CN114737093B - Aluminum alloy powder material for aviation additive manufacturing, and preparation method and application thereof - Google Patents

Aluminum alloy powder material for aviation additive manufacturing, and preparation method and application thereof Download PDF

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CN114737093B
CN114737093B CN202210461018.6A CN202210461018A CN114737093B CN 114737093 B CN114737093 B CN 114737093B CN 202210461018 A CN202210461018 A CN 202210461018A CN 114737093 B CN114737093 B CN 114737093B
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aluminum
aluminum alloy
alloy powder
powder material
smelting
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CN114737093A (en
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赵春禄
李振民
胡万谦
王联波
张志辉
刘干
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Jiangxi Baohang New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/06Alloys based on aluminium with magnesium as the next major constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20Direct sintering or melting
    • B22F10/28Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60Treatment of workpieces or articles after build-up
    • B22F10/64Treatment of workpieces or articles after build-up by thermal means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y10/00Processes of additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y40/00Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/20Post-treatment, e.g. curing, coating or polishing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y70/00Materials specially adapted for additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00Products made by additive manufacturing
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/026Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48After-treatment of electroplated surfaces
    • C25D5/50After-treatment of electroplated surfaces by heat-treatment
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0824Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0848Melting process before atomisation
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

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  • Physics & Mathematics (AREA)
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Abstract

The invention provides an aluminum alloy powder material for aviation additive manufacturing, a preparation method and application, wherein the aluminum alloy powder material comprises the following components in percentage by mass: 4.5-6.5 wt% of Sc: 1.0 to 1.5 wt%, Zr: 0.5 to 0.8 wt%, Mn: 0.7-1.2 wt%, and the balance of Al. Compared with the common aluminum alloy powder material, the aluminum alloy powder material can break through the solid solution limit of the material during material forming, additive manufacturing is realized, a large amount of dispersed fine primary phases are generated due to the interaction of main elements in the material, the recrystallization of the structure is inhibited, and meanwhile, secondary phases are separated out from a matrix along with the heat treatment, so that the strength of the material is further improved, and the aluminum alloy powder material can be suitable for machine body structural members.

Description

Aluminum alloy powder material for aviation additive manufacturing, and preparation method and application thereof
Technical Field
The invention relates to the technical field of additive manufacturing, in particular to an aluminum alloy powder material for aviation additive manufacturing, and a preparation method and application thereof.
Background
With the development of five generations of fighters into a main force type, the development of the aviation industry puts higher requirements on pneumatic layout and weight reduction of a fuselage, the existing fuselage structure mainly comprises welding and riveting, the material mainly comprises aluminum alloy, titanium alloy and carbon-carbon composite material, and the aluminum alloy accounts for 50-70% of the material consumption of the fuselage, so that the weight reduction effect of the weight reduction of the fuselage after the structure of the aluminum alloy material is improved is most obvious.
At present, the development of a laser additive manufacturing process provides a wider idea for the improvement of a material structure, namely a design end, and the method is mainly characterized in that a special metal material, a special non-metal material and a special medical biological material are stacked layer by layer through software and a numerical control system on the basis of a digital model file by fusing computer aided design, a material processing and forming technology to manufacture a solid object in modes of extrusion, sintering, melting, photocuring, spraying and the like. And enables the manufacture of complex structural members that were previously constrained by conventional manufacturing methods and were not possible.
In the prior art, only part of Al-Si alloy and a small amount of Al-Mg alloy in the aluminum alloy material for aviation manufacturing can be subjected to laser additive forming, however, the material is influenced by a material system and the inherent solid solubility of elements in the aluminum alloy, and cannot meet the requirements of a machine body structural member, so that the aluminum alloy material for manufacturing the machine body structural member and performing additive manufacturing is urgently needed.
Disclosure of Invention
In view of the above, the invention aims to provide an aluminum alloy powder material for aviation additive manufacturing, a preparation method and an application thereof, and aims to solve the problem that an aluminum alloy material in the prior art cannot meet the performance requirements of a fuselage structural member and the additive manufacturing capability at the same time.
The embodiment of the invention is realized as follows: the aluminum alloy powder material for the aviation additive manufacturing comprises the following components in percentage by mass:
mg: 4.5-6.5 wt% of Sc: 1.0 to 1.5 wt%, Zr: 0.5 to 0.8 wt%, Mn: 0.7-1.2 wt%, and the balance of Al.
Further, the aluminum alloy powder material for aviation additive manufacturing is prepared from a combination of pure magnesium, pure aluminum, an aluminum-scandium alloy, an aluminum-zirconium alloy and a Mn electrolyte solution.
Further, the aluminum alloy powder material for aviation additive manufacturing comprises nickel, titanium, copper, silicon, cerium and silver, wherein the content of each of the nickel, the titanium, the copper, the silicon, the cerium and the silver is less than or equal to 0.5 wt%.
Another object of the present invention is to provide a method for preparing an aluminum alloy powder material, for preparing the aluminum alloy powder material, the method comprising:
weighing pure magnesium, pure aluminum, aluminum scandium alloy and aluminum zirconium alloy in a set proportion, placing the pure magnesium, the pure aluminum, the aluminum scandium alloy and the aluminum zirconium alloy in a smelting device, vacuumizing the smelting device, filling inert gas to atmospheric pressure, and smelting to obtain a smelting solution;
keeping the temperature of the smelting solution and standing to obtain an alloy solution; then carrying out high-speed inert gas flow atomization on the alloy solution to obtain original powder;
and grading and drying the original powder to obtain the aluminum alloy powder base material.
Wherein the vacuum degree of the smelting device is less than or equal to 100 Pa.
Further, the preparation method of the aluminum alloy powder material, wherein the step of obtaining the aluminum alloy powder base material by classifying and drying the original powder further comprises:
preparing a Mn electrolyte solution;
depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition;
finally, the aluminum alloy powder material is obtained through heat treatment;
wherein the current density of the deposited Mn is 30-50 mA/cm 2 The deposition time is 1-3 min.
Further, the preparation method of the aluminum alloy powder material comprises the following steps of smelting at 950-1050 ℃ and continuously heating to 950-1050 ℃ at a heating rate of 20-30 ℃/min;
wherein, when smelting, the pure aluminum is preheated firstly; the preheating temperature is 150-250 ℃;
then, the smelting temperature is increased to 700-800 ℃, after the pure aluminum is melted, the smelting temperature is increased to 950-1050 ℃, and then the aluminum scandium alloy and the aluminum zirconium alloy are sequentially added;
and after the pure magnesium is completely melted, reducing the melting temperature to 700-800 ℃, adding the pure magnesium, and after the pure magnesium is melted, carrying out heat preservation and standing.
Further, in the preparation method of the aluminum alloy powder material, in the step of heat preservation and standing, the heat preservation temperature is 1000-1100 ℃, and the heat preservation and standing time is 5-10 min.
Another object of the present invention is to provide an application method of the aluminum alloy powder prepared by the above preparation method, the application method comprising:
and taking the aluminum alloy powder material as a printing material, and printing the printing material into a finished product by adopting 3D printing based on a three-dimensional graphic file to be printed, wherein the finished product comprises an airplane rear fuselage.
Further, in the application method, the aluminum alloy powder material is used as a printing material, and in the step of printing the printing material to form a finished product based on the three-dimensional graphic file to be printed by adopting 3D printing, the printing is carried out by adopting SLM printing, and the preheating temperature of a printer plate is 100-120 ℃; the laser power is 350-370W; the scanning speed is 1100-1290 mm/s; the scanning distance is 0.1-0.15 mm; the thickness of the scanning layer is 0.03-0.09 mm; the area overlap is 0.15 mm.
Further, the application method, wherein after the step of printing the finished product of the printed material based on the three-dimensional graphic file to be printed by using the aluminum alloy powder material as the printed material and adopting 3D printing, further comprises:
carrying out vacuum heat treatment on the finished product and then air cooling; wherein the heat preservation temperature of the vacuum heat treatment is 300 ℃, and the heat preservation time is 4 h.
Compared with the prior art: theThe aluminum alloy powder material can break through the solid solution limit of the material during material forming, additive manufacturing is realized, and Mg, Sc and Zr elements in the material can interact with each other to generate a large amount of dispersed fine primary phases, such as Al 3 (Sc,Zr)、AlMg 2 In addition, as the heat treatment progresses, the dispersed distribution of these particles suppresses the recrystallization of the structure, and the secondary phase precipitates to further improve the strength of the material. The addition of Mn greatly improves the weldability of the material, avoids matrix fracture caused by plasticity reduction in the secondary phase precipitation process, and is suitable for machine body structural members; the Mn element is added in an electrochemical deposition mode, so that the gravity segregation of the high-content Mn element in the smelting process can be greatly solved, the electrochemical deposition adhesion effect is good, and the Mn element is uniformly distributed.
In addition, the aluminum alloy powder material provided by the invention at least has the following beneficial effects:
1. the problem of the unable shaping of current aluminum alloy material is solved.
2. The problem of the fuselage structure subtracts heavy behind the aircraft among the prior art is solved.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, as used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items. In the detailed description and claims, a list of items connected by the term "one of" may mean any of the listed items. For example, if items a and B are listed, the phrase "one of a and B" means a alone or B alone. In another example, if items A, B and C are listed, the phrase "one of A, B and C" means only a; only B; or only C. Item a may comprise a single element or multiple elements. Item B may comprise a single element or multiple elements. Item C may comprise a single element or multiple elements. In the detailed description and claims, a list of items connected by the term "at least one of," "at least one of," or other similar terms may mean any combination of the listed items. For example, if items a and B are listed, the phrase "at least one of a and B" or "at least one of a or B" means a only; only B; or A and B. In another example, if items A, B and C are listed, the phrase "at least one of A, B and C" or "at least one of A, B or C" means a only; or only B; only C; a and B (excluding C); a and C (excluding B); b and C (excluding A); or A, B and all of C. Item a may comprise a single element or multiple elements. Item B may comprise a single element or multiple elements. Item C may comprise a single element or multiple elements.
The invention provides an aluminum alloy powder material, a preparation method and application, aiming at the problem that an aluminum alloy material which has the manufacturing capability of a machine body structural part and the additive manufacturing capability does not exist at present, wherein the aluminum alloy powder material comprises magnesium (Mg), scandium (Sc), zirconium (Zr), manganese (Mn) and aluminum (Al), and the raw materials of the aluminum alloy powder material are pure magnesium, pure aluminum, an aluminum-scandium alloy, an aluminum-zirconium alloy and a manganese electrolyte solution.
In some embodiments of the present invention, the magnesium (Mg) is 4.5 to 6.5 wt%, for example, 4.5 wt%, 5.0 wt%, 5.5 wt%, 6.0 wt%, 6.5 wt%, etc.; scandium (Sc) in an amount of 1.0 to 1.5 wt%, for example, 1.1 wt%, 1.2 wt%, 1.3 wt%, 1.4 wt%, 1.5 wt%; zirconium (Zr) in an amount of 0.5 to 0.8 wt%, for example, 0.5wt%, 0.6 wt%, 0.7 wt%, 0.8 wt%, etc.; manganese (Mn) is 0.7 to 1.2 wt%, for example, 0.7 wt%, 0.8 wt%, 0.9 wt%, 1.0 wt%, 1.1 wt%, 1.2 wt%, etc.; the balance being aluminum (Al).
The invention also provides a preparation method of the aluminum alloy powder material, which is used for preparing the aluminum alloy powder material, and the method comprises the following steps:
weighing pure magnesium, pure aluminum, aluminum scandium alloy and aluminum zirconium alloy in a set proportion, placing the pure magnesium, the pure aluminum, the aluminum scandium alloy and the aluminum zirconium alloy in a smelting device, vacuumizing the smelting device, filling inert gas to atmospheric pressure, and smelting to obtain a smelting solution;
keeping the temperature of the smelting solution and standing to obtain an alloy solution; then carrying out high-speed inert gas flow atomization on the alloy solution to obtain original powder;
grading and drying the original powder to obtain an aluminum alloy powder base material;
wherein the vacuum degree of the smelting device is less than or equal to 100 Pa.
Further, the above aluminum alloy powder material production method, wherein,
the step of obtaining the aluminum alloy powder base material by grading and drying the original powder further comprises the following steps:
preparing a Mn electrolyte solution;
depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition;
finally, the aluminum alloy powder material is obtained through heat treatment;
wherein the current density of Mn deposition is 30-50 mA/cm2, and the deposition time is 1-3 min.
Further, in the preparation method of the aluminum alloy powder material, the pure magnesium, the pure aluminum, the aluminum scandium alloy and the aluminum zirconium alloy in a set proportion are weighed and placed in a smelting device to be smelted to obtain a smelting solution, and the smelting temperature is 950 to 1050 ℃, for example, 950 ℃, 970 ℃, 1000 ℃ and 1050 ℃.
Further, in some preferred embodiments of the present invention, the heating is continuously performed to 950-1050 ℃ at a heating rate of 20-30 ℃/min.
Further, in the preparation method of the aluminum alloy powder material, in the step of obtaining the alloy solution by keeping the molten metal warm and standing, the temperature is kept at 1000-1100 ℃, and the temperature is kept and the standing time is kept for 5-10 min, for example, the temperature is kept at 1000 ℃, 1050 ℃ and 1100 ℃; keeping the temperature and standing for 5min, 7min and 10 min.
Further, in some optional embodiments of the present invention, the pure aluminum is preheated during smelting; the preheating temperature is 150-250 ℃;
then, the smelting temperature is increased to 700-800 ℃, after the pure aluminum is melted, the smelting temperature is increased to 950-1050 ℃, and then the aluminum scandium alloy and the aluminum zirconium alloy are sequentially added;
and after the pure magnesium is completely melted, reducing the melting temperature to 700-800 ℃, adding the pure magnesium, and after the pure magnesium is melted, carrying out heat preservation and standing.
In addition, in some preferred embodiments of the present invention, the aluminum alloy powder material further includes nickel, titanium, copper, silicon, cerium, and silver, and each content of the nickel, titanium, copper, silicon, cerium, and silver is 0.5wt% or less.
During preparation, nickel, titanium, copper, silicon, cerium and silver can be independently smelted in an alloy form, pure magnesium, pure aluminum, aluminum scandium alloy and aluminum zirconium alloy in set proportion are weighed and placed in a smelting device for smelting, respective smelting liquids are mixed, and finally, heat preservation and standing are carried out to obtain the final alloy solution for preparing the original powder.
The invention also provides an application method of the aluminum alloy powder prepared by the preparation method, which comprises the following steps:
and taking the aluminum alloy powder material as a printing material, and printing the printing material into a finished product by adopting 3D printing based on a three-dimensional graphic file to be printed, wherein the finished product comprises an airplane rear fuselage.
In some optional embodiments of the invention, in the step of printing the printing material to obtain a finished product based on the three-dimensional graphic file to be printed by 3D printing with the aluminum alloy powder material as the printing material, the printing is performed by SLM printing, and the preheating temperature of a printer plate is 100-120 ℃, for example, 100 ℃, 110 ℃ and 120 ℃; the laser power is 350-370W, such as 350W, 360W and 370W; the scanning speed is 1100-1290 mm/s, such as 1100mm/s, 1200mm/s and 1290 mm/s; the scanning interval is 0.1-0.15 mm, such as 0.1mm, 0.12mm, 0.15 mm; the thickness of the scanning layer is 0.03-0.09 mm, such as 0.03mm, 0.06mm and 0.09 mm; the area overlap is 0.15 mm.
In some optional embodiments of the present invention, the step of printing the printing material into a finished product based on the three-dimensional graphic file to be printed by 3D printing using the aluminum alloy powder material as the printing material further includes:
carrying out vacuum heat treatment on the finished product and then air cooling; wherein the heat preservation temperature of the vacuum heat treatment is 300 ℃, and the heat preservation time is 4 hours.
In order to facilitate an understanding of the invention, several embodiments of the invention are set forth below. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Example 1
According to the mass percentage of Mg: 4.5 wt%, Sc: 1.0 wt%, Zr: 0.5wt% and the balance of Al; weighing required amounts of raw materials, namely pure magnesium alloy, pure aluminum alloy, aluminum scandium alloy and aluminum zirconium alloy, and placing the raw materials into a smelting device; vacuumizing the smelting device until the vacuum degree is 90Pa, and then filling inert gas to atmospheric pressure; then placing the mixture into a 950 ℃ condition to be smelted into a smelting solution, and then placing the smelting solution into a 1000 ℃ condition to be kept warm and placed for 5min to obtain an alloy melt; nitrogen is filled into a smelting device, the prepared alloy smelting liquid is atomized by high-speed inert gas flow, and the alloy smelting liquid is crushed into small liquid drops to obtain original powder; grading and drying the original powder to obtain an aluminum alloy powder base material; preparing a Mn electrolyte solution according to the Mn content of 0.7 wt%; depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition; finally, the aluminum alloy powder material is obtained through heat treatment; wherein the current density of the deposited Mn is 30-50 mA/cm 2 The deposition time is 1-3 min.
The aluminum alloy powder material is subjected to additive manufacturing and forming by 3D printing under the conditions that the preheating temperature of a printer plate is 100 ℃, the laser power is 350W, the scanning speed is 1100mm/s, the scanning interval is 0.1mm, the scanning layer thickness is 0.03mm and the area overlapping is 0.15mm, and then is subjected to heat treatment under the conditions that the heat preservation temperature is 300 ℃ and the heat preservation time is 4 hours, and then is subjected to air cooling.
Example 2
According to the mass percentage of Mg: 5.0 wt%, Sc: 1.1 wt%, Zr: 0.6 wt% and the balance of Al; weighing required amounts of raw materials, namely pure magnesium alloy, pure aluminum alloy, aluminum scandium alloy and aluminum zirconium alloy, and placing the raw materials into a smelting device; vacuumizing the smelting device until the vacuum degree is 92Pa, and then filling inert gas to atmospheric pressure; then placing the mixture at 1000 ℃ to be smelted into a smelting solution, and then placing the smelting solution at 1020 ℃ to be kept warm and placed for 8min to obtain an alloy melt; nitrogen is filled into a smelting device, the prepared alloy smelting liquid is atomized by high-speed inert gas flow, and the alloy smelting liquid is crushed into small liquid drops to obtain original powder; grading and drying the original powder to obtain an aluminum alloy powder base material; preparing a Mn electrolyte solution according to the Mn content of 0.8 wt%; depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition; finally, the aluminum alloy powder material is obtained through heat treatment; wherein the current density of the deposited Mn is 30-50 mA/cm2, and the deposition time is 1-3 min.
The aluminum alloy powder material is subjected to additive manufacturing and forming by 3D printing under the conditions that the preheating temperature of a printer plate is 110 ℃, the laser power is 360W, the scanning speed is 1150mm/s, the scanning interval is 0.11mm, the scanning layer thickness is 0.04mm and the zone overlapping is 0.15mm, and then is subjected to heat treatment under the conditions that the heat preservation temperature is 300 ℃ and the heat preservation time is 4 hours, and then is subjected to air cooling.
Example 3
According to the mass percentage of Mg: 5.5 wt%, Sc: 1.2 wt%, Zr: 0.7 wt% and the balance of Al; weighing required amounts of raw materials, namely pure magnesium alloy, pure aluminum alloy, aluminum scandium alloy and aluminum zirconium alloy, and placing the raw materials into a smelting device; vacuumizing the smelting device until the vacuum degree is 92Pa, and then filling inert gas to atmospheric pressure; then placing the mixture at 1000 ℃ to be smelted into a smelting solution, then placing the smelting solution at 1050 ℃ to be kept warm and kept stand for 8min to obtain an alloy melt; nitrogen is filled into a smelting device, the prepared alloy smelting liquid is atomized by high-speed inert gas flow, and the alloy smelting liquid is crushed into small liquid drops to obtain original powder; grading and drying the original powder to obtain an aluminum alloy powder base material; preparing a Mn electrolyte solution according to the Mn content of 0.9 wt%; depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition; finally, the aluminum alloy powder material is obtained through heat treatment; wherein the current density of Mn deposition is 30-50 mA/cm2, and the deposition time is 1-3 min.
The method comprises the steps of conducting additive manufacturing forming on an aluminum alloy powder material through 3D printing under the conditions that the preheating temperature of a printer plate is 120 ℃, the laser power is 365W, the scanning speed is 1200mm/s, the scanning distance is 0.12mm, the scanning layer thickness is 0.05mm, and the area overlapping is 0.15mm, conducting heat treatment on the aluminum alloy powder material under the conditions that the heat preservation temperature is 300 ℃, the heat preservation time is 4 hours, and then conducting air cooling.
Example 4
According to the mass percentage of Mg: 6.0 wt%, Sc: 1.2 wt%, Zr: 0.7 wt% and the balance of Al; weighing required amounts of raw materials, namely pure magnesium alloy, pure aluminum alloy, aluminum scandium alloy and aluminum zirconium alloy, and placing the raw materials into a smelting device; vacuumizing the smelting device until the vacuum degree is 88Pa, and then filling inert gas to atmospheric pressure; then placing the mixture into a 950 ℃ condition to be smelted into a smelting solution, then placing the smelting solution into a 1050 ℃ condition to be kept warm and placed for 5min to obtain an alloy solution; nitrogen is filled into a smelting device, the prepared alloy smelting liquid is atomized by high-speed inert gas flow, and the alloy smelting liquid is crushed into small liquid drops to obtain original powder; grading and drying the original powder to obtain an aluminum alloy powder base material; preparing a Mn electrolyte solution according to the Mn content of 1.1 wt%; depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition; finally, obtaining the aluminum alloy powder material through heat treatment; wherein the current density of Mn deposition is 30-50 mA/cm2, and the deposition time is 1-3 min.
The aluminum alloy powder material is subjected to additive manufacturing and molding by 3D printing under the conditions that the preheating temperature of a printer plate is 120 ℃, the laser power is 365W, the scanning speed is 1200mm/s, the scanning interval is 0.12mm, the scanning layer thickness is 0.03mm and the zone overlapping is 0.15mm, and then is subjected to heat treatment under the conditions that the heat preservation temperature is 300 ℃ and the heat preservation time is 4 hours, and then is subjected to air cooling.
Example 5
According to the mass percentage of Mg: 6.5 wt%, Sc: 1.3 wt%, Zr: 0.8 wt% and the balance of Al; weighing required amounts of raw materials, namely pure magnesium alloy, pure aluminum alloy, aluminum scandium alloy and aluminum zirconium alloy, and placing the raw materials into a smelting device; vacuumizing the smelting device until the vacuum degree is 88Pa, and then filling inert gas to atmospheric pressure; then placing the mixture at 1000 ℃ to be smelted into a smelting solution, then placing the smelting solution at 1050 ℃ to be kept warm and kept stand for 10min to obtain an alloy melt; nitrogen is filled into a smelting device, the prepared alloy smelting liquid is atomized by high-speed inert gas flow, and the alloy smelting liquid is crushed into small liquid drops to obtain original powder; grading and drying the original powder to obtain an aluminum alloy powder base material; preparing a Mn electrolyte solution according to the Mn content of 1.0 wt%; depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition; finally, obtaining the aluminum alloy powder material through heat treatment; wherein the current density of Mn deposition is 30-50 mA/cm2, and the deposition time is 1-3 min.
The aluminum alloy powder material is subjected to additive manufacturing and molding by 3D printing under the conditions that the preheating temperature of a printer plate is 120 ℃, the laser power is 365W, the scanning speed is 1250mm/s, the scanning interval is 0.13mm, the scanning layer thickness is 0.04mm and the area overlapping is 0.15mm, and then is subjected to heat treatment under the conditions that the heat preservation temperature is 300 ℃ and the heat preservation time is 4 hours, and then is subjected to air cooling.
Example 6
According to the mass percentage of Mg: 6.5 wt%, Sc: 1.4 wt%, Zr: 0.8 wt% and the balance of Al; weighing required amounts of raw materials, namely pure magnesium alloy, pure aluminum alloy, aluminum scandium alloy and aluminum zirconium alloy, and placing the raw materials into a smelting device; vacuumizing the smelting device until the vacuum degree is 95Pa, and then filling inert gas to atmospheric pressure; then placing the mixture into 1020 ℃ to be smelted into smelting liquid, then placing the smelting liquid into 1050 ℃ to be kept warm and kept stand for 10min to obtain alloy melt; introducing nitrogen into a smelting device, atomizing the prepared alloy smelting liquid by using high-speed inert gas flow, and crushing the alloy smelting liquid into small liquid drops to obtain original powder; grading and drying the original powder to obtain an aluminum alloy powder base material; preparing a Mn electrolyte solution according to the Mn content of 1.1 wt%; depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition; finally, the aluminum alloy powder material is obtained through heat treatment; wherein the current density of Mn deposition is 30-50 mA/cm2, and the deposition time is 1-3 min.
The aluminum alloy powder material is subjected to additive manufacturing and forming by 3D printing under the conditions that the preheating temperature of a printer plate is 120 ℃, the laser power is 370W, the scanning speed is 1270mm/s, the scanning distance is 0.14mm, the scanning layer thickness is 0.05mm and the zone overlapping is 0.15mm, and then the aluminum alloy powder material is subjected to heat treatment under the conditions that the heat preservation temperature is 300 ℃ and the heat preservation time is 4 hours and then air cooling.
Example 7
According to the mass percentage of Mg: 6.5 wt%, Sc: 1.5 wt%, Zr: 0.8 wt% and the balance Al; weighing required amounts of raw materials, namely pure magnesium alloy, pure aluminum alloy, aluminum scandium alloy and aluminum zirconium alloy, and placing the raw materials into a smelting device; vacuumizing the smelting device until the vacuum degree is 88Pa, and then filling inert gas to atmospheric pressure; then placing the mixture at 1050 ℃ to be smelted into smelting liquid, then placing the smelting liquid at 1050 ℃ to be kept warm and kept stand for 10min to obtain alloy melt; nitrogen is filled into a smelting device, the prepared alloy smelting liquid is atomized by high-speed inert gas flow, and the alloy smelting liquid is crushed into small liquid drops to obtain original powder; grading and drying the original powder to obtain an aluminum alloy powder base material; preparing a Mn electrolyte solution according to the Mn content of 1.2 wt%; depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition; finally, obtaining the aluminum alloy powder material through heat treatment; wherein the current density of the deposited Mn is 30-50 mA/cm2, and the deposition time is 1-3 min.
The aluminum alloy powder material is subjected to additive manufacturing and molding by 3D printing under the conditions that the preheating temperature of a printer plate is 120 ℃, the laser power is 370W, the scanning speed is 1290mm/s, the scanning interval is 0.15mm, the scanning layer thickness is 0.06mm and the zone overlapping is 0.15mm, and then the aluminum alloy powder material is subjected to heat treatment under the conditions that the heat preservation temperature is 300 ℃ and the heat preservation time is 4 hours and then air cooling is carried out.
Example 8
According to the mass percentage of Mg: 6.5 wt%, Sc: 1.5 wt%, Zr: 0.8 wt% and the balance Al; weighing required amounts of raw materials, namely pure magnesium alloy, pure aluminum alloy, aluminum scandium alloy and aluminum zirconium alloy, and placing the raw materials into a smelting device; vacuumizing the smelting device until the vacuum degree is 80Pa, and then filling inert gas to atmospheric pressure; then placing the mixture at 1050 ℃ to be smelted into a smelting solution, and then placing the smelting solution at 1100 ℃ for heat preservation and standing for 10min to obtain an alloy melt; introducing nitrogen into a smelting device, atomizing the prepared alloy smelting liquid by using high-speed inert gas flow, and crushing the alloy smelting liquid into small liquid drops to obtain original powder; grading and drying the original powder to obtain an aluminum alloy powder base material; preparing a Mn electrolyte solution according to the Mn content of 1.2 wt%; depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition; finally, the aluminum alloy powder material is obtained through heat treatment; wherein the current density of Mn deposition is 30-50 mA/cm2, and the deposition time is 1-3 min.
The method comprises the steps of conducting additive manufacturing forming on an aluminum alloy powder material through 3D printing under the conditions that the preheating temperature of a printer plate is 120 ℃, the laser power is 370W, the scanning speed is 1290mm/s, the scanning distance is 0.15mm, the scanning layer thickness is 0.09mm, and the area overlapping is 0.15mm, then conducting heat treatment under the conditions that the heat preservation temperature is 300 ℃ and the heat preservation time is 4 hours, and then conducting air cooling.
Example 9
According to the mass percentage of Mg: 6.5 wt%, Sc: 1.5 wt%, Zr: 0.8 wt% and the balance of Al; weighing required amounts of raw materials, namely pure magnesium alloy, pure aluminum alloy, aluminum scandium alloy and aluminum zirconium alloy, and placing the raw materials into a smelting device; vacuumizing the smelting device until the vacuum degree is 80Pa, and then filling inert gas to atmospheric pressure; continuously heating to 950 ℃ at the heating rate of 20-30 ℃/min, smelting into a smelting solution, and standing the smelting solution at 1100 ℃ for 10min to obtain an alloy solution; nitrogen is filled into a smelting device, the prepared alloy smelting liquid is atomized by high-speed inert gas flow, and the alloy smelting liquid is crushed into small liquid drops to obtain original powder; grading and drying the original powder to obtain an aluminum alloy powder base material; preparing a Mn electrolyte solution according to the Mn content of 1.2 wt%; depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition; finally, the aluminum alloy powder material is obtained through heat treatment; wherein the current density of Mn deposition is 30-50 mA/cm2, and the deposition time is 1-3 min.
The aluminum alloy powder material is subjected to additive manufacturing molding by 3D printing under the conditions that the preheating temperature of a printer plate is 120 ℃, the laser power is 370W, the scanning speed is 1290mm/s, the scanning interval is 0.15mm, the scanning layer thickness is 0.09mm and the zone overlapping is 0.15mm, and then the aluminum alloy powder material is subjected to heat treatment under the conditions that the heat preservation temperature is 300 ℃ and the heat preservation time is 4 hours and then air cooling is carried out.
Example 10
According to the mass percentage of Mg: 6.5 wt%, Sc: 1.5 wt%, Zr: 0.8 wt% and the balance of Al; vacuumizing the smelting device until the vacuum degree is 80Pa, and then filling inert gas to atmospheric pressure; adding pure aluminum, and preheating the pure aluminum; the preheating temperature is 200 ℃; then, the melting temperature is increased to 750 ℃, and after the pure aluminum is melted, the melting temperature is increased to 1050 ℃, and then the aluminum-scandium alloy and the aluminum-zirconium alloy are sequentially added; and after the pure magnesium is completely melted, reducing the melting temperature to 750 ℃, adding the pure magnesium, and after the pure magnesium is melted, keeping the temperature and standing. Then placing the smelting solution at 1100 ℃ and standing for 10min to obtain an alloy solution; nitrogen is filled into a smelting device, the prepared alloy smelting liquid is atomized by high-speed inert gas flow, and the alloy smelting liquid is crushed into small liquid drops to obtain original powder; grading and drying the original powder to obtain an aluminum alloy powder base material; preparing a Mn electrolyte solution according to the Mn content of 1.2 wt%; depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition; finally, obtaining the aluminum alloy powder material through heat treatment; wherein the current density of Mn deposition is 30-50 mA/cm2, and the deposition time is 1-3 min.
The aluminum alloy powder material is subjected to additive manufacturing molding by 3D printing under the conditions that the preheating temperature of a printer plate is 120 ℃, the laser power is 370W, the scanning speed is 1290mm/s, the scanning interval is 0.15mm, the scanning layer thickness is 0.09mm and the zone overlapping is 0.15mm, and then the aluminum alloy powder material is subjected to heat treatment under the conditions that the heat preservation temperature is 300 ℃ and the heat preservation time is 4 hours and then air cooling is carried out.
Example 11
According to the mass percentage of Mg: 6.5 wt%, Sc: 1.5 wt%, Zr: 0.8 wt% and the balance of Al; vacuumizing the smelting device until the vacuum degree is 80Pa, and then filling inert gas to atmospheric pressure; adding pure aluminum, and preheating the pure aluminum; the preheating temperature is 200 ℃; then, the melting temperature is increased to 750 ℃, and after the pure aluminum is melted, the melting temperature is increased to 1050 ℃, and then the aluminum-scandium alloy and the aluminum-zirconium alloy are sequentially added; after the mixture is completely melted, reducing the melting temperature to 750 ℃, adding pure magnesium, obtaining a melting solution after the pure magnesium is melted, respectively melting dopants of nickel, titanium, copper, silicon, cerium and silver in an alloy mode, wherein the doping content of each dopant is less than or equal to 0.5wt%, mixing the dopants with the melting solution after the melting is finished, and then placing the mixed melting solution at 1100 ℃ for heat preservation and standing for 10min to obtain an alloy solution; nitrogen is filled into a smelting device, the prepared alloy smelting liquid is atomized by high-speed inert gas flow, and the alloy smelting liquid is crushed into small liquid drops to obtain original powder; grading and drying the original powder to obtain an aluminum alloy powder base material; preparing a Mn electrolyte solution according to the Mn content of 1.2 wt%; depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition; finally, the aluminum alloy powder material is obtained through heat treatment; wherein the current density of Mn deposition is 30-50 mA/cm2, and the deposition time is 1-3 min.
The aluminum alloy powder material is subjected to additive manufacturing molding by 3D printing under the conditions that the preheating temperature of a printer plate is 120 ℃, the laser power is 370W, the scanning speed is 1290mm/s, the scanning interval is 0.15mm, the scanning layer thickness is 0.09mm and the zone overlapping is 0.15mm, and then the aluminum alloy powder material is subjected to heat treatment under the conditions that the heat preservation temperature is 300 ℃ and the heat preservation time is 4 hours and then air cooling is carried out.
Referring to Table 1 below, the parameters for the above examples 1-11 of the present invention are shown in the following table:
TABLE 1
Figure BDA0003622211630000131
In practical applications, the molded parts prepared by the above-mentioned examples 1-10 of the present invention were tested, and the test data are shown in the following table 2
TABLE 2
Figure BDA0003622211630000132
Figure BDA0003622211630000141
In summary, it is apparent from the data in tables 1 and 2 that the formed part prepared by the present invention breaks through the solid solution limit of the material, and generates a large amount of dispersed fine primary phases such as Al3(Sc, Zr) and AlMg2, etc. through the interaction of Mg, Sc and Zr elements, and as the heat treatment progresses, the particles are dispersed and distributed to inhibit the recrystallization of the structure, and simultaneously, the secondary phase is precipitated to further improve the strength of the material. The addition of Mn element greatly improves the weldability of the material and avoids the fracture of the matrix caused by the reduction of plasticity in the secondary phase precipitation process. Meanwhile, the 3D printing method is adopted to realize the interaction of all elements in the multi-element alloy, and the restriction of the solid solubility of the components on the improvement of the material performance is greatly improved. On the basis of the existing components, after the addition of elements such as Ni, Ti, Cu, Si, Ce, Ag and the like is tried, a large amount of fine and dispersed hard particles are formed in the heat treatment process, the strength is improved, and meanwhile, the ductility of the material is improved to a certain extent.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (9)

1. A method of making an aluminum alloy powder material, the method comprising:
weighing pure magnesium, pure aluminum, aluminum scandium alloy and aluminum zirconium alloy in a set proportion, placing the pure magnesium, the pure aluminum, the aluminum scandium alloy and the aluminum zirconium alloy in a smelting device, vacuumizing the smelting device, filling inert gas to atmospheric pressure, and smelting to obtain a smelting solution;
keeping the temperature of the smelting solution and standing to obtain an alloy solution; then carrying out high-speed inert gas flow atomization on the alloy solution to obtain original powder;
grading and drying the original powder to obtain an aluminum alloy powder base material;
preparing a Mn electrolyte solution;
depositing a layer of Mn on the aluminum alloy powder substrate by electrochemical deposition;
finally, obtaining an aluminum alloy powder material through heat treatment;
wherein the vacuum degree of the smelting device is less than or equal to 100Pa, and the current density of the deposited Mn is 30-50 mA/cm 2 The deposition time is 1-3 min.
2. The method for preparing an aluminum alloy powder material according to claim 1, wherein during smelting, the smelting temperature is 950 to 1050 ℃, and the aluminum alloy powder material is continuously heated to 950 to 1050 ℃ at a heating rate of 20 to 30 ℃/min;
wherein, when smelting, pure aluminum is preheated firstly; the preheating temperature is 150-250 ℃;
then, the smelting temperature is increased to 700-800 ℃, after the pure aluminum is melted, the smelting temperature is increased to 950-1050 ℃, and then the aluminum scandium alloy and the aluminum zirconium alloy are sequentially added;
and after the magnesium is completely melted, reducing the melting temperature to 700-800 ℃, adding pure magnesium, and after the pure magnesium is melted, carrying out heat preservation and standing.
3. The method for preparing the aluminum alloy powder material according to claim 1 or 2, wherein in the step of holding and standing, the holding temperature is 1000 to 1100 ℃, and the holding and standing time is 5 to 10 min.
4. An aluminum alloy powder material for aviation additive manufacturing, which is prepared by the method for preparing the aluminum alloy powder material according to any one of claims 1 to 3, and comprises the following components in percentage by mass:
mg: 4.5-6.5 wt% of Sc: 1.0 to 1.5 wt%, Zr: 0.5 to 0.8 wt%, Mn: 0.7-1.2 wt%, and the balance of Al.
5. The aluminum alloy powder material for aerospace additive manufacturing according to claim 4, wherein the raw material of the aluminum alloy powder material is a combination of pure magnesium, pure aluminum, aluminum scandium alloy, aluminum zirconium alloy, and Mn electrolyte solution.
6. The aluminum alloy powder material for aerospace additive manufacturing of claim 4, further comprising nickel, titanium, copper, silicon, cerium, and silver, each content of nickel, titanium, copper, silicon, cerium, and silver being 0.5wt% or less.
7. An application method of the aluminum alloy powder material prepared by the preparation method of any one of claims 1 to 3, which is characterized by comprising the following steps:
and taking the aluminum alloy powder material as a printing material, and printing the printing material into a finished product based on a three-dimensional graphic file to be printed by adopting 3D printing.
8. The application method of the aluminum alloy powder material as the printing material, wherein in the step of printing the printing material to be a finished product based on the three-dimensional graphic file to be printed by 3D printing, the printing is performed by adopting SLM printing, and the preheating temperature of a printer plate is 100-120 ℃; the laser power is 350-370W; the scanning speed is 1100-1290 mm/s; the scanning distance is 0.1-0.15 mm; the thickness of the scanning layer is 0.03-0.09 mm; the area overlap is 0.15 mm.
9. The application method of claim 7, wherein the step of printing the aluminum alloy powder material as a printing material into a finished product based on a three-dimensional graphic file to be printed by 3D printing further comprises the following steps:
carrying out vacuum heat treatment on the finished product and then air-cooling; wherein the heat preservation temperature of the vacuum heat treatment is 300 ℃, and the heat preservation time is 4 h.
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