CN113462949B - Method for preparing dispersion oxide reinforced section steel based on powder metallurgy process - Google Patents
Method for preparing dispersion oxide reinforced section steel based on powder metallurgy process Download PDFInfo
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 38
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- 239000006185 dispersion Substances 0.000 title claims abstract description 16
- 238000004663 powder metallurgy Methods 0.000 title claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 84
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- 239000000463 material Substances 0.000 claims abstract description 21
- 239000011159 matrix material Substances 0.000 claims abstract description 20
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 35
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- 238000000227 grinding Methods 0.000 claims description 11
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- 239000011812 mixed powder Substances 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 238000002490 spark plasma sintering Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
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- 229910001566 austenite Inorganic materials 0.000 abstract description 4
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- 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
- C22C33/0235—Starting from compounds, e.g. oxides
-
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
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- 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
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- 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
-
- 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
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/001—Austenite
Abstract
The invention discloses a method for preparing dispersion oxide strengthened steel based on a powder metallurgy process, which belongs to the technical field of preparation of ODS steel by applying powder metallurgy to 316L powder as a matrix and adding Y powder and Fe2O3The powder is used for improving the mechanical property of the material. In the preparation process, the proportion of the mixed components is limited, so that Y powder and Fe powder2O3Powder reacts to generate Y2O3Uniformly mixing the mixture with a matrix, and gradually compacting the sintered composite material through intermittent ball milling; meanwhile, the sintering process of the large-amplitude temperature rise program is combined with the heat preservation and pressure maintaining process, so that Y is enabled to be2O3The aggregate grows in the crystal grains and in the crystal boundary, improves the functions of pinning dislocation and the crystal boundary, promotes the grain size to be maintained in a small range, and improves the mechanical property of the austenite ODS steel material.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a preparation technology for preparing dispersion oxide reinforced section steel.
Background
The 316L steel, as a Cr-Ni-Mo type ultra-low carbon stainless steel, has very excellent performance of resisting corrosion of sulfur and compounds thereof, non-oxidizing acid and organic acid, and in addition, has very excellent ductility, and the plastic deformation amount at normal temperature can reach 40%. However, the tensile strength (about 520MPa) and the yield strength (about 205MPa) of the 316L stainless steel are low, and therefore, the method cannot be applied to a supporting member with a large stress in practical application, and therefore, the method for obviously improving the mechanical property of the 316L stainless steel is particularly critical.
As a preferential candidate material for the fourth generation nuclear reactor vessel sheath, oxide dispersion strengthened steel (namely ODS steel) has excellent high-temperature creep property, neutron irradiation resistance and high-temperature mechanical property. By introducing stable nano oxide particles into the matrix, the particles can block dislocation movement and grain boundary migration in the service process, and further the comprehensive performance of the material is improved. However, although the introduction of nano-oxides into 316L steel can improve the tensile strength and yield strength of the material, the pinning effect of the oxides can greatly reduce the plasticity of the material. Therefore, how to continuously improve the mechanical properties of the 316L steel while ensuring the ductility and the toughness becomes a problem to be considered in the performance development of the 316L steel.
Disclosure of Invention
The invention aims to provide a powder metallurgy process for preparing dispersion oxide strengthened steel so as to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a method for preparing dispersion oxide strengthened section steel based on a powder metallurgy process, which takes 316L powder as a matrix and Y powder and Fe powder2O3The powder is used as reinforcing agent. Y powder and Fe in the process of mixing2O3Powder reacts to generate Y2O3And uniformly mixing with the matrix, the composite material is gradually densified in the sintering process, Y2O3The crystal grains are separated out again in the crystal grains and at the crystal boundary to play the role of pinning dislocation and the crystal boundary, and the crystal grains are not grown much by the rapid sintering process, so that the mechanical property of the material is improved together.
Further, the method for preparing the dispersion oxide strengthened steel section based on the powder metallurgy process comprises the following steps:
(1) adding Y powder and Fe into 316L powder2O3Powdering to produce Y2O3The mass fraction in the system is 0.20-0.50%, and the powder is uniformly mixed;
(2) placing the mixed powder obtained in the step (1) in a ball milling tank, packaging after oxygen discharge, performing ball milling on the mixed powder in an inert gas atmosphere, performing ball milling on the mixed powder in the inert gas atmosphere, ensuring that the reaction is fully performed, and generating Y2O3Thinning and uniformly dispersing with matrix powder;
(3) and putting the ball-milled powder into a die, putting the die into a hearth of a discharge plasma sintering furnace, pressurizing and vacuumizing, electrifying for discharge plasma sintering, and preserving heat after sintering is finished so as to activate the surfaces of powder particles and fully diffuse the powder particles to form a uniform and compact structure.
The particle size range of the 316L powder is 50-100 mu m, the particle size range of the Y powder is 50-100 mu m, and the Fe powder2O3The particle size of the powder is 50-200nm, and the Y powder and Fe powder2O3The powder molar ratio was 2: 1.
Further, argon or helium is used for oxygen discharge in the ball milling process in the step (2), the rotation speed of the ball mill in the step (2) is controlled at 200-; the ball milling time is set to be 20-80 hours, preferably 30-40 hours, so that the ball milling time is shortened as much as possible on the basis that the reaction can be fully carried out and the powder is uniformly mixed, and the pollution caused by the loss of the grinding balls and the tank body in the ball milling process is reduced.
Further, in the step (2), the 316L pre-alloyed powder accounts for 99.25-99.70 wt%, the Y powder accounts for 0.157-0.400 wt%, and the Fe powder accounts for2O3The powder accounts for 0.140 to 0.350 weight percent, and Y powder and Fe are added2O3The powder molar ratio is 2:1, and the ball-to-material ratio in the ball milling process is 5-10: 1, preventing too high a pellet-to-feed ratio also leads to powder blocking and reduces the powder yield.
Furthermore, the ball milling mode in the step (2) is intermittent ball milling, the ball milling is carried out for 1-2 hours, the intermittent time is 0.5 hour, and the serious heating condition in the high-energy ball milling process is prevented in consideration of the bearing capacity of a ball milling tank and steel balls.
Further, the pressurizing pressure of the die in the spark plasma sintering furnace in the step (3) is 30-50 MPa.
Further, the temperature rise rate of the spark plasma sintering in the step (3) is 50-100 ℃/min, the sintering temperature is 850-.
The invention discloses the following technical effects:
the preparation method adopts a powder metallurgy method to ensure that the added Y and Fe2O3Fully react to generate nano-scale Y2O3The particles are dispersed in the austenite matrix, and the compact ODS-316L steel with uniform structure is obtained by spark plasma sintering. By observing the structure and testing the performance of the ODS steel obtained by the method, the nanoscale Fe obtained by the reaction ball milling in the method can be obtained2O3The addition of the particles leads the tensile strength of the material to be obviously improved under the condition of not losing more plasticity, and to a certain extent, the intermittent ball milling is adopted, the raw material ratio and the ball milling rotating speed are limited, the heat preservation and pressure maintaining time in the sintering process is prolonged, and the density and the plasticity of the material are favorably improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is an SEM image of the matrix grain distribution of example 1.
FIG. 2 shows Y in example 12O3SEM images of dispersion distribution in the matrix.
FIG. 3 shows Y in example 12O3STEM images of the distribution of particles in the matrix grain boundaries and within the grains.
FIG. 4 is an SEM image of the matrix grain distribution of example 2.
FIG. 5 shows Y in example 22O3SEM images of dispersion distribution in the matrix.
FIG. 6 shows Y in example 22O3STEM images of the distribution of particles in the matrix grain boundaries and within the grains.
FIG. 7 is an SEM image of the matrix grain distribution of example 3.
FIG. 8 is a stress-strain curve under room temperature conditions for examples 1-4 and comparative example 1.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The technical solution of the present invention is further illustrated by the following examples.
Example 1
Weighing 99.48 wt% of 316L pre-alloyed powder with the particle size of 75 microns, putting the powder into a ball milling tank, and adding 0.275 wt% of pure Y powder with the average particle size of 50 microns and 0.245 wt% of Fe with the average particle size of 100nm into the ball milling tank2O3And (3) adding 304 stainless steel balls as grinding media into the ball milling tank, wherein the ball-to-material ratio is 6: 1, wherein the weight ratio of stainless steel balls with the diameters of 6mm and 10mm is 4: 1. then, the ball milling tank filled with the steel balls and the powder is filled with argon gas in a glove box and is packaged, so that the ball milling process is carried out in the argon gas environment. The ball milling adopts a QM-3SP4 type planetary high-energy ball mill produced by Nanjing large instrument factories. The ball milling speed is 300 r/min, and the ball milling time is 36 h. In addition, in consideration of the bearing capacity of the ball milling tank and the steel balls, severe heating in the high-energy ball milling process is prevented, the ball milling mode is intermittent operation, each ball milling time is 1.5 hours, the ball milling is stopped for 0.5 hour, and then the ball milling is continuously operated. The ball-milled powder is put into a graphite die with the diameter of 20mm, and a piece of graphite paper is respectively added between the upper punch and the lower punch and between the upper punch and the die. Then, vacuumizing the furnace chamber and pressurizing the die, wherein the pressure is 50 MPa; heating to 1050 ℃ at a heating rate of 100 ℃/min, keeping the temperature and the pressure for 5 minutes, and cooling along with the furnace to obtain the oxide dispersion strengthened austenitic steel.
The oxide dispersion strengthened austenitic steel prepared in this example was sampled and examined. Wherein FIG. 1 is a SEM image of the grain distribution, and the average grain size is 1.36 μm; FIG. 2 is Y2O3The particles are uniformly sized and densely distributed in the SEM image of the dispersion distribution in the matrix, and FIG. 3 is Y2O3STEM image of the distribution of particles in the matrix grain boundary and the grain boundary, and the dense Y is dispersed and distributed in the grain boundary and the grain boundary2O3And (3) granules.
Example 2
Weighing 99.48 wt% of 316L pre-alloyed powder with the particle size of 75 microns, putting the powder into a ball milling tank, and adding 0.275 wt% of pure Y powder with the average particle size of 50 microns and 0.245 wt% of pure Y powder with the particle size of 100nm into the ball milling tankFe2O3Pulverizing; then putting 304 stainless steel balls as grinding media into the ball milling tank, wherein the ball-material ratio is 6: 1, wherein the weight ratio of stainless steel balls with the diameters of 6mm and 10mm is 4: 1. then, the ball milling tank filled with the steel balls and the powder is filled with argon gas in a glove box and is packaged, so that the ball milling process is carried out in the argon gas environment. The ball milling adopts a QM-3SP4 type planetary high-energy ball mill produced by Nanjing large instrument factories. The ball milling speed is 300 r/m, and the ball milling time is 36 hours; the ball milling mode is intermittent operation, each ball milling time is 1.5 hours, the ball milling is stopped for 0.5 hour, and then the operation is continued. The ball-milled powder is put into a graphite die with the diameter of 20mm, and a piece of graphite paper is respectively added between the upper punch and the lower punch and between the upper punch and the die. Then, vacuumizing the furnace chamber and pressurizing the die, wherein the pressure is 50 MPa; heating to 1050 ℃ at a heating rate of 100 ℃/min, keeping the temperature and the pressure for 10 minutes, and cooling along with the furnace to obtain the oxide dispersion strengthened austenitic steel.
The oxide dispersion strengthened austenitic steel prepared in this example was sampled and examined. Wherein FIG. 4 is a SEM photograph showing the distribution of crystal grains, the average grain size is 1.41 μm, and there is a slight increase in the size of comparative example 1, which is caused by the increase in the holding time; FIG. 5 is Y2O3The SEM images of the dispersion distribution in the matrix show that the particles in the SEM images of the dispersion distribution are uniform in size and relatively dense in distribution; FIG. 6 is Y2O3STEM image of the distribution of particles in the matrix grain boundary and grain boundary, and the relatively dense Y distributed in the grain boundary and grain boundary2O3Particles;
example 3
Weighing 99.48 wt% of 316L pre-alloyed powder with the particle size of 75 microns, putting the powder into a ball milling tank, and adding 0.275 wt% of pure Y powder with the average particle size of 50 microns and 0.245 wt% of Fe with the average particle size of 100nm into the ball milling tank2O3And (3) adding 304 stainless steel balls as grinding media into the ball milling tank, wherein the ball-to-material ratio is 6: 1, wherein the weight ratio of stainless steel balls with the diameters of 6mm and 10mm is 4: 1. then, the ball milling tank filled with the steel balls and the powder is filled with argon gas in a glove box and is packaged, so that the ball milling process is carried out in the argon gas environment. Ball milling is carried out byA QM-3SP4 planetary high-energy ball mill produced by Nanjing large instrument factory. The ball milling speed is 200 r/min, and the ball milling time is 30 hours. In addition, in consideration of the bearing capacity of the ball milling tank and the steel balls, severe heating in the high-energy ball milling process is prevented, the ball milling mode is intermittent operation, each ball milling time is 1 hour, the ball milling is stopped for 0.5 hour, and then the ball milling tank and the steel balls continue to operate. The ball-milled powder is put into a graphite die with the diameter of 20mm, and a piece of graphite paper is respectively added between the upper punch and the lower punch and between the upper punch and the die. And then, vacuumizing the furnace chamber and pressurizing the die, wherein the pressure is 50MPa, the temperature is raised to 1050 ℃ at the heating rate of 100 ℃/min, the temperature and the pressure are kept for 10 minutes, and the oxide dispersion strengthened austenitic steel is obtained after furnace cooling.
The oxide dispersion strengthened austenitic steel prepared in this example was sampled and examined. Wherein FIG. 7 is a SEM image of the crystal grain distribution, the average crystal grain size is 1.58 μm, and the comparative example 2 shows a large increase in size due to the fact that the rotation speed is low and the intermittence is frequent during the ball milling process, so that Y is large2O3The generated thermodynamics is insufficient, the final generated amount is less, and the pinning effect on the grain growth in the sintering process is weak; further as shown in FIG. 7, Y2O3Very sparse distribution in the matrix.
Example 4
Weighing 99.48 wt% of 316L pre-alloyed powder with the particle size of 75 microns, putting the powder into a ball milling tank, and adding 0.400 wt% of pure Y powder with the average particle size of 50 microns and 0.350 wt% of Fe with the average particle size of 100nm into the ball milling tank2O3And (3) adding 304 stainless steel balls as grinding media into the ball milling tank, wherein the ball-to-material ratio is 6: 1, wherein the weight ratio of stainless steel balls with the diameters of 6mm and 10mm is 4: 1. then, the ball milling tank filled with the steel balls and the powder is filled with argon gas in a glove box and is packaged, so that the ball milling process is carried out in the argon gas environment. The ball milling adopts a QM-3SP4 type planetary high-energy ball mill produced by Nanjing large instrument factories. The ball milling speed is 300 r/min, and the ball milling time is 36 h. In addition, the ball milling mode is intermittent operation, each ball is in intermittent operation in consideration of the bearing capacity of the ball milling tank and the steel balls and prevents serious heating in the high-energy ball milling processMilling for 1.5 hours, stopping for 0.5 hour, and then continuing the operation. The ball-milled powder is put into a graphite die with the diameter of 20mm, and a piece of graphite paper is respectively added between the upper punch and the lower punch and between the upper punch and the die. And then, vacuumizing the furnace chamber and pressurizing the die, wherein the pressure is 50MPa, the temperature is raised to 1050 ℃ at the heating rate of 100 ℃/min, the temperature and the pressure are kept for 10 minutes, and the oxide dispersion strengthened austenitic steel is obtained after furnace cooling.
The oxide dispersion strengthened austenitic steel prepared in this example was sampled and examined. Average grain size 1.48 μm due to the addition of Y and F2O3Higher content of Y leads to2O3More are. And excessive Y2O3The particles are easy to agglomerate and coarsen in the sintering process to form larger particles, and the large particles are easy to fall off when dislocation and grain boundary pinning is performed, so that the strengthening effect is reduced.
Comparative example 1
The comparative example is identical to example 2, except that no Y or Fe is added2O3And (3) powder.
FIG. 8 is a graph showing stress-strain curves of the tensile experiments conducted in examples 1 to 4 and comparative example 1, and it can be seen from FIG. 8 that the tensile strength of examples 1 to 4 is significantly higher than that of comparative example 1 because Y formed by the reaction during the process of being subjected to the tensile2O3Plays a role in pinning and blocking dislocation slip and grain boundary migration.
Comparative example 2
The process of this comparative example is the same as example 2 except that there is no holding process.
Under the condition, because of no heat preservation and pressure maintaining process, gas in gaps among the powder cannot be fully removed, the connection part between the powder is very weak, the density of the block obtained by sintering is extremely low, and the tensile strength cannot be tested.
Comparative example 3
The comparative example was conducted in the same manner as in example 2 except that the ball milling speed was selected to be 600 rpm.
Under the condition, because the rotating speed is too high, the austenite powder which is relatively soft originally is seriously attached to the inner wall of the ball milling tank and the grinding balls, so that the powder yield is extremely low, and subsequent sintering and test representation cannot be carried out.
Comparative example 4
The comparative example was conducted in the same manner as in example 2 except that the ball milling speed was selected to be 100 rpm.
Under the condition, the ball milling rotating speed is too low, so that the ball milling strength in the tank body is seriously insufficient, and Y cannot be successfully generated2O3Meanwhile, uniform mixing of the powder cannot be effectively realized.
Comparative example 5
The process of this comparative example is the same as example 3 except that the ball to feed ratio is 1: 15. Under the condition, because the ball-material ratio is too high, the collision frequency between grinding balls in the tank and between the grinding balls and the tank wall is greatly increased, the ball-milling strength is obviously increased, so that relatively soft austenite powder is seriously attached to the inner wall and the grinding balls of the ball-milling tank, the powder yield is extremely low, and subsequent sintering and test characterization cannot be carried out.
Comparative example 6
The process of this comparative example is the same as example 3 except that the ball milling time is 100 hours. Under this condition, the ball milling for an excessively long time severely increases the abrasion of the milling balls and the milling pot, resulting in an increase of impurities in the powder.
The composite materials obtained in examples 1 to 4 were subjected to sample treatment to obtain tensile samples meeting the test requirements. The tensile properties were measured on a stretching machine (model CMT5105, manufactured by Meitess Industrial systems, Inc., China) under the conditions of normal temperature and a stretching rate of 0.48 mm/min. In addition to the test, the polished specimens were subjected to corrosion treatment, microstructure observation and analysis. Tissue characterization was performed using SEM (manufactured by Hitachi, Japan, model No. S4800) and TEM (manufactured by JEOL, Japan, model No. JEM-2100 f).
TABLE 1 comparison of Properties
| At room temperature | Yield strength/MPa | Tensile strength/MPa | Elongation/percent |
| Example 1 | 441 | 860 | 17.0 |
| Example 2 | 457 | 865 | 20.5 |
| Example 3 | 416 | 836 | 21.0 |
| Example 4 | 452 | 834 | 22.0 |
| Comparative example 1 | 424 | 722 | 21.5 |
| Comparative example 2 | — | — | — |
| Comparative example 3 | — | — | — |
| Comparative example 4 | 413 | 692 | 18.5 |
| Comparative example 5 | - | - | - |
| Comparative example 6 | 437 | 824 | 16.0 |
From Table 1, it is found that by comparing with comparative examples 1 to 6, it is possible to obtain nano-sized Y obtained by reaction ball milling in the present invention2O3The tensile strength of the material is obviously improved under the condition of not losing much plasticity due to the addition of the particles, so that the density and the plasticity of the material are improved by adopting intermittent ball milling, limiting the raw material ratio, the ball milling rotating speed and time and properly prolonging the heat preservation and pressure maintaining time in the sintering process; fig. 8 is a stress-strain curve under room temperature conditions for examples 1-4 and comparative example 1, and it can be seen that the maximum tensile strength and yield strength of examples 1-4 are significantly higher than those of comparative example 1.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (4)
1. A method for preparing dispersion oxide strengthened section steel based on a powder metallurgy process is characterized in that 316L powder is used as a matrix, and Y powder and Fe powder are used2O3Powder as a reinforcing agent;
the method comprises the following steps:
(1) adding Y powder and Fe into 316L powder2O3Powdering, to Y2O3The mass fraction in the system is 0.20-0.50%, and the powder is uniformly mixed;
(2) placing the mixed powder obtained in the step (1) in a ball milling tank, and carrying out ball milling in an inert gas atmosphere after oxygen discharge;
(3) putting the ball-milled powder into a mould, putting the mould into a discharge plasma sintering furnace, pressurizing and vacuumizing the mould, performing discharge plasma sintering, and preserving heat and pressure after sintering;
in the step (2), argon or helium is used for oxygen discharge, the ball milling speed is 200-; the ball milling mode is intermittent ball milling, the ball milling is carried out for 1 to 2 hours, and the intermittent ball milling is carried out for 0.2 to 0.7 hour;
the temperature rise rate of the spark plasma sintering in the step (3) is 50-200 ℃/min, the sintering temperature is 1000-1200 ℃, and the heat preservation and pressure maintaining time is 5-20 min.
2. The method for preparing the dispersion oxide strengthened steel based on the powder metallurgy process according to claim 1, wherein the 316L powder has a particle size range of 50-100 μm, the Y powder has a particle size range of 50-100 μm, and Fe2O3The particle size of the powder is in the range of 20-200 nm.
3. The method for preparing the dispersion oxide strengthened steel based on the powder metallurgy process according to claim 1, wherein the ball-to-material ratio in the ball milling process in the step (2) is 5-10: 1.
4. the method for manufacturing a dispersion oxide strengthened steel according to claim 1, wherein the pressurizing pressure in the step (3) is 30 to 60 MPa.
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| CN107385306A (en) * | 2016-05-16 | 2017-11-24 | 中国科学院上海硅酸盐研究所 | A kind of stainless base steel composite materials of SiC particles reinforced 316L and preparation method thereof |
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| CN1639369A (en) * | 2002-08-08 | 2005-07-13 | 日本核燃料循环开发机构 | Dispersed oxide reinforced martensitic steel excellent in high temperature strength and method for production thereof |
| CN107385306A (en) * | 2016-05-16 | 2017-11-24 | 中国科学院上海硅酸盐研究所 | A kind of stainless base steel composite materials of SiC particles reinforced 316L and preparation method thereof |
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