CN114523125A - Method for preparing alloy block through SLM (selective laser melting) in-situ alloying - Google Patents
Method for preparing alloy block through SLM (selective laser melting) in-situ alloying Download PDFInfo
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- 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
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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
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- B22F10/366—Scanning parameters, e.g. hatch distance or scanning strategy
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- 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
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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
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- 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
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- 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
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- B33Y70/00—Materials specially adapted for additive manufacturing
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- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- 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%
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- C—CHEMISTRY; METALLURGY
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- 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%
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- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
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Abstract
The invention relates to a method for preparing an alloy block by SLM (selective laser melting) in-situ alloying, which comprises the following steps: mixing the materials: the method comprises the following steps of (1) taking 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 according to the set forming process parameters by using finite element software COMSOL; and under the protection of Ar gas, printing the mixed powder by using a 3D printer. The method uses more than two kinds of powder as raw materials to replace prealloying powder with a single component for SLM printing, adopts a mode of selective laser melting and multistage laser post-heat treatment, calculates optimal process parameters by using finite element software COMSOL, can greatly reduce time and cost of trial and error tests, has sample density higher than 99.9 percent, uniform components, 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 (selective laser melting) in-situ alloying.
Background
Selective Laser Melting (SLM) is one of the mainstream processing technologies for metal additive manufacturing, and the used materials are usually pre-alloyed powders, i.e. the raw material powder materials are melted and alloyed before being prepared. The powder used by the SLM is mainly prepared by a vacuum atomization process, but only less than half or less of the prepared powder generally meets the use requirement of the SLM, different materials need to be matched by a corresponding powder preparation process, the development of a novel SLM material is restricted by complicated processes and high cost, and the variety of the current commercial material brands is very limited.
The element powder in-situ alloying technology is a method for directly completing alloying and synchronously forming a high-density sample piece in the selective laser melting process by adopting mixed simple substance powder or specific alloy powder as raw materials, is a high-efficiency and low-cost material research and development method, can break through the limitation of the powder preparation process of customized powder, has extremely high flexibility in the aspect of changing alloy components compared with an alloy powder SLM (selective laser melting), and can be used in the fields of new material development and multi-material printing.
However, due to the difference of physical property parameters of each component in the mixed powder, the in-situ alloying sample prepared by adopting the traditional SLM laser scanning strategy and process has a large number of defects, not only is the component uniformity poor, but also a large number of structural defects such as unmelted particles, holes and the like are caused, the mechanical property, the corrosion resistance and other service performances of the sample are greatly reduced, and the application of the technology is severely restricted. In addition, as the SLM process parameters are numerous, the regulation and control range of each parameter is wide, and the SLM process needs to be groped through multiple rounds of trial and error experiments in the process of optimizing the process, so that the SLM process is time-consuming, labor-consuming and high in cost.
The present invention has been made in view of the above 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 pre-alloy powder with a single component for SLM printing, adopts a mode of selective laser melting and multistage laser post-heat treatment, and utilizes finite element software COMSOL to calculate optimal process parameters, thereby greatly reducing the time and cost of trial and error tests, and the sample density of the alloy block obtained by the method is higher than 99.9%, and the alloy block has uniform components, no tissue segregation, no obvious holes and other common printing defects.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method of SLM in-situ alloying production of an alloy mass, the method comprising the steps of:
(1) mixing the materials: the method comprises the following steps of (1) drying and deoxidizing each powder by using more than two kinds of powder as raw materials, and uniformly mixing to obtain mixed powder;
(2) setting molding process parameters, and determining the process parameters of 3D printing according to the set molding process parameters by using finite element software COMSOL;
(3) and under the protection of Ar gas, printing the mixed powder by using a 3D printer, and separating a sample from the substrate by using linear cutting after printing to obtain the SLM in-situ alloying prepared alloy block.
Further, the powder in the step (1) comprises pure elemental metal powder and/or pre-alloyed powder.
Further, the pure metal elemental powder comprises at least one of Fe, Cr, Ni, Co, Mn and Mo, and the prealloyed powder comprises at least one of an iron-based alloy, a nickel-based alloy, a cobalt-based alloy and a high-entropy alloy.
Further, in the step (1), the minimum 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, the Hall flow rate is less than 20s/50g, and preferably, the purity of the pure metal elementary powder is more than 99.5%.
Further, in the step (1), the drying temperature is 100-.
Further, in the step (2), the 3D printing process adopts selective laser melting and multi-stage laser post-heat treatment on each layer of powder.
Further, the selective laser melting parameters are specifically set as follows: the thickness of the powder layer is 20-50 μm, the laser power is 100-250W, the scanning speed is 600-1500mm/s, the scanning line interval is 50-200 μm, the spot diameter is 50-100 μm, the single-layer scanning path is the turn-back type scanning, and the scanning path between layers is the 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 spacing is 50-120 μm, the spot diameter is 50-100 μm, the single-layer scanning path is a zigzag scanning, and the scanning path between layers is a vertical scanning.
Furthermore, the multi-stage laser post-heat treatment adopts 2-6 stages, and the laser power of each stage in the scanning process is increased by 0-80W compared with that of the previous stage.
Further, the following parameters are set first: the time length of the single-layer liquid state melting is more than or equal to 0.1s, the depth of the molten pool is more than 1.5 times of the layer thickness, the width of the molten pool is more than or equal to 0.5 times of the depth of the molten pool, the set parameters are used as constraint conditions, the set selective laser melting parameters and the set multi-stage laser post-heat treatment parameters are input into finite element software COMSOL, and the process parameters of 3D printing are determined.
Further, the oxygen content in the 3D printing in the step (3) is controlled within 1000 ppm.
The invention utilizes finite element software COMSOL to determine the technological parameters of 3D printing according to the set molding technological parameters, firstly establishes an SLM multi-channel scanning temperature field model, and the modeling mainly comprises the following steps:
(1) defining parameters: the method comprises the steps of selecting a laser area to melt parameters and performing multi-stage laser post-heat treatment;
(2) defining variables: the heat source adopts a Gaussian body heat source, and the path comprises 5 passes;
(3) establishing a model: comprises a base plate and a powder bed model;
(4) loading material from the software materials library: adding material properties to the substrate and the powder bed;
(5) setting a boundary condition: adding environmental radiation and Gaussian body heat source condition boundary conditions to the top surface of the powder bed;
(6) grid division: the mesh size of the powder bed is very fine, and the substrate has a conventional size;
(7) the study setup was: setting transient state research time;
(8) and (4) calculating.
And inputting the set selective laser melting parameters and the set multistage post-laser heat treatment parameters into a finite element model, and calculating appropriate 3D printing process parameters under the constraint conditions that the single-layer liquid melting time is more than or equal to 0.1s, the depth of a molten pool is more than 1.5 times of the layer thickness, and the width of the molten pool is more than or equal to 0.5 times of the depth of the molten pool.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention uses more than two kinds of powder as raw materials to replace the prealloying powder with single component to perform SLM printing, adopts a mode of selective laser melting and multi-stage laser post-heat treatment, and the multi-stage laser post-heat treatment can obviously improve the liquid state retention time of a molten pool in the printing process, so that various elements are fully diffused to form a homogenized solid solution, and the defects of tissue segregation, interface phase, unmelted particles and the like generated by the SLM of mixed powder can be effectively overcome; in addition, the multi-stage laser post-heat treatment can eliminate splashing particles, unmelted particles, spheroidized particles and unfused holes on the surface of a molten pool in a remelting mode, and is beneficial to improving the surface roughness of a sample, so that the number of hole defects in the sample is reduced, and the density of the sample is improved. The method has the advantages that the optimized technological parameters are calculated by using finite element software COMSOL, the time and the cost of trial and error tests can be greatly reduced, the sample density of the alloy block obtained by the method is higher than 99.9%, the components are uniform, the structure segregation is avoided, common printing defects such as obvious holes and the like are avoided, and the alloy block has good forming performance;
(2) the alloy block prepared by the method can break through the limitation of a powder preparation process of customized powder, has extremely high flexibility and strong universality in the aspect of 3D printing metal material component design, and is suitable for elemental powder of Fe, Cr, Ni, Co, Mn, Mo and the like and prealloy powder materials of iron-based alloy, nickel-based alloy, cobalt-based alloy, high-entropy alloy and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a diagram of a single layer scan path in a 3D printing process as described in the present invention;
FIG. 2 is a diagram of an inter-layer scan path in a 3D printing process as described in the present invention;
FIG. 3 is a finished drawing of a 304L stainless steel alloy block made according to example 1 of the present invention;
FIG. 4 is a graph of the density and defect analysis results of the 304L stainless steel alloy block prepared in example 1 of the present invention;
FIG. 5 is an EDS scan of a 304L stainless steel alloy block made according to example 1 of the present invention;
FIG. 6 is an XRD pattern of a bulk 304L stainless steel alloy prepared according to example 1 of the present invention;
FIG. 7 is a graph comparing the mechanical properties of 304L stainless steel alloy blocks prepared in example 1 of the present invention with those of 304L prealloyed powder stainless steel alloy blocks of the prior art.
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 is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
The 3D printing single layer scan path described in the present invention is shown in fig. 1, and the interlayer scan 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 the materials: weighing three elementary powder, namely spherical iron powder, chromium powder and nickel powder, prepared by a vacuum atomization method, according to the following mass fractions, wherein the three elementary powder comprises 73.0% of Fe, 18.0% of Cr and 9% of Ni, 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 pure metal elementary powder is more than 99.5%, drying each powder respectively at the drying temperature of 100 ℃ and the vacuum degree of less than 10KPa absolute pressure for 2h, placing each dried powder in a mixer, and fully and uniformly mixing, wherein the powder is mixed for 10h at the rotating speed of 50 r/min;
(2) setting forming process parameters, adopting a 3D printing process, wherein the 3D printing process adopts selective laser melting and multistage laser post-heat treatment on each layer of powder, establishing an SLM multi-channel scanning temperature field model by using finite element software COMSOL, and obtaining the following optimal process parameters through calculation:
the selective laser melting parameters are specifically set as follows: the thickness of the powder layer is 30 microns, the laser power is 150W, the scanning speed is 800mm/s, the scanning line interval is 100 microns, the diameter of a light spot is 60 microns, the single-layer scanning path is a turn-back type scanning, and the scanning path between layers is a 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 interval is 100 μm, the spot diameter is 50 μm, the single-layer scanning path is a turn-back type scanning, the scanning path between layers is a vertical scanning, the laser power of the 2 nd and 3 rd levels is respectively increased by 40W and 80W on the basis of the 1 st level, and the rest parameters are the same;
(3) and (2) placing the dried and deoxidized mixed powder into a metal 3D printer for printing, constructing a plurality of blocks (10mm multiplied by 8mm) with preset sizes, adopting Ar gas for protection in the printing process, wherein the oxygen content is within 1000ppm, adopting 304 stainless steel as a printing substrate, the size of the substrate is 300cm multiplied by 2cm, and separating a sample from the substrate by linear cutting after printing is finished to obtain the high-density and high-uniformity 304L stainless steel alloy block prepared by SLM in-situ alloying.
The finished product picture of the 304L stainless steel alloy block prepared in this example is shown in fig. 3, the density and defect analysis results are shown in fig. 4, it can be seen from fig. 4 that the components are uniform and have no segregation and no unmelted particles, the density is 99.96%, the EDS energy spectrum scanning diagram is shown in fig. 5, the maximum component fluctuation of the sample through EDS point scanning detection (10 points in total, and the minimum distance between every two points is 500 μm) is only 0.7%, the XRD analysis result is shown in fig. 6, the microstructure is a single-phase austenite structure, and is the same as the room temperature structure of the sample prepared by melting the 304L laser selective area of the pre-alloyed powder.
The mechanical property comparison of the 304L stainless steel alloy block prepared by the method of the present embodiment and the prealloyed powder 304L stainless steel alloy block of the prior art is shown in fig. 7. As can be seen from 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 182 HV. The tensile strength of the pre-alloyed powder 304L laser selective melting sample is 623MPa, the yield strength is 375MPa, the elongation is 63%, and the microhardness is 184 HV. In terms of mechanical properties, 304L stainless steel samples prepared by SLM in-situ alloying were at comparable levels to those prepared by selective laser melting of prealloyed powder 304L.
Example 2
The embodiment provides a method for preparing an Inconel625 nickel-based high-temperature alloy block with high compactness and high uniformity by SLM in-situ alloying, which comprises the following steps:
(1) mixing the materials: weighing five simple substance powders of spherical iron powder, chromium powder, nickel powder, molybdenum powder and niobium powder prepared by a vacuum atomization method according to the following mass fractions, wherein the particle size distribution of the single substance powders 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 more than 99.5 percent, drying the powders respectively at the drying temperature of 150 ℃ and the vacuum degree of less than 10KPa for 2.5h, placing the dried powders in a mixer, and fully and uniformly mixing the powders, wherein the powders are mixed for 24h at the rotating speed of 25 r/min;
(2) setting forming process parameters, adopting a 3D printing process, wherein the 3D printing process adopts selective laser melting and multistage laser post-heat treatment on each layer of powder, establishing an SLM multi-channel scanning temperature field model by using finite element software COMSOL, and obtaining the following optimal process parameters through calculation:
the selective laser melting parameters are specifically set as follows: the thickness of the powder layer is 20 microns, the laser power is 100W, the scanning speed is 600mm/s, the scanning line interval is 50 microns, the diameter of a light spot is 75 microns, the single-layer scanning path is a turn-back type scanning, and the scanning path between layers is a 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 interval is 50 μm, the spot diameter is 75 μm, the single-layer scanning path is a turn-back type scanning, the scanning path between layers is a 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 basis of the 1 st stage, and other parameters are the same;
(3) and (2) placing the dried and deoxidized mixed powder into a metal 3D printer for printing, constructing a plurality of blocks (10mm multiplied by 8mm) with preset sizes, adopting Ar gas for protection in the printing process, wherein the oxygen content is within 1000ppm, adopting 304 stainless steel as a printing substrate, the size of the substrate is 300cm multiplied by 2cm, and separating a sample from the substrate by linear cutting after printing is finished to obtain the Inconel625 nickel-based high-temperature alloy block with high density and high uniformity prepared by SLM in-situ alloying.
The compactness of the alloy block prepared in the embodiment is 99.94% through testing, and the maximum fluctuation of the components of the sample detected by EDS point scanning (taking 10 points in total and the minimum distance between every two points is 500 mu m) is only 1.1%.
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 the materials: weighing four simple substance powders of spherical iron powder, cobalt powder, chromium powder and nickel powder prepared by a vacuum atomization method, wherein the four simple substance powders comprise 24.76% of Fe, 26.13% of Co, 23.07% of Cr and 26.04% of Ni, 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 pure metal simple substance powder is more than 99.5%, drying the powders respectively at the drying temperature of 200 ℃ and the vacuum degree of less than 10KPa absolute pressure for 3h, and placing the dried powders in a mixer to be fully and uniformly mixed, wherein the mixing is carried out for 3h at the rotating speed of 100 r/min;
(2) setting forming process parameters, adopting a 3D printing process, wherein the 3D printing process adopts selective laser melting and multistage laser post-heat treatment on each layer of powder, establishing an SLM multi-channel scanning temperature field model by using finite element software COMSOL, and obtaining the following optimal process parameters through calculation:
the selective laser melting parameters are specifically set as follows: the thickness of the powder layer is 50 μm, the laser power is 250W, the scanning speed is 1500mm/s, the scanning line spacing is 200 μm, the spot diameter is 50 μm, the single-layer scanning path is a turn-back type scanning, and the scanning path between layers is a 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 interval is 120 μm, the spot diameter is 100 μm, the single-layer scanning path is a turn-back type scanning, the scanning path between layers is a vertical scanning, the laser energy values of the 2 nd, the 3 rd and the 4 th stages are increased by 12W step by step on the basis of the 1 st stage parameter, and the rest parameters are the same;
(3) and (2) placing the dried and deoxidized mixed powder into a metal 3D printer for printing, constructing a plurality of blocks (10mm multiplied by 8mm) with preset sizes, adopting Ar gas for protection in the printing process, wherein the oxygen content is within 1000ppm, adopting 304 stainless steel as a printing substrate, the size of the substrate is 300cm multiplied by 2cm, and separating a sample from the substrate by linear cutting after printing is finished to obtain the high-density and high-uniformity CoCrFeNi high-entropy alloy block prepared by SLM in-situ alloying.
The compactness of the alloy block prepared in the embodiment is 99.97% through testing, and the maximum fluctuation of the components of the sample detected by EDS point scanning (taking 10 points in total and the minimum distance between every two points is 500 μm) is only 0.9%.
Example 4
The embodiment provides a method for preparing a 304L-Inconel625 alloy block with high compactness and high uniformity by SLM (selective laser melting) in-situ alloying, which comprises the following steps:
(1) mixing the materials: weighing spherical 304L and Inconel625 alloy powder prepared by a vacuum atomization method, wherein the 304L is 50.00 percent, the Inconel 62550.00 percent are weighed according to the following mass fraction, 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, each powder is dried respectively, the drying temperature is 200 ℃, the vacuum degree is less than the absolute pressure of 10KPa for 3 hours, each dried powder is placed in a mixer to be fully and uniformly mixed, and the mixing is carried out for 3 hours at the rotating speed of 100 r/min;
(2) setting forming process parameters, adopting a 3D printing process, wherein the 3D printing process adopts selective laser melting and multistage laser post-heat treatment on each layer of powder, establishing an SLM multi-channel scanning temperature field model by using finite element software COMSOL, and obtaining the following optimal process parameters through calculation:
the selective laser melting parameters are specifically set as follows: the thickness of the powder layer is 30 microns, the laser power is 200W, the scanning speed is 1200mm/s, the distance between scanning lines is 150 microns, the diameter of a light spot is 60 microns, the single-layer scanning path is a turn-back type scanning, and the scanning path between layers is a 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 interval is 80 μm, the spot diameter is 80 μm, the single-layer scanning path is a turn-back type scanning, the scanning path between layers is a vertical scanning, the laser energy values of 2 nd and 3 rd stages are increased by 10W step by step on the basis of the 1 st stage parameter, and the rest parameters are the same;
(3) and (2) placing the dried and deoxidized mixed powder into a metal 3D printer for printing, constructing a plurality of blocks (10mm multiplied by 8mm) with preset sizes, adopting Ar gas for protection in the printing process, wherein the oxygen content is within 1000ppm, adopting 304 stainless steel as a printing substrate, the size of the substrate is 300cm multiplied by 2cm, and separating a sample from the substrate by linear cutting after printing is finished to obtain the high-density and high-uniformity 304L-Inconel625 alloy block prepared by SLM in-situ alloying.
The compactness of the alloy block prepared in the embodiment is 99.98% through testing, and the maximum fluctuation of the components of the sample detected by EDS point scanning (taking 10 points in total and the minimum distance between every two points is 500 mu m) is only 0.7%.
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 the materials: weighing two kinds of powder, namely spherical CoCrFeNi high-entropy alloy powder and Mo elemental powder, prepared by a vacuum atomization method, with the atomic ratio of CoCrFeNi being 72.00% and Mo28.00%, the particle size distribution of each powder being 15-53 mu m, the oxygen content being less than 500ppm, the Hall flow rate being less than 20s/50g, the purity of pure metal elemental powder being more than 99.5%, respectively drying each powder at the drying temperature of 200 ℃ and the vacuum degree being less than 10KPa absolute pressure for 3h, placing each dried powder in a mixer, and fully and uniformly mixing, wherein mixing is carried out for 3h at the rotating speed of 100 r/min;
(2) setting forming process parameters, adopting a 3D printing process, wherein the 3D printing process adopts selective laser melting and multistage laser post-heat treatment on each layer of powder, establishing an SLM multi-channel scanning temperature field model by using finite element software COMSOL, and obtaining the following optimal process parameters through calculation:
the selective laser melting parameters are specifically set as follows: the thickness of the powder layer is 30 microns, the laser power is 250W, the scanning speed is 1200mm/s, the distance between scanning lines is 150 microns, the diameter of a light spot is 60 microns, the single-layer scanning path is a turn-back type scanning, and the scanning path between layers is a 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 interval is 80 μm, the spot diameter is 80 μm, the single-layer scanning path is a turn-back type scanning, the scanning path between layers is a vertical scanning, the laser energy values of the 2 nd, the 3 rd and the 4 th stages are increased by 8W step by step on the basis of the 1 st stage parameter, and the rest parameters are the same;
(3) and (2) placing the dried and deoxidized mixed powder into a metal 3D printer for printing, constructing a plurality of blocks (10mm multiplied by 8mm) with preset sizes, adopting Ar gas for protection in the printing process, wherein the oxygen content is within 1000ppm, adopting 304 stainless steel as a printing substrate, the size of the substrate is 300cm multiplied by 2cm, and separating a sample from the substrate by linear cutting after printing is finished to obtain the high-density and high-uniformity CoCrFeNiMo high-entropy alloy block prepared by SLM in-situ alloying.
The compactness of the alloy block prepared in the embodiment is 99.95% through testing, and the maximum fluctuation of the components of the sample detected by EDS point scanning (taking 10 points in total and the minimum distance between every two points is 500 mu m) is only 0.8%.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily think of the changes or substitutions within the technical scope of the present invention, and shall cover 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 (10)
1. A method for preparing an alloy block by SLM (selective laser melting) in-situ alloying, which is characterized by comprising the following steps:
(1) mixing the materials: the method comprises the following steps of (1) drying and deoxidizing each powder by using more than two kinds of powder as raw materials, and uniformly mixing to obtain mixed powder;
(2) setting molding process parameters, and determining the process parameters of 3D printing according to the set molding process parameters by using finite element software COMSOL;
(3) and under the protection of Ar gas, printing the mixed powder by using a 3D printer, and separating a sample from the substrate by using linear cutting after printing to obtain the SLM in-situ alloying prepared alloy block.
2. The SLM in-situ alloying method for producing alloy block as claimed in claim 1, characterized in that the powder in step (1) comprises pure elemental metal powder and/or pre-alloyed powder.
3. The SLM in-situ alloying method for producing alloy block as claimed in claim 2, characterized in that said pure metal elemental powder comprises at least one of Fe, Cr, Ni, Co, Mn, Mo, and said prealloyed powder comprises at least one of Fe-based alloy, Ni-based alloy, Co-based alloy, high entropy alloy.
4. A SLM in-situ alloying method for the preparation of alloy blocks according to any of the claims 1-3 characterized in that in step (1) the minimum mixing ratio of each powder is 1%, said powder is spherical, the particle size distribution is 15-53 μm, the oxygen content is < 500ppm, the hall flow rate is < 20s/50g, preferably the purity of pure elemental metal powder is > 99.5%.
5. The SLM in-situ alloying method for preparing alloy block as claimed in claim 1, wherein the drying temperature in step (1) is 100-.
6. The SLM in-situ alloying method for preparing the alloy block body as claimed in claim 1, wherein the 3D printing process in step (2) adopts selective laser melting and multi-stage laser post-heat treatment for each layer of powder.
7. The SLM in-situ alloying method for preparing the alloy block as claimed in claim 6, wherein the selective laser melting parameters are specifically set as follows: the thickness of the powder layer is 20-50 μm, the laser power is 100-250W, the scanning speed is 600-1500mm/s, the scanning line interval is 50-200 μm, the spot diameter is 50-100 μm, the single-layer scanning path is the turn-back type scanning, and the scanning path between layers is the vertical scanning.
8. The SLM in-situ alloying method for preparing the alloy block according to claim 6, wherein the multi-stage laser post-heat treatment parameters are specifically set as follows: the laser power is 100-300W, the scanning speed is 500-1200mm/s, the scanning line spacing is 50-120 μm, the spot diameter is 50-100 μm, the single-layer scanning path is the turn-back type scanning, the scanning path between layers is the vertical scanning, preferably, the multi-stage laser post-heat treatment adopts 2-6 stages, and the laser power of each stage in the scanning process is increased by 0-80W compared with the previous stage.
9. A method for preparing alloy blocks by SLM in-situ alloying according to any of claims 6-8, characterized in that the following parameters are set first: the time length of the single-layer liquid state melting is more than or equal to 0.1s, the depth of the molten pool is more than 1.5 times of the layer thickness, the width of the molten pool is more than or equal to 0.5 times of the depth of the molten pool, the set parameters are used as constraint conditions, the set selective laser melting parameters and the set multi-stage laser post-heat treatment parameters are input into finite element software COMSOL, and the process parameters of 3D printing are determined.
10. The method for preparing the alloy block through SLM (selective laser melting) in-situ alloying according to claim 1, wherein the oxygen content in the 3D printing in the step (3) is controlled within 1000 ppm.
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