CN115058631B - Manufacturing method suitable for coaxial powder feeding composite friction stir treatment of oxide dispersion strengthening steel - Google Patents
Manufacturing method suitable for coaxial powder feeding composite friction stir treatment of oxide dispersion strengthening steel Download PDFInfo
- Publication number
- CN115058631B CN115058631B CN202210837892.5A CN202210837892A CN115058631B CN 115058631 B CN115058631 B CN 115058631B CN 202210837892 A CN202210837892 A CN 202210837892A CN 115058631 B CN115058631 B CN 115058631B
- Authority
- CN
- China
- Prior art keywords
- powder
- friction stir
- yttrium oxide
- layer
- steel
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/12—Metallic powder containing non-metallic particles
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- 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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/25—Direct deposition of metal particles, e.g. direct metal deposition [DMD] or laser engineered net shaping [LENS]
-
- 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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/50—Treatment of workpieces or articles during build-up, e.g. treatments applied to fused layers during build-up
-
- 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
- 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
-
- 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
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- 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
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
-
- 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
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
-
- 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
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention provides a manufacturing method suitable for coaxial powder feeding composite friction stir processing of oxide dispersion strengthening steel, which comprises the steps of depositing a first layer on a substrate layer by layer in an upward growth mode according to a preset program until a last Nth layer is deposited, so as to obtain a required oxide dispersion strengthening steel member; in the process of depositing the first layer to the N layer, the yttrium oxide and the steel powder are remelted through stirring friction to obtain a current deposited layer, so that the aggregation and growth of yttrium oxide particles in the current deposited layer are inhibited, the loss of yttrium oxide is prevented, the yttrium oxide particles are dispersed in the alloy steel matrix, and meanwhile, grains of the alloy steel matrix structure are thinned to a first grain size interval. The invention suppresses the aggregation and growth of yttrium oxide particles by a coaxial powder feeding and compound friction stir processing mode, and the yttrium oxide particles are dispersed in an alloy steel matrix, so that the loss of yttrium oxide is prevented, the utilization rate of yttrium oxide materials is improved, and the performance of ODS steel is improved.
Description
Technical Field
The invention relates to the technical field related to additive manufacturing, in particular to a manufacturing method suitable for coaxial powder feeding composite friction stir processing of oxide dispersion strengthening steel.
Background
Oxide dispersion strengthening Steel (Oxide Dispersion Strengthened Steel, ODS Steel) is widely regarded as an important candidate structural material (mainly 9-18Cr ferrite/austenitic Steel) of key parts of advanced nuclear energy systems such as a fuel cladding material of a fourth generation nuclear reactor in the future, a high-temperature structural member material, a first wall of a fusion reactor cladding in the future and the like due to excellent irradiation swelling resistance, helium embrittlement resistance, good high-temperature strength and creep property, has a severe service environment, needs to bear high-energy neutron irradiation, high surface heat flow, high nuclear heat deposition, liquid metal corrosion, high pressure, complex mechanical load and the like, and has extremely high requirements on structural materials, molding quality and molding accuracy of products.
The conventional preparation process of ODS steel mainly comprises the following steps: the pure metal powder (or prealloy powder) and nano oxide (such as Y-Ti-O, Y-Si-O, Y-Al-O, Y-Zr-O or Y-Hf-O) powder are mixed, ball milled and mechanically alloyed, and then thermally solidified and formed by Hot Isostatic Pressing (HIP), hot rolling or high-temperature sintering and the like, and the ODS steel is small in preparation scale and difficult to realize industrial scale production due to the limitation of mechanical alloying efficiency and the capability of thermal curing forming equipment. In addition, because the specific gravity of the nano oxide in the ODS steel is smaller than that of the matrix alloy, the conventional fusion welding processing can lead oxide particles to float upwards towards the surface of the weld joint along with the melting of weld metal, so that oxide dispersion strengthening particles in a tissue are separated and aggregated, the dispersion distribution state of the nano oxide in the steel is damaged, the high-temperature creep property and the irradiation resistance of the welded joint are reduced, and finally the material property is deteriorated. Thus, the component forming of ODS steel also becomes a bottleneck limiting its component fabrication and mass-scale application in the nuclear energy field.
In recent years, a 3D printing technology which is rapidly developed provides a new way for molding ODS steel, and Chinese patent publication No. CN110565002A discloses a selective laser melting additive manufacturing method suitable for oxide reinforced steel, which comprises the steps of firstly uniformly mixing yttrium-containing nano-oxide with 9-18Cr ferrite/austenitic steel powder and then filling the mixture into a powder feeding box; secondly, a three-dimensional solid model is built in a computer, layering and slicing are carried out, and the powder paving thickness and sedimentation compensation of each powder layer are set; and sequentially forming the powder layers by adopting laser beams according to the layering slice shape, and finally performing heat treatment to obtain the composite material.
Chinese patent publication No. CN111590079A discloses a nano oxide dispersion strengthening steel piece and an additive manufacturing method thereof, wherein alloy powder is firstly ball-milled and made into a flux-cored wire, and then the oxide dispersion steel piece is printed by adopting an arc fuse additive manufacturing technology, so that a die and rapid cooling are not needed, and the efficiency of the preparation process is improved.
ODS steel prepared by the two 3D printing technologies has the characteristics of forming a small micro-molten pool and rapid cooling and solidification, so that aggregation and growth of nano oxides are inhibited to a certain extent, and a large number of nano oxide particles are dispersed and distributed in a steel matrix. However, the above processes all need to use a high temperature heat source, the printing process has higher temperature, the higher temperature can cause burning loss of nano yttrium oxide, and the nano yttrium oxide cannot be melted into a steel matrix, so that the loss of nano yttrium oxide is caused, and the yttrium oxide cannot be uniformly dispersed in the steel matrix; meanwhile, due to the higher temperature, the yttrium oxide can be decomposed and recombined to grow up to form large-particle yttrium oxide, so that the nano morphology is lost, and the performance of the ODS steel is affected.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a manufacturing method of coaxial powder feeding composite friction stir processing suitable for oxide dispersion strengthening steel, which inhibits the aggregation and growth of yttrium oxide particles, disperses the yttrium oxide particles in an alloy steel matrix, prevents the loss of yttrium oxide, improves the utilization rate of materials and improves the performance of ODS steel by adopting a coaxial powder feeding composite friction stir processing mode.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the manufacturing method of the coaxial powder feeding composite friction stir processing suitable for the oxide dispersion strengthening steel comprises the following steps:
s1, mixing nanoscale yttrium oxide particles with alloy steel powder in proportion to obtain mixed powder;
s2, adopting a coaxial powder feeding friction stir additive manufacturing process, and depositing layer by layer on the substrate in an upward growth mode from a first layer according to a preset program until the deposition of the last layer is completed, so as to obtain an oxide dispersion reinforced steel member;
in the process of depositing the first layer to the N layer, remelting yttrium oxide particles and alloy steel powder through stirring friction on each layer to obtain a deposited layer, inhibiting the aggregation and growth of yttrium oxide particles in the deposited layer, preventing the loss of yttrium oxide, dispersing the yttrium oxide particles in a steel member matrix, and refining grains of a steel member matrix structure to a first grain size interval.
Preferably, the first grain size range is 10-20 μm.
Preferably, in the mixed powder, the average particle size of the nano yttrium oxide is 10-90nm.
Preferably, in the mixed powder, the alloy steel powder is stainless steel powder or alloy steel powder with other specific purposes, and the average grain diameter of the alloy steel powder is 30-60 mu m.
Preferably, in the mixed powder, the total mass of the alloy powder and the nano yttrium oxide raw material is 100%, wherein the nano yttrium oxide powder accounts for 0.1% -10% of the mixed powder by mass.
Preferably, the coaxial powder feeding friction stir additive manufacturing process is configured to determine the powder feeding speed and the process parameters of friction stir processing according to the alloy component parameters, and set a printing program according to the process parameters to perform printing and forming of the component.
Preferably, the conditions of the coaxial powder feeding friction stir additive manufacturing process are as follows: the advancing speed of friction stir processing is 40mm/min-300mm/min, the rotating speed of friction stir processing is 500-1800rpm, the pressing amount of each pass of friction stir processing is 0.1-0.5mm, the pressing force is 8000-45000N, and the powder feeding speed is 2-12g/min.
Preferably, a ball milling process is adopted to obtain the nano yttrium oxide, wherein the ball milling process conditions are as follows: under the argon condition with the volume purity more than or equal to 99.99 percent, the ball material mass ratio (5-20) is 1 and ball milling is carried out for 20-50 hours at the rotating speed of 300-500 r/min.
According to the technical scheme, the manufacturing method is suitable for the coaxial powder feeding composite friction stir processing of the oxide dispersion strengthening steel, the powder feeding is carried out in a stirring head in a coaxial powder feeding mode, friction stir additive manufacturing is carried out while the powder is fed, the yttrium oxide and the steel powder are remelted through friction stir, a deposited layer is obtained, the current deposited layer is obtained, the aggregation and growth of yttrium oxide particles in the current deposited layer are inhibited, the loss of yttrium oxide is prevented, the yttrium oxide particles are dispersed in an alloy steel matrix, grains of an alloy steel matrix structure are thinned, and the performance of ODS steel is improved.
Drawings
Fig. 1 is a process flow diagram of a method of manufacturing a coaxial powder feed composite friction stir processing suitable for oxide dispersion strengthened steel of the present invention.
FIG. 2 is a schematic diagram of an exemplary coaxial powder feed friction stir apparatus of the present invention.
FIG. 3 is a cross-sectional view of an exemplary coaxial powder feed friction stir apparatus of the present invention.
Fig. 4 is a schematic drawing of the process of the manufacturing method of the coaxial powder feeding composite friction stir processing applicable to oxide dispersion strengthened steel of the present invention.
FIG. 5 is a schematic view showing the structure of ODS steel obtained by the method of the invention.
FIG. 6 is a schematic view showing the structure of ODS steel obtained by laser melt deposition.
Detailed Description
For a better understanding of the technical content of the present invention, specific examples are set forth below, along with the accompanying drawings.
Aspects of the invention are described in this disclosure with reference to the drawings, in which are shown a number of illustrative embodiments. The embodiments of the present disclosure are not necessarily intended to include all aspects of the invention. It should be appreciated that the various concepts and embodiments described above, as well as those described in more detail below, may be implemented in any of a wide variety of ways.
In oxide dispersion strengthening steel, yttrium oxide can play a role only in a nano form, but in the prior art, the prepared ODS steel still has the problems of yttrium oxide particle aggregation and growth, and the problems that yttrium oxide particles cannot be melted into a steel matrix, volatilize and lose in the preparation process, so that the material utilization rate is low, and the performance of the formed ODS steel is affected.
As shown in FIG. 1, the invention provides a manufacturing method suitable for the coaxial powder feeding composite friction stir processing of oxide dispersion strengthening steel, which inhibits the aggregation length of yttrium oxide particles in the friction stir material increase manufacturing process and disperses the yttrium oxide particles in an alloy steel matrix by adopting the material increase manufacturing process of the coaxial powder feeding composite friction stir, prevents the loss of yttrium oxide, improves the utilization rate of yttrium oxide materials and improves the performance of ODS steel.
The invention adopts a coaxial powder feeding mode, wherein the coaxial powder feeding means that a powder feeding channel is arranged in a stirring head, in the printing process, mixed powder mixed by a powder mixer is fed into the powder feeding channel by the powder feeder, and stirring and material adding are started while powder feeding, so that the printing process of stirring while powder feeding is completed.
In an exemplary embodiment of the present invention, referring to fig. 2 to 4, there is provided a coaxial powder feeding friction stir apparatus including a rotation shaft 1, a clamping portion 2, a shaft shoulder 3, and a stirring pin 4, wherein the clamping portion 2, the shaft shoulder 3, and the stirring pin 4 are defined as a stirring head.
The rotary shaft 1 is connected with the clamping part 2, the rotary shaft 1 is connected with the driving device, and the stirring head is driven to rotate at a high speed through the driving device, so that the friction stir material increase manufacturing process is carried out.
The center shaft of the rotating shaft 1 is provided with a first channel 11 for conveying powder, the powder feeding device 5 is connected with the first channel 11, and the powder feeding device, the rotating shaft and the stirring head are kept relatively static through a bearing, so that the stability of powder feeding is ensured.
The stirring head is internally provided with a second channel 6 connected with the first channel 11, the second channel is arranged at the central shaft position of the clamping part 2, the shaft shoulder 3 and the stirring needle 4, and powder is conveyed to the inlet of the first channel through the powder conveying device 5 and sequentially passes through the rotating shaft 1, the clamping part 2, the shaft shoulder 3 and the stirring needle 4 and is conveyed to a region to be added.
In an exemplary embodiment of the present invention, on the basis of the above coaxial powder feeding friction stir apparatus, in combination with fig. 3, there is provided a manufacturing method of a coaxial powder feeding composite friction stir processing suitable for oxide dispersion strengthened steel, comprising the steps of:
s1, mixing the nano yttrium oxide particles with alloy steel powder in proportion to obtain mixed powder.
S2, adopting a coaxial powder feeding friction stir additive manufacturing process, depositing layer by layer on the substrate in an upward growth mode from the first layer according to a preset program until the last Nth layer is deposited, and completing the whole friction stir additive manufacturing printing process to obtain the oxide dispersion strengthening steel member.
The specific treatment process comprises the following steps: in the process of depositing the first layer to the N layer, the yttrium oxide particles and the alloy steel powder are remelted through stirring friction in each layer to obtain each deposited layer, so that the aggregation and growth of the yttrium oxide particles in the current deposited layer are inhibited, the loss of yttrium oxide is prevented, the yttrium oxide particles are dispersed in the steel member matrix, and meanwhile, the grains of the steel member matrix structure are thinned to a first grain size interval.
In a preferred embodiment, the first grain size interval is 10-20 μm.
In a preferred embodiment, the average particle size of the nano yttrium oxide in the mixed powder is 10-90nm.
In a preferred embodiment, the alloy steel powder is stainless steel powder or other alloy steel powder with specific application, and the average grain size of the alloy steel powder is 30-60 mu m.
In a preferred embodiment, in the mixed powder, the total mass of the alloy powder and the nano yttrium oxide raw material is 100%, wherein the nano yttrium oxide powder accounts for 0.1% -10% of the mixed powder by mass.
In a preferred embodiment, the coaxial powder feed friction stir additive manufacturing process is configured to determine the powder feed rate and process parameters of the friction stir process based on alloy component parameters, and to set a printing program based thereon to perform a print forming of the component.
In a preferred embodiment, the conditions of the coaxial powder feed friction stir additive manufacturing process are: the advancing speed of friction stir processing is 40mm/min-300mm/min, the rotating speed of friction stir processing is 500-1800rpm, the pressing amount of each pass of friction stir processing is 0.1-0.5mm, the pressing force is 8000-45000N, and the powder feeding speed is 2-12g/min.
In a preferred embodiment, a ball milling process is used to obtain nano yttrium oxide, wherein the ball milling process conditions are as follows: under the argon condition with the volume purity more than or equal to 99.99 percent, the ball material mass ratio (5-20) is 1 and the ball milling time is 20-50h at the rotating speed of 300-500 r/min.
For a better understanding, the present invention will be further described with reference to several specific examples, but the processing technique is not limited thereto, and the present invention is not limited thereto.
The following examples and comparative examples print ODS steel workpieces having dimensions 45mm by 20mm in length and width.
Wherein the grain diameter of the used micron-sized alloy powder (316L or 304L) is 5-60 mu m, the grain diameter of the nanometer yttrium oxide powder is 15-70nm, and the specific components of the alloy steel powder are shown in the table 1 and the table 2.
Table 1 (316L alloy steel composition)
| C | Mn | Si | Ni | Cr | Mo | S | P |
| ≤0.03 | ≤2.0 | ≤1.0 | 12-16 | 16-18 | 1.8-2.5 | ≤0.030 | ≤0.035 |
Table 2 (304L alloy steel composition)
| C | Mn | Si | Ni | Cr | S | P |
| ≤0.03 | ≤2.0 | ≤1.0 | 9.0-12.0 | 18.0-20.0 | ≤0.03 | ≤0.045 |
[ example 1 ]
Step one: selecting 316L stainless steel powder with average particle diameter of 45 μm and nanometer yttrium oxide powder with average particle diameter of 50nm as raw materials, oven drying, mixing with a mixer, and ball milling for 25 hr, wherein Y 2 O 3 The proportion incorporated is 1%; and simultaneously, placing the substrate subjected to the advanced sand blasting into a vacuum glove box for coordinate positioning.
Step two: and (3) loading the powder mixed in the step one into a powder feeding barrel of a powder feeder, feeding the powder in a coaxial powder feeding mode, and setting the parameter powder feeding speed to be 5g/min.
Step three: the established STL three-dimensional model is led into a printing computer, a numerical control system is adopted for stirring and material adding, parameters are set according to the technological parameter requirements, the advancing speed of the stirring friction processing is 40mm/min, the rotating speed is 350rpm, and the pressing amount is 0.1mm.
Step four: stirring and material adding are carried out according to the set parameter path, the material is deposited layer by layer in an upward growth mode from the first layer until the last layer is deposited, and the formed steel member is obtained.
Step five: and (3) after printing is completed, opening the cabin door when the part to be formed is completely cooled (2 hours), and taking out the prepared oxide dispersion strengthening steel.
[ example 2 ]
Step one: 304L stainless steel powder with average grain diameter of 45 mu m and nano yttrium oxide powder with average grain diameter of 50nm are selected as raw materials, are subjected to drying proportion configuration, are put into a powder mixer for full mixing, and ball milling time is 25 hours, wherein Y is 2 O 3 The proportion incorporated is 1%; and simultaneously, placing the substrate subjected to the advanced sand blasting into a vacuum glove box for coordinate positioning.
Step two: and (3) loading the powder mixed in the step one into a powder feeding barrel of a powder feeder, feeding the powder in a coaxial powder feeding mode, and setting the parameter powder feeding speed to be 5g/min.
Step three: the established STL three-dimensional model is led into a printing computer, a numerical control system is adopted for stirring and material adding, parameters are set according to the technological parameter requirements, the advancing speed of the stirring friction processing is 100mm/min, the rotating speed is 800rpm, and the pressing amount is 0.5mm.
Step four: stirring and material adding are carried out according to the set parameter path, the material is deposited layer by layer in an upward growth mode from the first layer until the last layer is deposited, and the molded component is obtained.
Step five: and (3) after printing is completed, opening the cabin door when the part to be formed is completely cooled (2 hours), and taking out the prepared oxide dispersion strengthening steel.
[ example 3 ]
Step one: 316L stainless steel powder with average grain diameter of 45 μm and nanometer yttrium oxide powder with average grain diameter of 45nm are selected as raw materials, and are arranged according to a drying proportion, and are put into a powder mixer for fully mixingBall milling time 25h, wherein Y 2 O 3 The proportion incorporated is 1%; and simultaneously, placing the substrate subjected to the advanced sand blasting into a vacuum glove box for coordinate positioning.
Step two: and (3) loading the powder mixed in the step one into a powder feeding barrel of a powder feeder, feeding the powder in a coaxial powder feeding mode, and setting the parameter powder feeding speed to be 5g/min.
Step three: introducing the established STL format three-dimensional model into a printing computer, stirring and adding materials by adopting a numerical control system, setting parameters according to technological parameter requirements, wherein the advancing speed of stirring friction processing is 300mm/min, and the rotating speed is 1200rpm; the amount of depression was 0.8mm.
Step four: stirring and material adding are carried out according to the set parameter path, the material is deposited layer by layer in an upward growth mode from the first layer until the last layer is deposited, and the molded component is obtained.
Step five: and (3) after printing is completed, opening the cabin door when the part to be formed is completely cooled (2 hours), and taking out the prepared oxide dispersion strengthening steel.
[ example 4 ]
Step one: 316L stainless steel powder with average grain diameter of 40 mu m and nanometer yttrium oxide powder with average grain diameter of 50nm are selected as raw materials, are subjected to drying proportion configuration, are put into a powder mixer for full mixing, and ball milling time is 25 hours, wherein Y is 2 O 3 The proportion incorporated is 1%; and simultaneously, placing the substrate subjected to the advanced sand blasting into a vacuum glove box for coordinate positioning.
Step two: and (3) loading the powder mixed in the step one into a powder feeding barrel of a powder feeder, feeding the powder in a coaxial powder feeding mode, and setting the parameter powder feeding speed to be 7g/min.
Step three: introducing the established STL format three-dimensional model into a printing computer, stirring and adding materials by adopting a numerical control system, setting parameters according to technological parameter requirements, wherein the advancing speed of stirring friction processing is 600mm/min, and the rotating speed is 1800rpm; the amount of depression was 1.2mm.
Step four: stirring and material adding are carried out according to the set parameter path, the material is deposited layer by layer in an upward growth mode from the first layer until the last layer is deposited, and the molded component is obtained.
Step five: and (3) after printing is completed, opening the cabin door when the part to be formed is completely cooled (2 hours), and taking out the prepared oxide dispersion strengthening steel.
[ example 5 ]
Step one: 304L stainless steel powder with average grain diameter of 40 mu m and nanometer yttrium oxide powder with average grain diameter of 50nm are selected as raw materials, and are subjected to drying proportion configuration, and are placed into a powder mixer for full mixing, wherein Y is 2 O 3 The proportion incorporated is 1%; and simultaneously, placing the substrate subjected to the advanced sand blasting into a vacuum glove box for coordinate positioning.
Step two: and (3) loading the powder mixed in the step one into a powder feeding barrel of a powder feeder, feeding the powder in a coaxial powder feeding mode, and setting the parameter powder feeding speed to be 5g/min.
Step three: introducing the established STL format three-dimensional model into a printing computer, stirring and adding materials by adopting a numerical control system, setting parameters according to technological parameter requirements, wherein the advancing speed of stirring friction processing is 40mm/min, and the rotating speed is 500rpm; the amount of depression was 0.2mm.
Step four: stirring and material adding are carried out according to the set parameter path, the material is deposited layer by layer in an upward growth mode from the first layer until the last layer is deposited, and the molded component is obtained.
Step five: and (3) after printing is completed, opening the cabin door when the part to be formed is completely cooled (2 hours), and taking out the prepared oxide dispersion strengthening steel.
Comparative example 1
Step one: selecting 316L stainless steel powder with average particle diameter of 45 μm and nanometer yttrium oxide powder with average particle diameter of 50nm as raw materials, oven drying, mixing with a mixer, and ball milling for 25 hr, wherein Y 2 O 3 The proportion incorporated was 1%.
Step two: creating a three-dimensional entity model for the part to be molded by using drawing software in a computer, inputting a three-dimensional entity graph of the part to be molded into molding control software of a BLT-C600 selective laser melting equipment control computer, and according to the size of the part: a vertical molding mode is selected 45×45mm×20mm, and the layering thickness is set to be 0.5mm according to the material characteristics, and the powder laying thickness is increased by 10 μm for every 10 layers deposited.
Step three: vacuumizing the forming chamber until the vacuum degree reaches 10 -3 Filling high-purity Ar with purity of 99.99 into the Pa level backward forming chamber 2 And (5) vacuum is carried out.
Step four: argon is protected in the forming chamber, the argon pressure is 20mbar, and the temperature in the forming chamber is ensured to be 300+/-50 ℃ in the whole forming process; spreading a layer of raw material mixed powder with the thickness of 0.5mm on a powder spreading plane through a powder feeding box, scanning and preheating the profile of the formed section of the layered slice by adopting small-power large-beam spot laser, and detecting by adopting infrared temperature to ensure that the powder preheating temperature reaches 200 ℃.
Laser scanning preheating process: laser power 120W, laser diameter 150 μm, scanning speed 1000mm/s, scanning mode: jumping and turning, scanning the lap joint rate to be 30%, and scanning the interval to be 80 mu m; and secondly, adopting high-power laser to carry out selective fusion forming according to the forming section profile information of the layered slice.
The melting scanning forming process comprises the following steps: laser power 400W, laser diameter 80 μm, scanning speed 500mm/s, scanning mode: the jump direction is changed, the scan overlap ratio is 30%, and the scan interval is 80 μm.
And finally, repairing spheroidization and microcracks among melting channels by adopting lower-power laser, reducing spheroidization defects and further improving molding compactness.
The laser repairing process comprises the following steps: the laser power is 300W, the laser diameter is 80 mu m, the scanning speed is 500mm/s, the scanning mode and the melting scanning path are mutually staggered, the mutual staggered interval is 30 mu m, the scanning interval is 80 mu m, and the lap joint rate is 20%.
Step five: after the first layer of powder is deposited and molded, a second layer of powder is paved through a powder paving box, the powder thickness is uniform and is the same as the first layer, the in-layer melting and deposition adopts the same molding process as the last layer, and the in-layer is deposited and molded in an orthogonal scanning mode in the direction of 90 DEG perpendicular to the layer to be molded and the deposited layer, so that the powder is piled layer by layer until the molding of the whole part is completed.
Step six: after the component is molded, the component is taken out from the molding chamber and subjected to vacuum heat treatment, so that nano oxides are ensured to be evenly precipitated, the residual stress in the component molding process is reduced, and the overall performance of the component is improved.
The heat treatment process comprises the following steps: in a vacuum annealing furnace, heating to 1050 ℃ along with the furnace at a heating rate of 20 ℃/min, preserving heat for 120min, cooling to below 50 ℃ along with the furnace at a cooling rate of 5 ℃/min, and discharging to obtain the prepared ODS steel piece.
The mechanical properties of the molded parts of comparative examples 1 to 5 and comparative example 1 were measured, and the results are shown in Table 3.
TABLE 3 Table 3
| Room temperature | Yield strength/MPa | Tensile strength/MPa | Elongation% |
| Example 1 | 773 | 976 | 14.6 |
| Example 2 | 842 | 963 | 16.2 |
| Example 3 | 883 | 986 | 17.0 |
| Example 4 | 848 | 895 | 15.3 |
| Example 5 | 804 | 903 | 16.5 |
| Comparative example 1 | 710 | 820 | 12.5 |
As can be seen from Table 3, the ODS steels prepared by friction stir (examples 1-5) have significantly higher yield strength and tensile strength than those prepared by laser melt deposition relative to those prepared by laser melt deposition (comparative example 1).
This is because, as shown in fig. 5, the precipitated phase yttria (combined with the a part of fig. 5) is more dispersed and distributed, and under the characteristic that the same amount of nano yttria and yttria itself are easy to aggregate and grow, the friction stir can greatly reduce the aggregation and growth of yttria so that the yttria is more dispersed, and the dispersed nano oxide has pinning grain boundary and dislocation movement resistance, so that the ODS steel has stable grain size and dislocation structure, thereby the oxide dispersion steel prepared with excellent high-temperature strength and irradiation swelling resistance performance has better performance, and the more dispersed nano precipitated phase is distributed, the more dislocation movement and dislocation pinning quantity are, and the greater the strength required by the oxide dispersion steel member during deformation is; meanwhile, the friction stir processing temperature is lower, so that the loss and loss of yttrium oxide are effectively prevented, grains of an alloy steel matrix structure (such as part b in fig. 5) are thinned, and the mechanical property of the material is further improved.
As shown in FIG. 6, the ODS steel prepared by laser fused deposition adopts a high-temperature heat source, the printing process has higher temperature, the higher temperature can cause burning loss of nano yttrium oxide, the nano yttrium oxide cannot be fused into a steel matrix, so that the loss of nano yttrium oxide is caused, the yttrium oxide cannot be uniformly dispersed in the steel matrix, meanwhile, the yttrium oxide can be decomposed and combined and grown again due to the higher temperature, so that large-particle yttrium oxide is formed, the nano morphology is lost (shown as a part a in FIG. 6), and the performance of the ODS steel is affected; and the grain size of the matrix structure (shown in part b of fig. 6) of the alloy steel is relatively coarse, which also affects the properties of the ODS steel to some extent.
While the invention has been described with reference to preferred embodiments, it is not intended to be limiting. Those skilled in the art will appreciate that various modifications and adaptations can be made without departing from the spirit and scope of the present invention. Accordingly, the scope of the invention is defined by the appended claims.
Claims (8)
1. The manufacturing method of the coaxial powder feeding composite friction stir processing suitable for the oxide dispersion strengthening steel is characterized by comprising the following steps of:
s1, mixing nanoscale yttrium oxide particles with alloy steel powder in proportion to obtain mixed powder;
s2, adopting a coaxial powder feeding friction stir additive manufacturing process, and depositing layer by layer on the substrate in an upward growth mode from a first layer according to a preset program until the deposition of the last layer is completed, so as to obtain an oxide dispersion reinforced steel member;
in the process of depositing the first layer to the N layer, remelting yttrium oxide particles and alloy steel powder through stirring friction on each layer to obtain a deposited layer, inhibiting the aggregation and growth of yttrium oxide particles in the deposited layer, preventing the loss of yttrium oxide, dispersing the yttrium oxide particles in a steel member matrix, and refining grains of a steel member matrix structure to a first grain size interval.
2. The method for producing a coaxial powder feed composite friction stir processing according to claim 1, wherein the first grain size range is 10 to 20 μm.
3. The method for producing a coaxial powder feed composite friction stir processing according to claim 1, wherein the average particle diameter of the yttrium oxide particles in the mixed powder is 10 to 90nm.
4. The method for producing the coaxial powder feeding composite friction stir processing of oxide dispersion strengthened steel according to claim 1, wherein the alloy steel powder in the mixed powder is stainless steel powder or alloy steel powder for other specific purposes, and the average grain size of the alloy steel powder is 30-60 μm.
5. The method for manufacturing the coaxial powder feeding composite friction stir processing of the oxide dispersion strengthened steel according to any one of claims 1 to 4, wherein yttrium oxide particles and alloy steel powder in the mixed powder are calculated according to mass percent, and the nano yttrium oxide powder accounts for 0.1 to 10 mass percent of the mixed powder.
6. The method of claim 1, wherein the coaxial powder feed friction stir additive manufacturing process is configured to determine the powder feed speed and the process parameters of the friction stir process according to the alloy member parameters, and to set a printing program according to the determined parameters to perform the printing forming of the member.
7. The method for manufacturing the coaxial powder feeding and friction stir processing for oxide dispersion strengthened steel according to claim 1, wherein the conditions of the coaxial powder feeding and friction stir additive manufacturing process are as follows: the advancing speed of friction stir processing is 40mm/min-300mm/min, the rotating speed of friction stir processing is 500-1800rpm, the pressing amount of each pass of friction stir processing is 0.1-0.5mm, the pressing force is 8000-45000N, and the powder feeding speed is 2-12g/min.
8. The manufacturing method for the coaxial powder feeding composite friction stir processing of the oxide dispersion strengthened steel according to claim 1, wherein the nanometer yttrium oxide is obtained by adopting a ball milling process, and the process conditions of the ball milling are as follows: under the argon condition with the volume purity more than or equal to 99.99 percent, the ball material mass ratio (5-20) is 1 and ball milling is carried out for 20-50 hours at the rotating speed of 300-500 r/min.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2022106653472 | 2022-06-13 | ||
| CN202210665347 | 2022-06-13 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115058631A CN115058631A (en) | 2022-09-16 |
| CN115058631B true CN115058631B (en) | 2023-09-01 |
Family
ID=83206877
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210837892.5A Active CN115058631B (en) | 2022-06-13 | 2022-07-17 | Manufacturing method suitable for coaxial powder feeding composite friction stir treatment of oxide dispersion strengthening steel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115058631B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07278726A (en) * | 1994-04-08 | 1995-10-24 | Mitsubishi Heavy Ind Ltd | Production of oxide dispersion strengthened ferrite steel |
| JP2005076087A (en) * | 2003-09-01 | 2005-03-24 | Japan Nuclear Cycle Development Inst States Of Projects | METHOD OF MANUFACTURING OXIDE DISPERSION-STRENGTHENED MARTENSITIC STEEL HAVING RESIDUAL alpha-GRAIN AND EXCELLENT HIGH-TEMPERATURE STRENGTH |
| CN101328562A (en) * | 2008-07-17 | 2008-12-24 | 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 |
| CN104404509A (en) * | 2014-11-28 | 2015-03-11 | 中南大学 | Metal laser melting additive manufacturing method |
| CN108356263A (en) * | 2018-04-28 | 2018-08-03 | 苏州大学 | Heat-resisting steel alloy powder of laser gain material manufacture novel martensitic and preparation method thereof |
| CN110565002A (en) * | 2019-10-17 | 2019-12-13 | 中国科学院合肥物质科学研究院 | selective laser melting additive manufacturing method suitable for oxide reinforced steel |
| CN111590079A (en) * | 2020-05-08 | 2020-08-28 | 华中科技大学 | Nano oxide dispersion strengthened steel part and rapid additive manufacturing method thereof |
| WO2022041258A1 (en) * | 2020-08-30 | 2022-03-03 | 中南大学 | Nano ceramic metal composite powder for 3d printing, and application |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20220111437A1 (en) * | 2020-10-14 | 2022-04-14 | Central South University | Method for preparing nano spherical oxide dispersion strengthening phase |
-
2022
- 2022-07-17 CN CN202210837892.5A patent/CN115058631B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07278726A (en) * | 1994-04-08 | 1995-10-24 | Mitsubishi Heavy Ind Ltd | Production of oxide dispersion strengthened ferrite steel |
| JP2005076087A (en) * | 2003-09-01 | 2005-03-24 | Japan Nuclear Cycle Development Inst States Of Projects | METHOD OF MANUFACTURING OXIDE DISPERSION-STRENGTHENED MARTENSITIC STEEL HAVING RESIDUAL alpha-GRAIN AND EXCELLENT HIGH-TEMPERATURE STRENGTH |
| CN101328562A (en) * | 2008-07-17 | 2008-12-24 | 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 |
| CN104404509A (en) * | 2014-11-28 | 2015-03-11 | 中南大学 | Metal laser melting additive manufacturing method |
| CN108356263A (en) * | 2018-04-28 | 2018-08-03 | 苏州大学 | Heat-resisting steel alloy powder of laser gain material manufacture novel martensitic and preparation method thereof |
| CN110565002A (en) * | 2019-10-17 | 2019-12-13 | 中国科学院合肥物质科学研究院 | selective laser melting additive manufacturing method suitable for oxide reinforced steel |
| CN111590079A (en) * | 2020-05-08 | 2020-08-28 | 华中科技大学 | Nano oxide dispersion strengthened steel part and rapid additive manufacturing method thereof |
| WO2022041258A1 (en) * | 2020-08-30 | 2022-03-03 | 中南大学 | Nano ceramic metal composite powder for 3d printing, and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115058631A (en) | 2022-09-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108941560B (en) | A method of it eliminating Rene104 nickel base superalloy laser gain material and manufactures crackle | |
| CN112935252B (en) | Method for preparing high-toughness eutectic high-entropy alloy based on selective laser melting technology | |
| CN109439962B (en) | Method for selective laser melting forming of nickel-based superalloy | |
| CN111590079B (en) | Nano oxide dispersion strengthened steel part and rapid additive manufacturing method thereof | |
| CN112795828B (en) | Tantalum-tungsten alloy for 3D printing and method for preparing tantalum-tungsten alloy thin-walled plate | |
| CN109332695B (en) | Selective laser melting preparation method of molybdenum-based alloy with enhanced oxidation resistance | |
| CN110565002B (en) | Selective laser melting additive manufacturing method suitable for oxide reinforced steel | |
| CN112267056A (en) | High-entropy alloy component and manufacturing method thereof | |
| CN113186444B (en) | Nano oxide and carbide dispersion strengthening low activation steel and preparation method and application thereof | |
| CN109332717B (en) | Preparation method of spherical molybdenum titanium zirconium alloy powder | |
| CN115058631B (en) | Manufacturing method suitable for coaxial powder feeding composite friction stir treatment of oxide dispersion strengthening steel | |
| KR20120072235A (en) | Fe-based oxide dispersion strengthened alloy, and manufacturing method thereof | |
| CN114855030B (en) | Ni-Cr-W-based superalloy suitable for selective laser melting forming and preparation method thereof | |
| CN115109981B (en) | Oxide dispersion strengthening TaNbVTi refractory high-entropy alloy and preparation method and application thereof | |
| CN116117164A (en) | Method for regulating and controlling tissues in selective melting process of TiAl alloy electron beam | |
| CN115029587B (en) | Oxide dispersion strengthening nickel-based superalloy manufactured by additive and preparation method thereof | |
| CN114480901B (en) | Method for manufacturing nickel-based superalloy performance through carbide reinforced additive, nickel-based superalloy powder and application of nickel-based superalloy powder | |
| CN108044122B (en) | Preparation method of Nb-Si-based alloy hollow turbine blade | |
| CN116275010A (en) | In-situ nitride reinforced 3D printing nickel-based superalloy powder | |
| CN115106540A (en) | Tantalum-tungsten alloy product and preparation method thereof | |
| KR102008721B1 (en) | Manufacturing method of Cr-Al binary alloy powder having excellent oxidation and corrosion resistance, the Cr-Al binary alloy powder, manufacturing method of Cr-Al binary alloy PVD target having excellent oxidation and corrosion resistance and the Cr-Al binary alloy PVD target | |
| CN113463086A (en) | Method for preparing wear-resistant coating on titanium alloy surface by laser melt injection | |
| CN116657019B (en) | NiTiAlVCMo powder-based laser additive alloy, composite coating and preparation method of composite coating | |
| CN115319114B (en) | Method for preparing SnBi-xFe low-melting-point composite material by using selective laser melting process | |
| CN114921714B (en) | Y 2 O 3 Nano-particle dispersion strengthened steel and preparation method thereof |
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 |