ball milling and solid solution; wherein the low-activation steel powder is Eurofer97 steel powder, the size of the low-activation steel powder is 50-100 mu m, and the nano Y is2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm; nanometer Y2O3The mass ratio of the nano Ti powder to the low-activation steel powder is 0.6: (0.9: 100; ball-to-material ratio of high-speed ball milling is 10:1.3, the rotating speed is 535 r/min, the ball milling time is 13h, and the ball milling atmosphere is inert atmosphere;
(2) ball-milling and solid-dissolving submicron particles: mixing sub-micron Y2O3Carrying out medium-speed ball milling and solid solution on the powder prepared in the step 1, wherein the ball-material ratio of the medium-speed ball milling is 5:1.2, the rotating speed is 345 r/min, the ball milling time is 2.5h, and the ball milling atmosphere is inert atmosphere; submicron Y2O3The mass of the powder is 0.035% of the mass of the powder prepared in the step (1);
(3) and (3) carrying out ball milling and mixing on micron particles: mixing Ti2O3Performing low-speed ball milling and mixing on the particles and the powder prepared in the step 2, wherein the ball-material ratio of the low-speed ball milling is 5:1.25, the rotating speed is 135 r/min, the ball milling time is 2.5h, and the ball milling atmosphere is inert atmosphere; the addition amount of the micron particles is 1.6 percent of the mass of the powder prepared in the step (2);
(4) carrying out powder feeding laser printing molding on the powder obtained in the step (3): the laser power is 3.8kW, the powder feeding speed is 1.35kg/h, the scanning speed is 1000m/min, and argon protection is carried out in the whole printing process;
(5) and (3) carrying out high-temperature stress regulation on the formed body obtained in the step (4): and (3) placing the formed steel sample at 960 ℃ for heat preservation for 2.3 h.
In the multi-scale particle reinforced low activation steel prepared in the embodiment, the micron particles (i.e. Ti) are calculated by mass percentage2O3Particles) of 0.017%, a particle size of 0.5 to 1.5 μm and a number of 5.3X 1013Per m3(ii) a Submicron particles (i.e. Y)2O3Particles) in an amount of 0.018%, the particles having a size of 0.1 to 0.5 μm and a number of 8.4X 1017Per m3(ii) a The content of the nano particles is 0.14 percent, the particle size is 10-20 nm, and the number is 6.1 multiplied by 1023Per m3。
The table for testing the properties of the multi-scale particle reinforced low activation steel prepared in this example is shown in table 1.
Example 4
(1) Ball-milling and solid-dissolving nano particles: nano Y2O3Placing the nano Ti powder and the low-activation steel powder in a ball mill for high-speed ball milling and solid solution; wherein the low-activation steel powder is 9Cr2WVTa steel powder and is low in contentThe size of the activated steel powder is 50-100 mu m and the size of the activated steel powder is nano Y2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm; nanometer Y2O3The mass ratio of the nano Ti powder to the low-activation steel powder is 0.55: 1: 100; the ball-material ratio of the high-speed ball milling is 10:1.35, the rotating speed is 540 r/min, the ball milling time is 14h, and the ball milling atmosphere is inert atmosphere;
(2) ball-milling and solid-dissolving submicron particles: mixing sub-micron Y2O3Carrying out medium-speed ball milling and solid solution on the powder prepared in the step 1, wherein the ball-material ratio of the medium-speed ball milling is 5:1.2, the rotating speed is 330 revolutions per minute, the ball milling time is 2.5 hours, and the ball milling atmosphere is inert atmosphere; submicron Y2O3The mass of the powder is 0.035% of the mass of the powder prepared in the step (1);
(3) and (3) carrying out ball milling and mixing on micron particles: performing low-speed ball milling on the TiN particles and the powder prepared in the step 2 to mix the materials, wherein the ball-to-material ratio of the low-speed ball milling is 5:1.3, the rotating speed is 120 r/min, the ball milling time is 2.8h, and the ball milling atmosphere is inert atmosphere; the addition amount of the micron particles is 1.8 percent of the mass of the powder prepared in the step (2);
(4) carrying out powder feeding laser printing molding on the powder obtained in the step (3): the laser power is 3.8kW, the powder feeding speed is 1.4kg/h, the scanning speed is 1000m/min, and argon protection is carried out in the whole printing process;
(5) and (3) carrying out high-temperature stress regulation on the formed body obtained in the step (4): and (4) placing the formed steel sample at 970 ℃ for heat preservation for 2.2 h.
In the multi-scale particle reinforced low activation steel prepared by the embodiment, the content of the micron particles (namely TiN particles) is 0.017 percent by mass, the particle size is 0.5-1.5 mu m, and the number is 8.1 multiplied by 1013Per m3(ii) a Submicron particles (i.e. Y)2O3Particles) of 0.016%, particle size of 0.1-0.5 μm, and number of 7.1 × 1017Per m3(ii) a The content of the nano particles is 0.16 percent, the particle size is 10-20 nm, and the number is 6.4 multiplied by 1023Per m3。
The table for testing the properties of the multi-scale particle reinforced low activation steel prepared in this example is shown in table 1.
Example 5
(1) Ball-milling and solid-dissolving nano particles: nano Y2O3Placing the nano Ti powder and the low-activation steel powder in a ball mill for high-speed ball milling and solid solution; wherein the low-activation steel powder is F82H steel powder, the size of the low-activation steel powder is 50-100 mu m, and the nano Y is2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm; nanometer Y2O3The mass ratio of the nano Ti powder to the low-activation steel powder is 1: 0.5: 100; the ball-material ratio of the high-speed ball milling is 10:1.5, the rotating speed is 550 r/min, the ball milling time is 10h, and the ball milling atmosphere is inert atmosphere;
(2) ball-milling and solid-dissolving submicron particles: mixing sub-micron Y2O3Carrying out medium-speed ball milling and solid solution on the powder prepared in the step 1, wherein the ball-material ratio of the medium-speed ball milling is 5:1.5, the rotating speed is 350 r/min, the ball milling time is 2h, and the ball milling atmosphere is inert atmosphere; submicron Y2O3The mass of (2) is 0.04% of the mass of the powder prepared in the step (1);
(3) and (3) carrying out ball milling and mixing on micron particles: mixing Ti2O3Performing low-speed ball milling and mixing on the particles and the powder prepared in the step 2, wherein the ball-material ratio of the low-speed ball milling is 5:1.5, the rotating speed is 150 r/min, the ball milling time is 2h, and the ball milling atmosphere is inert atmosphere; the addition amount of the micron particles is 1 percent of the mass of the powder prepared in the step (2);
(4) carrying out powder feeding laser printing molding on the powder obtained in the step (3): the laser power is 4kW, the powder feeding speed is 1.5kg/h, the scanning speed is 1000m/min, and argon protection is carried out in the whole printing process;
(5) and (3) carrying out high-temperature stress regulation on the formed body obtained in the step (4): and (3) placing the formed steel sample at 980 ℃ for heat preservation for 2 h.
In the multi-scale particle reinforced low activation steel prepared in the embodiment, the micron particles (i.e. Ti) are calculated by mass percentage2O3Particles) of 0.013%, the particle size of 0.5 to 1.5 μm, and the number of particles of 6.7X 1013Per m3(ii) a Submicron particles (i.e. Y)2O3Particles) of 0.019%, a particle size of 0.1 to 0.5 μm and a number of 7.3X 1017Per m3(ii) a The content of the nano particles is 0.13%, the particle size is 10-20 nm, and the number is 4.9×1023Per m3。
The table for testing the properties of the multi-scale particle reinforced low activation steel prepared in this example is shown in table 1.
Example 6
(1) Ball-milling and solid-dissolving nano particles: nano Y2O3Placing the nano Ti powder and the low-activation steel powder in a ball mill for high-speed ball milling and solid solution; wherein the low-activation steel powder is JLF-1 steel powder, the size of the low-activation steel powder is 50-100 mu m, and the nano Y is2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm; nanometer Y2O3The mass ratio of the nano Ti powder to the low-activation steel powder is 1: 1: 100; the ball-material ratio of the high-speed ball milling is 10:1, the rotating speed is 500 r/min, the ball milling time is 10h, and the ball milling atmosphere is inert atmosphere;
(2) ball-milling and solid-dissolving submicron particles: mixing sub-micron Y2O3Carrying out medium-speed ball milling and solid solution on the powder prepared in the step 1, wherein the ball-material ratio of the medium-speed ball milling is 5:1.5, the rotating speed is 350 r/min, the ball milling time is 2h, and the ball milling atmosphere is inert atmosphere; submicron Y2O3The mass of (2) is 0.02% of the mass of the powder prepared in the step (1);
(3) and (3) carrying out ball milling and mixing on micron particles: performing low-speed ball milling and mixing on the TiN particles and the powder prepared in the step 2, wherein the ball-material ratio of the low-speed ball milling is 5:1, the rotating speed is 150 r/min, the ball milling time is 2 hours, and the ball milling atmosphere is inert atmosphere; the addition amount of the micron particles is 2 percent of the mass of the powder prepared in the step (2);
(4) carrying out powder feeding laser printing molding on the powder obtained in the step (3): the laser power is 3.5kW, the powder feeding speed is 1.2kg/h, the scanning speed is 1000m/min, and argon protection is carried out in the whole printing process;
(5) and (3) carrying out high-temperature stress regulation on the formed body obtained in the step (4): and (3) placing the formed steel sample at 950 ℃ for heat preservation for 2.5 h.
In the multi-scale particle reinforced low activation steel prepared by the embodiment, the content of the micron particles (namely TiN particles) is 0.019 percent by mass, the particle size is 0.5-1.5 mu m, and the number is 8.2 multiplied by 1013～1014Per m3(ii) a Submicron particles (i.e. Y)2O3Particles) of 0.012%, a particle size of 0.1 to 0.5 μm, and a number of 3.9 × 1017Per m3(ii) a The content of the nano particles is 0.19 percent, the particle size is 10-20 nm, and the number is 8.7 multiplied by 1023Per m3。
The table for testing the properties of the multi-scale particle reinforced low activation steel prepared in this example is shown in table 1.
Example 7
(1) Ball-milling and solid-dissolving nano particles: nano Y2O3Placing the nano Ti powder and the low-activation steel powder in a ball mill for high-speed ball milling and solid solution; wherein the low-activation steel powder is CLAM steel powder, the size of the low-activation steel powder is 50-100 mu m, and the nano Y is2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm; nanometer Y2O3The mass ratio of the nano Ti powder to the low-activation steel powder is 0.5: 0.5: 100; the ball-material ratio of the high-speed ball milling is 10:1.5, the rotating speed is 500 r/min, the ball milling time is 15h, and the ball milling atmosphere is inert atmosphere;
(2) ball-milling and solid-dissolving submicron particles: mixing sub-micron Y2O3Carrying out medium-speed ball milling and solid solution on the powder prepared in the step 1, wherein the ball-material ratio of the medium-speed ball milling is 5:1.5, the rotating speed is 350 r/min, the ball milling time is 2h, and the ball milling atmosphere is inert atmosphere; submicron Y2O3The mass of (2) is 0.02% of the mass of the powder prepared in the step (1);
(3) and (3) carrying out ball milling and mixing on micron particles: mixing Ti2O3Performing low-speed ball milling and mixing on the particles and the powder prepared in the step 2, wherein the ball-material ratio of the low-speed ball milling is 5:1.5, the rotating speed is 150 r/min, the ball milling time is 2h, and the ball milling atmosphere is inert atmosphere; the addition amount of the micron particles is 2 percent of the mass of the powder prepared in the step (2);
(4) carrying out powder feeding laser printing molding on the powder obtained in the step (3): the laser power is 4kW, the powder feeding speed is 1.5kg/h, the scanning speed is 1000m/min, and argon protection is carried out in the whole printing process;
(5) and (3) carrying out high-temperature stress regulation on the formed body obtained in the step (4): and (3) placing the formed steel sample at 980 ℃ for heat preservation for 2 h.
The multiscale prepared in this exampleIn the particle-reinforced low activation steel, the particles are micron particles (i.e. Ti) in mass percentage2O3Particles) of 0.019%, a particle size of 0.5 to 1.5 μm and a number of 8.8X 1013Per m3(ii) a Submicron particles (i.e. Y)2O3Particles) of 0.012%, a particle size of 0.1 to 0.5 μm and a number of 3.6 × 1017Per m3(ii) a The content of the nano particles is 0.11 to 0.2 percent, the particle size is 10 to 20nm, and the number is 4.7 multiplied by 1023Per m3。
The table for testing the properties of the multi-scale particle reinforced low activation steel prepared in this example is shown in table 1.
Example 8
(1) Ball-milling and solid-dissolving nano particles: nano Y2O3Placing the nano Ti powder and the low-activation steel powder in a ball mill for high-speed ball milling and solid solution; wherein the low-activation steel powder is CLF-1 steel powder, the size of the low-activation steel powder is 50-100 mu m, and the nano Y is2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm; nanometer Y2O3The mass ratio of the nano Ti powder to the low-activation steel powder is 0.8: 0.8: 100; the ball-material ratio of the high-speed ball milling is 10:1.3, the rotating speed is 530 r/min, the ball milling time is 14h, and the ball milling atmosphere is inert atmosphere;
(2) ball-milling and solid-dissolving submicron particles: mixing sub-micron Y2O3Carrying out medium-speed ball milling and solid solution on the powder prepared in the step 1, wherein the ball-material ratio of the medium-speed ball milling is 5:1.35, the rotating speed is 320 r/min, the ball milling time is 2.5h, and the ball milling atmosphere is inert atmosphere; submicron Y2O3The mass of (2) is 0.036% of the mass of the powder prepared in the step (1);
(3) and (3) carrying out ball milling and mixing on micron particles: mixing Ti2O3Performing low-speed ball milling and mixing on the particles and the powder prepared in the step 2, wherein the ball-material ratio of the low-speed ball milling is 5:1.3, the rotating speed is 140 r/min, the ball milling time is 2.4h, and the ball milling atmosphere is inert atmosphere; the addition amount of the micron particles is 1.6 percent of the mass of the powder prepared in the step (2);
(4) carrying out powder feeding laser printing molding on the powder obtained in the step (3): the laser power is 3.8kW, the powder feeding speed is 1.35kg/h, the scanning speed is 1000m/min, and argon protection is carried out in the whole printing process;
(5) and (3) carrying out high-temperature stress regulation on the formed body obtained in the step (4): and (3) placing the formed steel sample at 975 ℃ for heat preservation for 2.25 h.
In the multi-scale particle reinforced low activation steel prepared in the embodiment, the micron particles (i.e. Ti) are calculated by mass percentage2O3Particles) of 0.014%, particle size of 0.5 to 1.5 μm and number of 4.8X 1013Per m3(ii) a Submicron particles (i.e. Y)2O3Particles) of 0.015% by weight, a particle size of 0.1 to 0.5 μm and a number of 5.5X 1017Per m3(ii) a The content of the nano particles is 0.15 percent, the particle size is 10-20 nm, and the number is 6.8 multiplied by 1023Per m3。
The table for testing the properties of the multi-scale particle reinforced low activation steel prepared in this example is shown in table 1.
Example 9
(1) Ball-milling and solid-dissolving nano particles: nano Y2O3Placing the nano Ti powder and the low-activation steel powder in a ball mill for high-speed ball milling and solid solution; wherein the low-activation steel powder is ARAA steel powder, the size of the low-activation steel powder is 50-100 mu m, and the nano Y is2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm; nanometer Y2O3The mass ratio of the nano Ti powder to the low-activation steel powder is 1: 0.5: 100; the ball-material ratio of the high-speed ball milling is 10:1, the rotating speed is 500 r/min, the ball milling time is 10h, and the ball milling atmosphere is inert atmosphere;
(2) ball-milling and solid-dissolving submicron particles: mixing sub-micron Y2O3Carrying out medium-speed ball milling and solid solution on the powder prepared in the step 1, wherein the ball-material ratio of the medium-speed ball milling is 5:1.5, the rotating speed is 350 r/min, the ball milling time is 2h, and the ball milling atmosphere is inert atmosphere; submicron Y2O3The mass of (2) is 0.04% of the mass of the powder prepared in the step (1);
(3) and (3) carrying out ball milling and mixing on micron particles: mixing Ti2O3And (3) performing low-speed ball milling and mixing on the powder prepared in the step (2) in particle neutralization, wherein the ball-material ratio of low-speed ball milling is 5:1.5, the rotating speed is 150 r/min, the ball milling time is 2h, and the ball milling atmosphere isIs an inert atmosphere; the addition amount of the micron particles is 2 percent of the mass of the powder prepared in the step (2);
(4) carrying out powder feeding laser printing molding on the powder obtained in the step (3): the laser power is 3.5kW, the powder feeding speed is 1.2kg/h, the scanning speed is 1000m/min, and argon protection is carried out in the whole printing process;
(5) and (3) carrying out high-temperature stress regulation on the formed body obtained in the step (4): and (3) placing the formed steel sample at 980 ℃ for heat preservation for 2 h.
In the multi-scale particle reinforced low activation steel prepared in the embodiment, the micron particles (i.e. Ti) are calculated by mass percentage2O3Particles) in an amount of 0.018%, the particles having a size of 0.5 to 1.5 μm and a number of 7.9X 1013Per m3(ii) a Submicron particles (i.e. Y)2O3Particles) in an amount of 0.018%, the particles having a size of 0.1 to 0.5 μm and a number of 7.6X 1017Per m3(ii) a The content of the nano particles is 0.14 percent, the particle size is 10-20 nm, and the number is 3.1 multiplied by 1023Per m3。
The table for testing the properties of the multi-scale particle reinforced low activation steel prepared in this example is shown in table 1.
TABLE 1
Figure BDA0003047095610000141
As can be seen from Table 1, the multi-scale particle reinforced low-activation steel has excellent normal-temperature and high-temperature mechanical properties and smaller grain size before irradiation, the yield strength at room temperature before and after irradiation is far higher than that of the traditional low-activation steel (550MPa), the mechanical properties of the steel after irradiation are not greatly reduced or increased, and the effects of improving the mechanical properties and the anti-irradiation properties of the steel are realized.
In conclusion, the invention introduces various particles with different sizes into the steel to strengthen the low activation steel. The micron and submicron particles can pin the grain boundary to play a role in fine crystal strengthening, and the submicron and nanoparticles pin the dislocation to play a role in second phase strengthening. Different particles are introduced through different short-time ball milling processes, the using amount and the size of each scale of particles are optimized, and the multi-scale particles are uniformly distributed in the low-activation steel matrix through the powder feeding laser melting technology, so that the strength of the low-activation steel is obviously improved, and the method has important significance for improving the safety of a fusion reactor.

Claims (4)

1. The multi-scale particle reinforced low-activation steel is characterized by comprising a low-activation matrix and micro particles, sub-micro particles and nano particles which are uniformly distributed in the low-activation matrix, wherein the micro particles are TiN or Ti2O3The submicron particle is Y2O3The nano particles are Y-Ti-O;
in the multi-scale particle reinforced low-activation steel, the content of micron particles is 0.01-0.02 percent, the content of submicron particles is 0.01-0.02 percent, and the content of nano particles is 0.1-0.2 percent by mass percent;
the size of the microparticles is more than 0.5 μm and less than or equal to 1.5 μm, and the number of the microparticles is 1013~1014Per m3(ii) a The size of the sub-micron particles is more than or equal to 0.1 μm and less than or equal to 0.5 μm, and the number of the sub-micron particles is 1017~1018Per m3(ii) a The particle size of the nano particles is 10-20 nm, and the number of the nano particles is 1023~1024Per m3。
2. The multi-scale particle reinforced low activation steel as claimed in claim 1, wherein the low activation matrix is Eurofer97, 9Cr2WVTa, F82H, JLF-1, CLAMs, CLF-1 or ARAA.
3. A method for preparing the multi-scale particle reinforced low activation steel of claim 1 or 2, comprising the steps of:
performing laser printing forming in an inert gas atmosphere of powder C to obtain a forming body;
performing high-temperature stress regulation and control on the formed body;
wherein, the powder C is obtained by ball milling and mixing micron particles and the powder B; the powder B is submicronRice Y2O3Performing ball milling and solid solution on the powder A to obtain the powder A; the powder A is nanometer Y2O3Carrying out ball milling and solid solution on the nano Ti powder and the low-activation steel powder to obtain the low-activation steel powder;
nanometer Y2O3In the ball milling process of the nano Ti powder and the low-activation steel powder, the ball-material ratio is 10 (1-1.5), the ball milling speed is 500-550 r/min, the ball milling time is 10-15 h, and the ball milling atmosphere is inert atmosphere;
nanometer Y2O3Y is obtained by ball milling of nano Ti powder and low-activation steel powder2O3The mass ratio of the nano Ti powder to the low-activation steel powder is (0.5-1): (0.5-1) 100;
submicron Y2O3In the process of carrying out ball milling and solid solution on the powder A, the ball-material ratio is 5 (1-1.5), the ball milling rotating speed is 300-350 r/min, the ball milling time is 2-3 h, and the ball milling atmosphere is inert atmosphere;
submicron Y2O3The mass of the powder A is 0.02% -0.04% of that of the powder A;
in the process of ball milling and mixing the micron particles and the powder B, the ball-material ratio is 5 (1-1.5), the ball milling rotating speed is 100-150 r/min, the ball milling time is 2-3 h, and the ball milling atmosphere is inert atmosphere;
the mass of the micron particles is 1% -2% of that of the powder B;
in the process of carrying out laser printing forming in an inert gas atmosphere of powder C, the laser power is 3.5-4 kW, the powder feeding speed is 1.2-1.5 kg/h, the scanning speed is 1000m/min, and argon protection is carried out in the whole printing process;
the high-temperature stress regulating process of the formed body comprises the following steps: and heating the formed body to 950-980 ℃, preserving heat for 2-2.5 hours, and then cooling.
4. The method for preparing the multi-scale particle reinforced low activation steel according to claim 1 or 2, wherein the size of the low activation steel powder is 50-100 μm and the size of nano-Y is2O3The size of the nano Ti powder is 15-30 nm, and the size of the nano Ti powder is 15-20 nm.
CN202110475932.1A 2021-04-29 2021-04-29 Multi-scale particle reinforced low-activation steel and preparation method thereof Active CN113215480B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110475932.1A CN113215480B (en) 2021-04-29 2021-04-29 Multi-scale particle reinforced low-activation steel and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110475932.1A CN113215480B (en) 2021-04-29 2021-04-29 Multi-scale particle reinforced low-activation steel and preparation method thereof

Publications (2)

Publication Number Publication Date
CN113215480A CN113215480A (en) 2021-08-06
CN113215480B true CN113215480B (en) 2021-12-14

Family

ID=77090434

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110475932.1A Active CN113215480B (en) 2021-04-29 2021-04-29 Multi-scale particle reinforced low-activation steel and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113215480B (en)

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4963200A (en) * 1988-04-25 1990-10-16 Doryokuro Kakunenryo Kaihatsu Jigyodan Dispersion strengthened ferritic steel for high temperature structural use
JP4413549B2 (en) * 2002-08-08 2010-02-10 独立行政法人 日本原子力研究開発機構 Method for producing martensitic oxide dispersion strengthened steel with excellent high temperature strength
JP3792624B2 (en) * 2002-08-08 2006-07-05 核燃料サイクル開発機構 Method for producing ferritic oxide dispersion strengthened steel with coarse grain structure and excellent high temperature creep strength
CN101328562B (en) * 2008-07-17 2011-01-26 中国科学院等离子体物理研究所 Oxide dispersion strengthening low activity martensitic steel material and preparation thereof
CN101619408B (en) * 2009-07-28 2011-03-30 北京科技大学 Preparation method of nanoparticles formed in molten steel
CN107058852B (en) * 2017-02-20 2018-07-13 天津大学 A method of residual ferrite in refinement oxide dispersion intensifying martensite steel
CN108796345B (en) * 2017-11-10 2020-05-19 中国科学院金属研究所 Oxidation preparation method of nano composite oxide dispersion strengthening Fe-based alloy

Also Published As

Publication number Publication date
CN113215480A (en) 2021-08-06

Similar Documents

Publication Publication Date Title
CN111940723B (en) Nano ceramic metal composite powder for 3D printing and application
CN108080644B (en) Powder metallurgy preparation method of high-strength toughened metal-based composite material
CN108950343B (en) WC-based hard alloy material based on high-entropy alloy and preparation method thereof
WO2022041255A1 (en) Method for preparing nano-phase reinforced nickel-based high-temperature alloy using micron ceramic particles
CN112170854B (en) Method for preparing nano spherical oxide dispersion strengthening phase
CN105274445B (en) A kind of oxide dispersion intensifying low activation steel and preparation method thereof
CN112647009A (en) High-strength high-wear-resistance medium-entropy alloy and preparation method thereof
CN112063907B (en) Multi-principal-element high-temperature alloy and preparation method thereof
CN104630639A (en) Nano yttrium nitride dispersed reinforced iron-based alloy and preparation method
CN107058852B (en) A method of residual ferrite in refinement oxide dispersion intensifying martensite steel
CN113278895A (en) High-strength FeCrAl-based alloy
CN114774727B (en) Preparation method of nano zirconium dioxide reinforced NbMoTaW refractory high-entropy alloy
CN107952966A (en) The preparation method at spherical titanium aluminium-based alloyed powder end
CN113444962B (en) Method for preparing multi-nano-phase reinforced iron-based alloy
CN113215480B (en) Multi-scale particle reinforced low-activation steel and preparation method thereof
CN106399742B (en) A kind of nano dispersion reinforced copper alloy of Cu-NbC and preparation method thereof
CN111378870B (en) SPS sintering titanium-based composite material and preparation method thereof
CN115522144B (en) Preparation method of high-strength tungsten alloy
CN110066952B (en) Preparation method of zirconium oxide reinforced molybdenum alloy bar
CN116944518A (en) Method for forming CuAlFe shape memory alloy structure by ultra-fine SLM (selective laser melting)
CN113215470B (en) Nano-scale oxide reinforced low-activation steel composite material and preparation method thereof
CN108262485B (en) Industrial in-situ synthesis method of W-based composite powder capable of adding WC strengthening phase
CN115011838A (en) Rare earth modified titanium alloy and preparation method and application thereof
CN113231648B (en) High-strength austenitic stainless steel and preparation method thereof
CN113444981B (en) Method for preparing ODS-FeCrAl-based alloy

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant