CN117532012A - Al-Ce-Mg aluminum alloy for metal 3D printing and preparation method thereof - Google Patents

Al-Ce-Mg aluminum alloy for metal 3D printing and preparation method thereof Download PDF

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Publication number
CN117532012A
CN117532012A CN202311577270.4A CN202311577270A CN117532012A CN 117532012 A CN117532012 A CN 117532012A CN 202311577270 A CN202311577270 A CN 202311577270A CN 117532012 A CN117532012 A CN 117532012A
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aluminum alloy
alloy
printing
preparation
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魏午
胡继飞
黄晖
文胜平
高坤元
毕舰磊
翟玉妍
聂祚仁
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Beijing University of Technology
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Beijing University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/36—Process control of energy beam parameters
    • B22F10/366—Scanning parameters, e.g. hatch distance or scanning strategy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60—Treatment of workpieces or articles after build-up
    • B22F10/64—Treatment of workpieces or articles after build-up by thermal means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making 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
    • B22F9/082—Making 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/10—Pre-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/20—Post-treatment, e.g. curing, coating or polishing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00—Products made by additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0408—Light metal alloys
    • C22C1/0416—Aluminium-based alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/047—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with magnesium as the next major constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making 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
    • B22F9/082—Making 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
    • B22F2009/0848—Melting process before atomisation

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Abstract

An Al-Ce-Mg aluminum alloy for metal 3D printing and a preparation method thereof belong to the technical field of metal 3D printing materials. The components are as follows according to the mass percent: the content of Ce is 8-12%, the content of Mg is 7-10%, the content of Er is 0.3-0.9%, the content of Zr is 0.3-0.5, and the balance is Al. The eutectic structure can be thinned in the rapid solidification process of laser printing additive manufacturing compared with the traditional casting process, and the alloy prepared by the method can separate out tiny and dispersed Al in the aging process compared with the Al-Ce-Mg ternary alloy prepared by the same process 3 The (Er, zr) nano particles can play roles in precipitation strengthening and dislocation fixing, can effectively prevent coarsening of grain size in the heat exposure process, and have excellent mechanical properties and heat stability.

Description

Al-Ce-Mg aluminum alloy for metal 3D printing and preparation method thereof
Technical Field
The invention belongs to the technical field of special materials for metal 3D printing, and particularly relates to an Al-Ce-Mg aluminum alloy for metal 3D printing and a preparation method thereof, which are suitable for printing aluminum alloy with heat resistance requirements in the aerospace field.
Background
Additive manufacturing technology (also known as 3D printing technology) is a technology that uses bondable materials such as metal powder to construct objects by layer-by-layer printing. Because of the low density and high specific mechanical properties of aluminum alloys, there is a great interest in the field of additive manufacturing. Al-Ce eutectic alloys have attracted considerable attention due to their good high temperature properties and printability. As with the near-eutectic Al-Si alloy, the near-eutectic Al-Ce alloy has a narrower solidification range and can inhibit cracks in the solidification process. However, one limitation of near-eutectic Al-Ce alloys is that they are relatively low in strength compared to other aluminum alloys, but may be made by adding other alloying elements (e.g., mg, cu, mn, ni, etc.).
It has been found that additive manufacturing of aluminum-based alloys with small additions of alloying elements (Zr, sc, er) is capable of forming L1 2 Nano precipitate, primary L1 2 Al 3 The precipitate is precipitated during solidification, so that the crystal grains can be obviously thinned, and the alloy is fully reinforced to prevent cracks. These primary L1 s 2 The precipitates also fix grain boundaries and reduce grain boundary sliding, thereby improving creep resistance at high temperatures. In addition, er, zr, which remains in solid solution after solidification, forms secondary nano-sized Al during subsequent aging 3 The (Er, zr) precipitate can greatly improve the temperature and high temperature strength. However, no additive manufacturing technology has been reported to prepare Er, zr modified and 3D printed Al-Ce-Mg alloys. Therefore, how to prepare Al-Ce-Mg alloy with better heat resistance by adopting an additive manufacturing method is a technical problem to be solved.
Disclosure of Invention
The invention aims to provide a 3D printed Er-Zr modified Al-Ce-Mg heat-resistant alloy and a preparation method thereof.
The aluminum alloy material mainly comprises Ce, mg, er, zr elements, wherein the mass percent of the aluminum alloy material is 8-12%, the content of Ce is 7-10%, the content of Er is 0.3-0.9%, the content of Zr is 0.3-0.5%, and the balance of Al;
the aluminum alloy material further preferably comprises Ce, mg, er, zr elements, wherein the content of Ce is 8-12%, the content of Mg is 7-10%, the content of Er is 0.3-0.5%, the content of Zr is 0.3-0.5%, and the balance is Al;
as a comparative example of the invention, the aluminum alloy material mainly comprises Ce and Mg elements, wherein the content of Ce is 8-12%, the content of Mg is 7-10%, and the balance is Al.
The invention provides an Er, zr modified Al-Ce-Mg heat-resistant alloy and a preparation method thereof, which concretely comprises the following steps:
step one
Placing high-purity Al, mg, al-Ce intermediate alloy, al-Er intermediate alloy and Al-Zr intermediate alloy into a crucible according to a proportion, pre-vacuumizing, smelting in an argon atmosphere at 780 ℃, fully smelting, carrying out gas atomization (vacuum gas atomization) powder preparation under an inert atmosphere (argon) in a temperature range of 780-800 ℃ after fully smelting, carrying out powder sieving after cooling the powder; the high purity refers to purity of not less than 99.96%.
Step two
Drying the powder obtained in the step one in a vacuum drying oven;
step three
Printing the dried powder obtained in the second step by adopting a selective laser melting metal printer, wherein the process parameters are as follows: the laser power (P) is 200-300W, the scanning speed (V) is 600-1000mm/s, the hatch distance (h) is 60-100um, the layer thickness (t) is 20-30um, the preheating temperature is 150 ℃, and the energy density (E) is 100-300J/mm 3 The defocus distance (Δf) was 2.5mm;
step four
The printed alloy obtained in step three was heat treated at 300-350 c (preferably 350 c) and subjected to microhardness testing.
The invention has the following beneficial effects:
zr forms Al by adding Er to Al-Ce-Mg alloy 3 (Er, zr) nano-precipitate, primary Al 3 The (Er, zr) precipitates precipitate during solidification, which can significantly refine the grains, thereby fully strengthening the alloy to prevent cracking. These precipitates also fix grain boundaries and reduce grain boundary sliding, thereby improving thermal stability at high temperatures (e.g., 350 ℃), the degree of decrease in microhardness of the alloy over time is greater, and the thermal stability is higher as the microhardness decreases less. In addition, er, zr, which remains in solid solution after solidification, forms secondary nano-sized Al during subsequent aging 3 The (Er, zr) precipitate can greatly improve the room temperature strength and the high temperature stability.
Drawings
Fig. 1: the microhardness of the aluminum alloys prepared in examples 1,2 and 3 of the present invention is plotted against time.
Fig. 2: the inventive example 1 (right) was crack-free and example 3 (left) was crack-shaped with a golden phase diagram of the sample.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
The aluminum alloy of the embodiment comprises the following elements in percentage by mass: 10% of Ce, 10% of Mg and 10% of Er:0.4%, zr:0.4%, the remainder being Al. Firstly, placing high-purity Al, al-10% Ce intermediate alloy, al-5% Er intermediate alloy and Al-10% Zr intermediate alloy into a crucible according to a proportion, pre-vacuumizing, smelting in an argon atmosphere at 780 ℃, fully smelting, carrying out gas atomization in an argon atmosphere at 780-800 ℃ to obtain powder, wherein the gas pressure is 2MPa, cooling the powder, sieving the powder, and obtaining the powder with the granularity of 15-56 mu m. And secondly, drying the obtained powder in a vacuum drying oven. Third, adopting SLMSoltionM 280 metal printer, technological parameters: laser power (P) 350W, scanning speed (V) 2000mm/s, hatch distance (h) 100um, layer thickness (t) 30um, preheating temperature 150 ℃ and energy density (E) 200J/mm 3 The defocus distance (. DELTA.f) was 2.5mm.
Example 2
The aluminum alloy of the embodiment comprises the following elements in percentage by mass: 10% of Ce, 10% of Mg and 10% of Er:0.8%, zr:0.4%, the remainder being Al. The first step, high purity Al, al-10% Ce intermediate alloy, al-5% Er intermediate alloy and Al-10% Zr intermediate alloy are put into a crucible according to the proportion, and are pre-vacuumized, and then are smelted in argon atmosphere at 780 ℃, after being fully smelted, the temperature range is 780-800 ℃ after being fully smelted,and (3) carrying out gas atomization powder preparation under the argon atmosphere, wherein the gas pressure is 2MPa, and sieving the powder after cooling the powder to obtain the powder with the granularity of 15-58 mu m. And secondly, drying the obtained powder in a vacuum drying oven. Third, adopting SLMSoltionM 280 metal printer, technological parameters: laser power (P) 350W, scanning speed (V) 2000mm/s, hatch distance (h) 100um, layer thickness (t) 30um, preheating temperature 150 ℃ and energy density (E) 200J/mm 3 The defocus distance (. DELTA.f) was 2.5mm.
Example 3 (comparative example)
The aluminum alloy of the embodiment comprises the following elements in percentage by mass: 10% of Ce, 10% of Mg and the balance of Al. Firstly, placing high-purity Al and Al-10% Ce intermediate alloy into a crucible according to a proportion, pre-vacuumizing, smelting in an argon atmosphere at 780 ℃, fully smelting, then carrying out gas atomization powder preparation in an argon atmosphere at 780-800 ℃, wherein the gas pressure is 2MPa, and sieving powder after cooling the powder, thereby obtaining powder with the granularity of 15-58 mu m. And secondly, drying the obtained powder in a vacuum drying oven. Third, adopting SLMSoltionM 280 metal printer, technological parameters: laser power (P) 350W, scanning speed (V) 2000mm/s, hatch distance (h) 100um, layer thickness (t) 30um, preheating temperature 150 ℃ and energy density (E) 200J/mm 3 The defocus distance (. DELTA.f) was 2.5mm.
The Mg element added in the invention mainly plays a solid solution strengthening role. Example 1, example 2 and example 3 (comparative) differ mainly in the addition of different Er, zr. Example 1, example 2, example 3 had substantially consistent initial hardness (about 1600MPa microhardness), indicating that the addition of the elements Er and Zr had no effect on the initial microhardness, because of these primary Al' s 3 (Er, zr) is a submicron precipitate, and no nanoscale secondary strengthening phase Al is formed 3 (Er, zr), and compared with nano-scale Al precipitated during aging precipitation 3 (Er, zr) is much coarser, so the strengthening effect on the alloy is not significant enough. However, as the aging time is prolonged, significant differences in the thermal stability of the alloy occur. First, the alloy of example 3 (comparative) has a hardness that is constant over timeSlowly and continuously decreasing (linear trend over a period of 2-80 h) due to coarsening of the Ce-rich intermetallic compound, and no precipitated phase capable of suppressing such coarsening. Whereas examples 1 and 2 of the present invention showed a significant increase in microhardness at 2h due to the precipitation of Al in the alloy 3 The (Er, zr) phase has a significant solid solution strengthening, and after 2-20h, the microhardness slowly decreases with time and reaches 20h, the hardness reaches the lowest point (at this time the hardness of example 1 is still about 50MPa higher than that of example 3), then starts to slowly rise, and after 80h the aging end time still shows a rising trend, at this time the microhardness of example 1 is 1630MPa, about 150MPa higher than that of example 3, because the alloy generates nano-scale Al during aging 3 When the (Er, zr) strengthening phase is aged for 20 hours, a large amount of these precipitated phases start to precipitate, thereby playing a role in precipitation strengthening, and the grain boundary can be fixed to inhibit coarsening of crystal grains, so that the thermal stability is improved. Example 2 added more Er than example 1, the microhardness was substantially between example 1 and example 3 because more Er was added to make primary coarse Al 3 The increasing amount of (Er, zr) precipitates and the improving effect is reduced, so that the local concentration of Er, zr is sufficiently low to make Al be primary 3 The content of (Er, zr) is reduced, so that more Er, zr is dissolved in the matrix in the solidification process, and more nano-scale Al is precipitated in the aging process 3 The (Er, zr) reinforced phase can better improve the strength and the thermal stability of the Al-Ce-Mg alloy.

Claims (5)

1. The preparation method of the Al-Ce-Mg aluminum alloy for metal 3D printing is characterized in that the aluminum alloy mainly comprises Ce, mg, er, zr elements, wherein the content of Ce is 8-12%, the content of Mg is 7-10%, the content of Er is 0.3-0.9%, the content of Zr is 0.3-0.5%, and the balance is Al;
the preparation method comprises the following steps:
step one
The high-purity Al-Mg-Ce intermediate alloy, al-Er intermediate alloy and Al-Zr intermediate alloy: placing the materials into a crucible according to the proportion, pre-vacuumizing, smelting in an argon atmosphere at 780 ℃, fully melting, then carrying out gas atomization powder preparation in an inert atmosphere at 780-800 ℃ after fully melting, wherein the gas pressure is 2MPa, and sieving the powder after cooling;
step two
Drying the powder obtained in the step one in a vacuum drying oven;
step three
Printing the dried powder obtained in the second step by adopting a selective laser melting metal printer, wherein the process parameters are as follows: the laser power (P) is 200-300W, the scanning speed (V) is 600-1000mm/s, the hatch distance (h) is 60-100um, the layer thickness (t) is 20-30um, the preheating temperature is 150 ℃, and the energy density (E) is 100-300J/mm 3 The defocus distance (Δf) was 2.5mm;
step four
The printed alloy obtained in step three was heat treated at 300-350 c (preferably 350 c) and subjected to microhardness testing.
2. The method according to claim 1, wherein the aluminum alloy mainly contains Ce, mg, er, zr elements, wherein the content of Ce is 8-12%, the content of Mg is 7-10%, the content of Er is 0.3-0.5%, the content of Zr is 0.3-0.5%, and the balance of Al.
3. The method of claim 1, wherein the inert atmosphere is argon; the gas atomization is vacuum air atomization.
4. An aluminum alloy prepared according to the method of any one of claims 1-3.
5. An aluminum alloy produced by the method of any of claims 1-3 having a minimum microhardness of 1630MPa.
CN202311577270.4A 2023-11-23 2023-11-23 Al-Ce-Mg aluminum alloy for metal 3D printing and preparation method thereof Pending CN117532012A (en)

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