CN114523125B - Method for preparing alloy block by SLM in-situ alloying - Google Patents
Method for preparing alloy block by SLM in-situ alloying Download PDFInfo
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- CN114523125B CN114523125B CN202210211543.2A CN202210211543A CN114523125B CN 114523125 B CN114523125 B CN 114523125B CN 202210211543 A CN202210211543 A CN 202210211543A CN 114523125 B CN114523125 B CN 114523125B
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- 238000000034 method Methods 0.000 title claims abstract description 75
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 41
- 239000000956 alloy Substances 0.000 title claims abstract description 41
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 27
- 238000005275 alloying Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 95
- 238000002844 melting Methods 0.000 claims abstract description 34
- 230000008018 melting Effects 0.000 claims abstract description 34
- 238000007639 printing Methods 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 238000010146 3D printing Methods 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000011812 mixed powder Substances 0.000 claims abstract description 13
- 239000004615 ingredient Substances 0.000 claims abstract description 8
- 239000010410 layer Substances 0.000 claims description 30
- 239000002356 single layer Substances 0.000 claims description 19
- 239000000758 substrate Substances 0.000 claims description 19
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000003892 spreading Methods 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 229910000531 Co alloy Inorganic materials 0.000 claims description 3
- 230000007547 defect Effects 0.000 abstract description 9
- 238000005204 segregation Methods 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 abstract description 4
- 239000010964 304L stainless steel Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 229910001256 stainless steel alloy Inorganic materials 0.000 description 11
- 239000010963 304 stainless steel Substances 0.000 description 5
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 5
- 229910001119 inconels 625 Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 238000000889 atomisation Methods 0.000 description 4
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- 238000010586 diagram Methods 0.000 description 3
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- 239000011229 interlayer Substances 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 229910000601 superalloy Inorganic materials 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000004519 manufacturing process Methods 0.000 description 1
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- 239000007769 metal material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
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- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
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Classifications
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- 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
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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- 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
- B22F10/30—Process control
- B22F10/36—Process control of energy beam parameters
- B22F10/364—Process control of energy beam parameters for post-heating, e.g. remelting
-
- 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
- B22F10/30—Process control
- B22F10/36—Process control of energy beam parameters
- B22F10/366—Scanning parameters, e.g. hatch distance or scanning strategy
-
- 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
- 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
- B22F10/80—Data acquisition or data processing
- B22F10/85—Data acquisition or data processing for controlling or regulating additive manufacturing processes
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- 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
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- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
-
- 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
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0433—Nickel- or cobalt-based alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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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
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
-
- 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
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
-
- 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
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- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Automation & Control Theory (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to a method for preparing an alloy block by SLM in-situ alloying, which comprises the following steps: mixing ingredients and raw materials: adopting more than two kinds of powder as raw materials, drying and deoxidizing each powder, and uniformly mixing to obtain mixed powder; setting forming process parameters, and determining the process parameters of 3D printing by utilizing finite element software COMSOL according to the set forming process parameters; and printing the mixed powder by adopting a 3D printer under the protection of Ar gas. According to the invention, more than two kinds of powder are used as raw materials to replace prealloy powder with single component for SLM printing, a laser selective melting and multistage laser post heat treatment mode is adopted, and the finite element software COMSOL is used to calculate the optimal technological parameters, so that the time and cost of trial-and-error test can be greatly reduced, the sample density of the alloy rapid is higher than 99.9%, and the components are uniform and have no tissue segregation, no obvious holes and other common printing defects.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a method for preparing an alloy block by SLM in-situ alloying.
Background
Selective laser melting (Selective laser melting, SLM) is one of the mainstream processes for metal additive manufacturing, using materials that are typically prealloyed powders, i.e. the raw powder materials are first alloyed by melting prior to their preparation. The powder used by the SLM is mainly prepared by a vacuum gas atomization process, but the prepared powder usually meets the use requirement of the SLM in less than half, different materials need corresponding powder preparation processes to be matched, the development of novel SLM materials is restricted by complicated procedures and high cost, and the types of the commercial material brands are very limited at present.
The element powder in-situ alloying technology, namely a method that raw materials adopt mixed simple substance powder or specific alloy powder to directly complete alloying in the laser selective melting process and synchronously form high-density sample pieces, is an efficient and low-cost material research and development method, can break through the limitation of the powder process of customized powder, has extremely high flexibility in changing alloy components compared with alloy powder SLM, and can be used in the fields of new material development and multi-material printing.
However, due to the fact that physical parameters of all components in the mixed powder are different, the in-situ alloying sample prepared by adopting a traditional SLM laser scanning strategy and process has a large number of defects, not only is the uniformity of components poor, but also a large number of unmelted particles, holes and other tissue defects are formed, so that the mechanical property, corrosion resistance and other using properties of the sample are greatly reduced, and the application of the technology is severely restricted. In addition, due to the fact that the SLM process parameters are numerous, the regulation and control range of each parameter is wide, the process of optimizing the process needs to be searched through multiple rounds of trial and error experiments, and the method is time-consuming, labor-consuming and high in cost.
The present invention has been made in view of the above-mentioned circumstances.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for preparing an alloy block by SLM in-situ alloying, which uses more than two kinds of powder as raw materials to replace prealloy powder with single component for SLM printing, adopts a laser selective melting and multistage laser post heat treatment mode, calculates preferable technological parameters by utilizing finite element software COMSOL, can greatly reduce the time and cost of trial-and-error test, and has the advantages that the sample density of an alloy block obtained by the method is higher than 99.9%, and the components are uniform and have no tissue segregation, no obvious holes and other common printing defects.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method of preparing an alloy block by SLM in situ alloying, the method comprising the steps of:
(1) Mixing ingredients and raw materials: adopting more than two kinds of powder as raw materials, drying and deoxidizing each powder, and uniformly mixing to obtain mixed powder;
(2) Setting forming process parameters, and determining the process parameters of 3D printing by utilizing finite element software COMSOL according to the set forming process parameters;
(3) And under the protection of Ar gas, printing the mixed powder by a 3D printer, and separating a sample from a substrate by wire cutting after printing, thereby obtaining the SLM in-situ alloying preparation alloy block.
Further, the powder in step (1) comprises pure elemental metal powder and/or prealloyed powder.
Further, the pure metal simple substance powder comprises at least one of Fe, cr, ni, co, mn, mo, and the prealloy powder comprises at least one of iron-based alloy, nickel-based alloy, cobalt-based alloy and high-entropy alloy.
Further, the minimum mixing ratio of each powder in the step (1) is 1%, the powder is spherical, the particle size distribution is 15-53 mu m, the oxygen content is less than 500ppm, the Hall flow rate is less than 20s/50g, and the purity of the pure metal simple substance powder is preferably more than 99.5%.
Further, in the step (1), the drying temperature is 100-200 ℃, the drying is carried out for 2-3 hours under the vacuum degree of less than 10KPa absolute pressure, and the mixing is carried out for 3-24 hours at the rotating speed of 25-100 r/min.
Further, in the step (2), the 3D printing process adopts laser selective melting and multistage laser post heat treatment for each layer of powder.
Further, the laser selective melting parameters are specifically set as follows: the thickness of the powder spreading layer is 20-50 mu m, the laser power is 100-250W, the scanning speed is 600-1500mm/s, the scanning line distance is 50-200 mu m, the light spot diameter is 50-100 mu m, the single-layer scanning path is folded scanning, and the scanning path between layers is vertical scanning.
Further, the parameters of the multistage laser post-heat treatment are specifically set as follows: the laser power is 100-300W, the scanning speed is 500-1200mm/s, the scanning line distance is 50-120 mu m, the spot diameter is 50-100 mu m, the single-layer scanning path is foldback scanning, and the scanning path between layers is vertical scanning.
Further, the multistage laser post-heat treatment adopts 2-6 stages, and the laser power of each stage is increased by 0-80W compared with the previous stage in the scanning process.
Further, the following parameters are set first: the single-layer liquid state melting time length is more than or equal to 0.1s, the molten pool depth is more than 1.5 times of the layer thickness, the molten pool width is more than or equal to 0.5 times of the molten pool depth, the set laser selective melting parameters and the set multistage laser post heat treatment parameters are taken as constraint conditions, and the set laser selective melting parameters and the set multistage laser post heat treatment parameters are input into finite element software COMSOL to determine the technological parameters of 3D printing.
Further, in the step (3), the oxygen content in the 3D printing is controlled to be less than 1000 ppm.
In the invention, finite element software COMSOL is utilized to determine the technological parameters of 3D printing according to the set molding technological parameters, firstly, an SLM multi-channel scanning temperature field model is established, and the main steps of modeling comprise the following steps:
(1) Defining parameters: the method comprises a laser selective melting parameter and a multistage laser post heat treatment parameter;
(2) Defining variables: the heat source adopts a Gaussian heat source, and the path comprises 5 passes;
(3) And (3) establishing a model: comprises a base plate and a powder bed model;
(4) Loading material from a library of software materials: adding material properties to the substrate and the powder bed;
(5) Setting boundary conditions: adding environmental radiation and Gaussian heat source condition boundary conditions to the top surface of the powder bed;
(6) Dividing grids: the mesh size of the powder bed is extremely refined, and the substrate is of a conventional size;
(7) Study settings: setting transient research time;
(8) And (5) calculating.
Inputting the set laser selective melting parameters and the set multistage laser post-heat treatment parameters into a finite element model, and calculating proper 3D printing process parameters by taking the single-layer liquid state melting time length as a constraint condition, wherein the melting bath depth is greater than or equal to 0.1s, and the melting bath width is greater than or equal to 0.5 times of the melting bath depth.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, more than two kinds of powder are used as raw materials to replace single-component prealloyed powder for SLM printing, a laser selective melting and multistage laser post-heat treatment mode is adopted, the multistage laser post-heat treatment can obviously improve the liquid residence time of a molten pool in the printing process, so that various elements are fully mutually diffused to form a homogenized solid solution, and the defects of tissue segregation, interface phase, unmelted particles and the like generated by the mixed powder SLM can be effectively solved; in addition, the splash particles, unmelted particles, spheroidized particles and unfused holes on the surface of the molten pool can be eliminated by the multistage laser post-heat treatment in a remelting mode, so that the surface roughness of the sample is improved, the number of hole defects in the sample is reduced, and the compactness of the sample is improved. The preferred process parameters are calculated by utilizing finite element software COMSOL, so that the time and cost of trial-and-error test can be greatly reduced, the density of a sample of the alloy rapid body obtained by the method is higher than 99.9%, and the alloy rapid body has uniform components and no common printing defects such as tissue segregation, obvious holes and the like, and has good forming performance;
(2) The alloy block prepared by the method can break through the limitation of the powder preparation process of customized powder, has extremely high flexibility in the aspect of the component design of 3D printing metal materials, has strong universality, is suitable for simple substance powder such as Fe, cr, ni, co, mn, mo and prealloy powder materials such as iron-based alloy, nickel-based alloy, cobalt-based alloy, high-entropy alloy and the like, and is different from the method of the prior art that the micro-area in-situ metallurgy is directly generated in the 3D printing process, wherein the method is used for carrying out metallurgy and powder preparation before 3D printing.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a single layer scan path diagram in a 3D printing process according to the present invention;
FIG. 2 is a diagram of an inter-layer scan path in a 3D printing process according to the present invention;
FIG. 3 is a finished view of a 304L stainless steel alloy block prepared in example 1 of the present invention;
FIG. 4 is a graph showing the density and defect analysis results of a 304L stainless steel alloy block prepared in example 1 of the present invention;
FIG. 5 is an EDS spectroscopy scan of a 304L stainless steel alloy block prepared in example 1 of the present invention;
FIG. 6 is an XRD pattern of a 304L stainless steel alloy block prepared in example 1 of the present invention;
FIG. 7 is a graph comparing the mechanical properties of a 304L stainless steel alloy block prepared in example 1 of the present invention with a prior art prealloyed powder 304L stainless steel alloy block.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, based on the examples herein, which are within the scope of the invention as defined by the claims, will be within the scope of the invention as defined by the claims.
The 3D printing single-layer scanning path is shown in fig. 1, and the interlayer scanning path is shown in fig. 2.
Example 1
The embodiment provides a method for preparing a 304L stainless steel alloy block with high density and high uniformity by SLM in-situ alloying, which comprises the following steps:
(1) Mixing ingredients and raw materials: weighing three elementary powders of spherical iron powder, chromium powder and nickel powder prepared by a vacuum atomization method according to the following mass fractions, wherein the particle size distribution of each elementary powder is 15-53 mu m, the oxygen content is less than 500ppm, the Hall flow rate is less than 20s/50g, the purity of the pure metal elementary powder is more than 99.5%, the respective powders are dried respectively, the drying temperature is 100 ℃, the vacuum degree is less than the absolute pressure of 10KPa, the drying powders are dried for 2 hours, and the dried powders are placed in a mixer to be fully and uniformly mixed, wherein the mixing is carried out for 10 hours at the rotating speed of 50 r/min;
(2) Setting forming process parameters, adopting a 3D printing process, wherein each layer of powder is subjected to selective laser melting and multistage laser post heat treatment by the 3D printing process, an SLM multi-pass scanning temperature field model is established by utilizing finite element software COMSOL, and the calculated preferred process parameters are as follows:
the specific setting of the laser selective melting parameters is as follows: the thickness of the powder spreading layer is 30 mu m, the laser power is 150W, the scanning speed is 800mm/s, the scanning line distance is 100 mu m, the light spot diameter is 60 mu m, the single-layer scanning path is foldback scanning, and the scanning path between layers is vertical scanning;
the parameters of the multistage laser post-heat treatment are specifically set as follows: the multistage laser post heat treatment adopts 3 stages, and the parameters of the 1 st stage are as follows: the laser power is 200W, the scanning speed is 800mm/s, the scanning line distance is 100 mu m, the light spot diameter is 50 mu m, the single-layer scanning path is foldback scanning, the scanning path between layers is vertical scanning, the laser power of the 2 nd and the 3 rd stages is respectively increased by 40W and 80W on the 1 st stage, and the rest parameters are the same;
(3) And (3) placing the dried and deoxidized mixed powder in a metal 3D printer for printing, constructing a plurality of blocks (10 mm multiplied by 8 mm) with preset sizes, adopting Ar gas for protection in the printing process, enabling the oxygen content to be within 1000ppm, adopting 304 stainless steel as a printing substrate, enabling the size of the substrate to be 300cm multiplied by 2cm, separating a sample from the substrate by adopting linear cutting after printing, and obtaining the 304L stainless steel alloy block with high compactness and high uniformity prepared by SLM in-situ alloying.
The picture of the finished product of the 304L stainless steel alloy block prepared in the embodiment is shown in fig. 3, the density and defect analysis result is shown in fig. 4, the components are uniform, no segregation and no unmelted particles are found through fig. 4, the density is 99.96%, the EDS energy spectrum scanning diagram is shown in fig. 5, the component fluctuation of a sample (10 points are taken at a minimum of 500 μm between every two points) detected through EDS point scanning is only 0.7% at maximum, the XRD analysis result is shown in fig. 6, the microstructure is a single-phase austenite structure, and the microstructure is the same as the room temperature structure of the sample prepared through the laser selective melting of prealloyed powder 304L.
The mechanical properties of the 304L stainless steel alloy block prepared by the method of the embodiment and the pre-alloyed powder 304L stainless steel alloy block in the prior art are shown in FIG. 7. As can be seen in FIG. 7, the in situ alloyed 304L sample had a tensile strength of 620MPa, a yield strength of 378MPa, an elongation of 64.5% and a microhardness of 182HV. The tensile strength of the 304L laser selective melting sample of the prealloyed powder is 623Mpa, the yield strength is 375Mpa, the elongation is 63% and the microhardness is 184HV. In terms of mechanical properties, the 304L stainless steel sample prepared by SLM in-situ alloying is at a level equivalent to the sample prepared by selective laser melting of prealloyed powder 304L.
Example 2
The embodiment provides a method for preparing an Inconel625 nickel-based superalloy block with high density and high uniformity by SLM in-situ alloying, which comprises the following steps:
(1) Mixing ingredients and raw materials: weighing five simple substance powders of Ni 62.5%, cr 22.0%, mo 9.0%, nb 3.5% and Fe 3.0% prepared by adopting a vacuum atomization method according to the following mass fractions, wherein the particle size distribution of each simple substance powder is 15-53 mu m, the oxygen content is less than 500ppm, the Hall flow rate is less than 20s/50g, the purity of the pure metal simple substance powder is more than 99.5%, the powder is respectively dried, the drying temperature is 150 ℃, the vacuum degree is less than 10KPa absolute pressure and is dried for 2.5 hours, and the dried powder is placed in a mixer to be fully and uniformly mixed, wherein the mixture is mixed for 24 hours at the rotating speed of 25 r/min;
(2) Setting forming process parameters, adopting a 3D printing process, wherein each layer of powder is subjected to selective laser melting and multistage laser post heat treatment by the 3D printing process, an SLM multi-pass scanning temperature field model is established by utilizing finite element software COMSOL, and the calculated preferred process parameters are as follows:
the specific setting of the laser selective melting parameters is as follows: the thickness of the powder spreading layer is 20 mu m, the laser power is 100W, the scanning speed is 600mm/s, the scanning line distance is 50 mu m, the light spot diameter is 75 mu m, the single-layer scanning path is foldback scanning, and the scanning path between layers is vertical scanning;
the parameters of the multistage laser post-heat treatment are specifically set as follows: the multistage laser post heat treatment adopts 5 stages, and the parameters of the 1 st stage are as follows: the laser power is 100W, the scanning speed is 500mm/s, the scanning line distance is 50 mu m, the light spot diameter is 75 mu m, the single-layer scanning path is foldback scanning, the scanning path between layers is vertical scanning, the laser power of the 2 nd, 3 rd, 4 th and 5 th stages is increased by 10W step by step on the 1 st stage basis, and the rest parameters are the same;
(3) And (3) placing the dried and deoxidized mixed powder in a metal 3D printer for printing, constructing a plurality of blocks (10 mm multiplied by 8 mm) with preset sizes, adopting Ar gas for protection in the printing process, enabling the oxygen content to be within 1000ppm, adopting 304 stainless steel as a printing substrate, enabling the size of the substrate to be 300cm multiplied by 2cm, separating a sample from the substrate by adopting wire cutting after printing, and obtaining the SLM in-situ alloying preparation high-density high-uniformity Inconel625 nickel-based superalloy block.
The alloy block prepared in this example was tested to have a density of 99.94% and the sample was subjected to EDS point scanning detection (10 points in total, with a minimum 500 μm separation between each two points) for a maximum of only 1.1% composition fluctuation.
Example 3
The embodiment provides a method for preparing a CoCrFeNi high-entropy alloy block with high density and high uniformity by SLM in-situ alloying, which comprises the following steps:
(1) Mixing ingredients and raw materials: weighing four simple substance powders of Fe 24.76%, co 26.13%, cr 23.07% and Ni 26.04%, wherein the particle size distribution of each simple substance powder is 15-53 mu m, the oxygen content is less than 500ppm, the Hall flow rate is less than 20s/50g, the purity of the pure metal simple substance powder is more than 99.5%, drying the powder respectively at 200 ℃ and the vacuum degree is less than 10KPa absolute pressure for 3h, placing the dried powder into a mixer, fully and uniformly mixing, wherein the powder is mixed for 3h at the rotating speed of 100 r/min;
(2) Setting forming process parameters, adopting a 3D printing process, wherein each layer of powder is subjected to selective laser melting and multistage laser post heat treatment by the 3D printing process, an SLM multi-pass scanning temperature field model is established by utilizing finite element software COMSOL, and the calculated preferred process parameters are as follows:
the specific setting of the laser selective melting parameters is as follows: the thickness of the powder spreading layer is 50 mu m, the laser power is 250W, the scanning speed is 1500mm/s, the scanning line distance is 200 mu m, the light spot diameter is 50 mu m, the single-layer scanning path is foldback scanning, and the scanning path between layers is vertical scanning;
the parameters of the multistage laser post-heat treatment are specifically set as follows: the multistage laser post heat treatment adopts 4 stages, and the parameters of the 1 st stage are as follows: the laser power is 100W, the scanning speed is 1200mm/s, the scanning line distance is 120 mu m, the light spot diameter is 100 mu m, the single-layer scanning path is foldback scanning, the scanning path between layers is vertical scanning, the laser energy values of the 2 nd, 3 rd and 4 th stages are increased by 12W step by step on the basis of the 1 st stage parameters, and the rest parameters are the same;
(3) Printing the dried and deoxidized mixed powder in a metal 3D printer to construct a plurality of blocks (10 mm multiplied by 8 mm) with preset sizes, wherein Ar gas is adopted for protection in the printing process, the oxygen content is within 1000ppm, a printing substrate is made of 304 stainless steel, the size of the substrate is 300cm multiplied by 2cm, a sample is separated from the substrate by wire cutting after printing is finished, and the SLM in-situ alloying is adopted to prepare the CoCrFeNi high-entropy alloy block with high density and high uniformity.
The alloy block prepared in this example was tested to have a density of 99.97% and the sample was subjected to EDS point scanning detection (10 points in total, with a minimum 500 μm separation between each two points) for a maximum of only 0.9% composition fluctuation.
Example 4
The embodiment provides a method for preparing a 304L-Inconel625 alloy block with high density and high uniformity by SLM in-situ alloying, which comprises the following steps:
(1) Mixing ingredients and raw materials: weighing spherical 304L and Inconel625 alloy powder prepared by a vacuum atomization method according to the following mass fractions, wherein the particle size distribution of the powder is 15-53 mu m, the oxygen content is less than 500ppm, the Hall flow rate is less than 20s/50g, drying the powder respectively at 200 ℃ and the vacuum degree is less than absolute pressure 10KPa for 3h, placing the dried powder into a mixer, fully and uniformly mixing, and mixing for 3h at the rotating speed of 100 r/min;
(2) Setting forming process parameters, adopting a 3D printing process, wherein each layer of powder is subjected to selective laser melting and multistage laser post heat treatment by the 3D printing process, an SLM multi-pass scanning temperature field model is established by utilizing finite element software COMSOL, and the calculated preferred process parameters are as follows:
the specific setting of the laser selective melting parameters is as follows: the thickness of the powder spreading layer is 30 mu m, the laser power is 200W, the scanning speed is 1200mm/s, the scanning line distance is 150 mu m, the light spot diameter is 60 mu m, the single-layer scanning path is foldback scanning, and the scanning path between layers is vertical scanning;
the parameters of the multistage laser post-heat treatment are specifically set as follows: the multistage laser post heat treatment adopts 3 stages, and the parameters of the 1 st stage are as follows: the laser power is 120W, the scanning speed is 1200mm/s, the scanning line distance is 80 mu m, the light spot diameter is 80 mu m, the single-layer scanning path is foldback scanning, the scanning path between layers is vertical scanning, the laser energy values of the 2 nd and the 3 rd stages are increased by 10W step by step on the basis of the 1 st stage parameters, and the rest parameters are the same;
(3) And (3) placing the dried and deoxidized mixed powder in a metal 3D printer for printing to construct a plurality of blocks (10 mm multiplied by 8 mm) with preset sizes, wherein Ar gas is adopted for protection in the printing process, the oxygen content is within 1000ppm, a printing substrate is made of 304 stainless steel, the size of the substrate is 300cm multiplied by 2cm, and a sample is separated from the substrate by wire cutting after printing is finished, so that the 304L-Inconel625 alloy block with high density and high uniformity is prepared by in-situ alloying of the SLM.
The alloy block prepared in the embodiment has the compactness of 99.98% through testing, and the component fluctuation of the sample through EDS point scanning detection (10 points are taken at least 500 μm apart between every two points) is only 0.7% at maximum.
Example 5
The embodiment provides a method for preparing a CoCrFeNiMo high-entropy alloy block with high density and high uniformity by SLM in-situ alloying, which comprises the following steps:
(1) Mixing ingredients and raw materials: weighing two kinds of powder of spherical equal atomic ratio CoCrFeNi high entropy alloy powder and Mo simple substance powder prepared by adopting a vacuum atomization method according to the following mass fraction, wherein the CoCrFeNi is 72.00%, the Mo is 28.00%, the particle size distribution of each powder is 15-53 mu m, the oxygen content is less than 500ppm, the Hall flow rate is less than 20s/50g, the purity of the pure metal simple substance powder is more than 99.5%, each powder is dried respectively, the drying temperature is 200 ℃, the vacuum degree is less than absolute pressure of 10KPa, the drying is carried out for 3 hours, and each dried powder is placed into a mixer to be fully and uniformly mixed, wherein the mixture is mixed for 3 hours at the rotating speed of 100 r/min;
(2) Setting forming process parameters, adopting a 3D printing process, wherein each layer of powder is subjected to selective laser melting and multistage laser post heat treatment by the 3D printing process, an SLM multi-pass scanning temperature field model is established by utilizing finite element software COMSOL, and the calculated preferred process parameters are as follows:
the specific setting of the laser selective melting parameters is as follows: the thickness of the powder spreading layer is 30 mu m, the laser power is 250W, the scanning speed is 1200mm/s, the scanning line distance is 150 mu m, the light spot diameter is 60 mu m, the single-layer scanning path is foldback scanning, and the scanning path between layers is vertical scanning;
the parameters of the multistage laser post-heat treatment are specifically set as follows: the multistage laser post heat treatment adopts 4 stages, and the parameters of the 1 st stage are as follows: the laser power is 120W, the scanning speed is 1200mm/s, the scanning line distance is 80 mu m, the light spot diameter is 80 mu m, the single-layer scanning path is foldback scanning, the scanning path between layers is vertical scanning, the laser energy values of the 2 nd, 3 rd and 4 th stages are increased by 8W step by step on the basis of the 1 st stage parameters, and the rest parameters are the same;
(3) Printing the dried and deoxidized mixed powder in a metal 3D printer to construct a plurality of blocks (10 mm multiplied by 8 mm) with preset sizes, wherein Ar gas is adopted for protection in the printing process, the oxygen content is within 1000ppm, a printing substrate is made of 304 stainless steel, the size of the substrate is 300cm multiplied by 2cm, a sample is separated from the substrate by adopting wire cutting after printing is finished, and the SLM in-situ alloying is adopted to prepare the CoCrFeNiMo high-entropy alloy block with high density and high uniformity.
The alloy block prepared in this example was tested to have a density of 99.95% and the sample was subjected to EDS point scanning detection (10 points in total, with a minimum 500 μm separation between each two points) for a maximum of only 0.8% composition fluctuation.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (4)
1. A method of preparing an alloy block by SLM in situ alloying, said method comprising the steps of:
(1) Mixing ingredients and raw materials: adopting more than two kinds of powder as raw materials, drying and deoxidizing each powder, and uniformly mixing to obtain mixed powder; wherein:
the powder comprises pure metal simple substance powder and/or prealloyed powder;
the pure metal simple substance powder comprises at least one of Fe, cr, ni, co, mn, mo, and the prealloy powder comprises at least one of iron-based alloy, nickel-based alloy, cobalt-based alloy and high-entropy alloy;
the lowest mixing proportion of each powder is 1%, the powder is spherical, the particle size distribution is 15-53 mu m, the oxygen content is less than 500ppm, and the Hall flow rate is less than 20s/50g;
drying at 100-200deg.C under vacuum degree less than 10KPa absolute pressure for 2-3 hr;
(2) The following parameters were first set: the single-layer liquid state melting time length is more than or equal to 0.1s, the molten pool depth is more than 1.5 times of the layer thickness, the molten pool width is more than or equal to 0.5 times of the molten pool depth, the set parameters are used as constraint conditions, the set laser selective melting parameters and the set multistage laser post heat treatment parameters are input into finite element software COMSOL, and the technological parameters of 3D printing are determined; wherein:
the 3D printing process adopts laser selective melting and multistage laser post heat treatment to each layer of powder;
the specific setting of the laser selective melting parameters is as follows: the thickness of the powder spreading layer is 20-50 mu m, the laser power is 100-250W, the scanning speed is 600-1500mm/s, the scanning line distance is 50-200 mu m, the light spot diameter is 50-100 mu m, the single-layer scanning path is folded scanning, and the scanning path between layers is vertical scanning;
the parameters of the multistage laser post-heat treatment are specifically set as follows: the laser power is 100-300W, the scanning speed is 500-1200mm/s, the scanning line distance is 50-120 mu m, the spot diameter is 50-100 mu m, the single-layer scanning path is foldback scanning, and the scanning path between layers is vertical scanning;
(3) Under the protection of Ar gas, printing the mixed powder by a 3D printer, and separating a sample from a substrate by wire cutting after printing to obtain an SLM in-situ alloying preparation alloy block; wherein:
the oxygen content in 3D printing is controlled within 1000 ppm.
2. A method of preparing an alloy block by SLM in situ alloying according to claim 1, characterized in that in step (1) the purity of the pure elemental metal powder is > 99.5%.
3. A method of preparing an alloy block by SLM in situ alloying according to claim 2, characterized in that in step (1) mixing is performed for 3-24h at a rotational speed of 25-100 r/min.
4. The method for preparing an alloy block by SLM in-situ alloying according to claim 2, characterized in that in step (2), 2-6 stages are used for multi-stage laser post heat treatment, and the laser power of each stage is increased by 0-80W compared with the previous stage during scanning.
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| CN115401216B (en) * | 2022-09-21 | 2024-03-05 | 华北理工大学 | Method for preparing high-nitrogen stainless steel by alloy powder passing through selective laser melting |
| CN115446331B (en) * | 2022-09-21 | 2024-03-05 | 华北理工大学 | Method for preparing high-nitrogen stainless steel by laser melting of pure metal powder through selected area |
| CN116021035B (en) * | 2023-02-21 | 2024-10-15 | 上海工程技术大学 | Method for preparing high-strength and high-hardness stainless steel-based composite material by selective laser melting |
| CN117626030A (en) * | 2023-10-19 | 2024-03-01 | 东北电力大学 | Optimization method for high-entropy alloy performance and high-performance CoCrFeNiMn high-entropy alloy |
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