CN111471905B - Al-Zn-Mg-Sc aluminum alloy wire for 3D printing and preparation method thereof - Google Patents
Al-Zn-Mg-Sc aluminum alloy wire for 3D printing and preparation method thereof Download PDFInfo
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- 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
- C22C21/10—Alloys based on aluminium with zinc as the next major constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
- B21C37/047—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire of fine wires
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- 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
- C22F1/053—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 zinc as the next major constituent
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Abstract
The invention discloses a preparation method of an Al-Zn-Mg-Sc series aluminum alloy wire for 3D printing, which comprises the steps of batching, vacuum melting, casting, homogenizing, post-treatment of the surface of an ingot and wire drawing, and also discloses an aluminum alloy wire prepared by the method, wherein a workpiece is 3D printed by utilizing the aluminum alloy wire, and the workpiece has the tensile strength of 470-520MPa, the yield strength of 370-410MPa and the elongation of 9-12%. The metal 3D printing aluminum alloy wire meeting the printing requirement of high-strength parts, prepared by the method, has uniform chemical components, and the grain size is basically distributed in the range of 40-60 mu m.
Description
Technical Field
The invention relates to the field of 3D printing metal materials, in particular to an Al-Zn-Mg-Sc aluminum alloy wire for 3D printing and a preparation method thereof, which are suitable for printing workpieces with high strength requirements in the aerospace field.
Background
3D printing is an advanced digital manufacturing technologyThe technology is a technology for constructing an object by using filiform and powdery metal in a layer-by-layer printing mode on the basis of a digital model file. At present, the aluminum alloy printing material at home and abroad mainly takes powder as a main component and mainly comprises AlSi7Mg and AlSi10Mg two, with low printed article strength (σ)bLess than 350MPa), small size of finished products and the like.
With the development of printing technology, especially Electron Beam Melting (EBM) and electric arc additive process (WAAM), 3D printing technology based on metal wire is more and more widely used. The metal wire is produced by vacuum melting, ingot casting and wire drawing, so that the risk of oxidation of the powder printing material in the preparation process is effectively avoided. In addition, compared with a powder printing process, the wire printing efficiency is higher, the size of a printing part is larger, and the printing equipment is cheaper. 3D printing of metal wire opens up new thinking and direction for the opening of the times of high efficiency, large size and low cost of 3D printing.
Because the 3D printing research of the metal wire is still in the process of exploration and verification, no metal material specially used for the EBM and WAAM processes exists in the market at present; due to the difficulty of the Al-Zn-Mg series aluminum alloy wire preparation process and the particularity in the printing process, the development and verification of the Al-Zn-Mg series aluminum alloy wire-based 3D printing material preparation technology and the printing process are disclosed by few related reports all the time.
In a preparation method (publication number: CN110273076A) of an aluminum alloy wire for metal 3D printing, the preparation method comprises the following steps: alloy batching → press forming → vacuum induction furnace smelting → alloy casting → forging → rotary swaging → wire drawing → continuous electrolytic cleaning → heat treatment and straightening. The aluminum alloy wire prepared by the method provided by the invention has the advantages that the surface quality is obviously improved, the wire feeding speed is stable and the smoothness is good in the wire feeding 3D printing process, but the strength is not enough, and the aluminum alloy wire is not suitable for printing workpieces with high strength requirements in the aerospace field.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the problems in the prior art are solved, the Al-Zn-Mg-Sc aluminum alloy wire for 3D printing and the preparation method thereof are provided, and the prepared aluminum alloy wire is suitable for printing workpieces with high strength requirements in the aerospace field.
The technical scheme adopted by the invention is as follows:
a preparation method of an Al-Zn-Mg-Sc aluminum alloy wire for 3D printing comprises the following steps:
(1) preparing materials: weighing metal raw materials and proportioning, wherein the metal raw materials comprise the following chemical elements in percentage by weight: 6.5 to 7.5 percent of Zn, 2.5 to 3 percent of Mg, 0.3 to 0.8 percent of Mn, 0.05 to 0.25 percent of Zr, 0.3 to 0.8 percent of Cu, 0.1 to 0.5 percent of Sc, 0.03 to 0.06 percent of Ti, less than or equal to 0.3 percent of impurity and the balance of Al;
(2) vacuum smelting: vacuum melting is carried out on the metal raw material obtained by burdening, the vacuum degree is more than 0Pa and less than 5Pa, and the melting temperature is 720-800 ℃, so as to obtain a melted raw material;
(3) casting: standing the melted raw materials, and casting the melted raw materials into a water-cooled mold at the casting temperature of 720 ℃ and 740 ℃ to obtain a cast ingot;
(4) homogenizing: placing the ingot into an annealing furnace for homogenization treatment, heating to 350-400 ℃, preserving heat, discharging and cooling to obtain a homogenized ingot;
(5) post-treatment of the surface of the cast ingot: turning the surface of the ingot after the homogenization treatment to ensure that the surface roughness of the ingot is less than Ra3.2 to obtain the ingot after the surface treatment;
(6) wire drawing treatment: extruding the cast ingot after surface treatment into an extrusion rod with the thickness of 8-11mm by an extruder at the extrusion speed of 8-12mm/s, rolling into a wire with the thickness of 3-5mm by 5-7 rolling processes, preparing the wire with the thickness of 1-1.4mm by a scraping and drawing process, and finally obtaining the Al-Zn-Mg-Sc aluminum alloy finished wire by an ultrasonic cleaning-fine disc process. .
According to the invention, after the metal raw material is subjected to vacuum melting, the metal raw material is subjected to rapid water-cooling casting, and is subjected to homogenization treatment and cast ingot surface post-treatment and wire drawing, so that the prepared aluminum alloy wire has uniform chemical components, can effectively refine crystal grains, and is suitable for printing high-strength parts.
The vacuum smelting can avoid the oxidation and slag inclusion of the raw materials, the rapid cooling and forming of the high-temperature melt can effectively refine grains, and the plasticity of the material is improved.
The homogenization treatment can ensure that the unbalanced eutectic structure in the cast ingot is distributed in the matrix to be uniform, and supersaturated solid solution elements are precipitated from the solid solution, so as to achieve the purposes of eliminating casting stress, improving the plasticity of the cast ingot and improving the structure and the performance of a processed product.
Further, the cooling rate in the water-cooled mold in the step (3) is 80-100K/s.
Further, the metal raw materials in the step (1) comprise pure aluminum, pure zinc, pure magnesium, aluminum copper alloy, aluminum scandium alloy, aluminum zirconium alloy, aluminum manganese alloy and aluminum titanium alloy;
in the step (1), the metal raw materials comprise impurities Fe and Si, wherein Fe is less than or equal to 0.2 percent, and Si is less than or equal to 0.1 percent;
and (2) sequentially adding pure aluminum, pure zinc, pure magnesium, an aluminum-copper alloy, an aluminum-scandium alloy, an aluminum-zirconium alloy, an aluminum-manganese alloy and an aluminum-titanium alloy into a vacuum smelting furnace.
Further, the standing time in the step (3) is 10-20 min.
Further, the heat preservation time in the step (4) is 10-12 hours.
Further, the size of the water-cooling mold in the step (3) is (110-.
Further, the step (5) also comprises the step of cutting off two ends of the ingot after the homogenization treatment.
The invention also relates to an Al-Zn-Mg-Sc aluminum alloy wire for 3D metal printing, which is prepared by the method, and a product is 3D printed by using the aluminum alloy wire, wherein the product has the tensile strength of 470-520MPa, the yield strength of 370-410MPa and the elongation of 9-12%.
Further, the diameter of the aluminum alloy wire is 1.0-2.0 mm.
The invention comprises the following key innovation points:
1. the guarantee that the extrusion process in the wire drawing production process is smoothly carried out benefits from the following three points: 1) the vacuum melting casting die is a water-cooled die, the cooling rate reaches 100K/s, the ingot casting crystallization speed is high, the segregation degree of the supersaturated solid solution is reduced, the chemical components are more uniform, meanwhile, the high-temperature melt is rapidly cooled and formed, the crystal grains can be effectively refined, the size of the crystal grains is basically distributed in the range of 40-60 mu m, the plasticity of the material is improved, and the smooth implementation of subsequent processes such as extrusion, wire drawing and the like is facilitated; 2) the homogenization treatment makes the unbalanced eutectic structure in the cast ingot distributed homogeneously in the matrix and the supersaturated solid solution element separated out from the solid solution to eliminate casting stress, raise the plasticity of the cast ingot and improve the structure and performance of the product. The steps (1) to (5) are the basic and key steps for realizing normal wire drawing treatment in the step (6). 3) In addition, the cleaning process ensures that the produced Al-Zn-Mg-Sc aluminum alloy material meets the surface quality requirement of the 3D printing wire.
2. Sc and Zr are added in the alloy in a compounding way, so that the strength of the Al-Zn-Mg alloy can be effectively improved, and the reasons are as follows: the added Sc and Zr form coherent second phase particles with a matrix, and the second phase particles are subjected to strong nail-rolling dislocation and the crystal boundary of the matrix, so that the movement of the dislocation and the migration of the crystal boundary are hindered, and the recrystallization process of crystal grains is inhibited; secondly, the added Sc and Zr can generate large component supercooling degree after being enriched in a liquid phase at the front edge of a solidification interface of the cast ingot, so that a large amount of fine isometric crystals are nucleated; in addition, part of atoms are enriched at the root of a columnar dendritic crystal crystallized first, so that the dendritic crystal is contracted and developed into a free crystal, and finally a new nucleation core of an isometric crystal is formed to refine the crystal grains.
Zn, Mg: simultaneously adding into aluminum to form a strengthening phase MgZn2The MgZn has obvious strengthening effect on the alloy2The tensile strength and the yield strength can be obviously increased by increasing the content;
mn: can prevent the recrystallization process of the aluminum alloy, improve the crystallization temperature and obviously refine the recrystallized grains. MnAl6The compound dispersoid plays a role in inhibiting the growth of recrystallized grains.
CuAl with Cu-Al alloy structure having certain solid solution strengthening effect and being separated out by aging2Has obvious aging strengthening effect.
6. The invention realizes the 3D printing of the Al-Zn-Mg aluminum alloy wire and provides a high-efficiency and low-cost printing realization scheme of large-size parts.
The invention has the following beneficial effects:
1. sc and Zr elements are introduced into the Al-Zn-Mg series aluminum alloy. Sc and Zr have obvious recrystallization inhibition effect on alloy, and form coherent dispersoid Al through synergistic strengthening effect3(ScZr) and strengthening effect caused by grain refinement, and the thermal stability of the alloy is improved. After printing, through certain post-treatment, the tensile strength of the printed part reaches more than 470MPa, the yield strength is more than 370MPa, and the tensile strength, the yield strength and the elongation of the printed part are superior to those of the existing common AlSi7Mg and AlSi10Mg。
2. And adjusting the content ratio of Sc to Zr. The method has the best effect on solving the problems of grain refinement, secondary dendrite spacing reduction, recrystallization inhibition and the like.
3. The material provided by the invention can be used for printing large-size parts, the application range of 3D printing technology is enlarged, and the market of 3D printing is developed.
Drawings
FIG. 1 is a 200X metallographic photograph of the surface of an ingot after water-cooling treatment in example 1;
FIG. 2 is a 200X metallographic photograph of the ingot after the homogenization treatment in example 1;
FIG. 3 is a photograph of the ingot after surface treatment in example 1;
FIG. 4 is an SEM 200X photograph of the core structure of the aluminum alloy wire obtained in example 1;
FIG. 5 is a 200X metallographic photograph of the surface of the aluminum alloy wire obtained in example 1;
FIG. 6 is a 200X metallographic photograph of the surface of the aluminum alloy wire obtained in example 1;
FIG. 7 is a 200X metallographic photograph of a print obtained by using the domestic printer 1 for an aluminum alloy wire obtained in example 1;
FIG. 8 is a 200X metallographic photograph of a print made from the aluminum alloy wire obtained in example 1 using a domestic printer 2;
FIG. 9 is a 200X metallographic photograph of a print of the aluminum alloy wire obtained in example 1 obtained by using a foreign printer 1.
Detailed description of the preferred embodiments
In order to better understand the technical solution, the technical solution will be described in detail with reference to the drawings and the specific embodiments.
Examples
Pure aluminum, pure zinc, pure magnesium, aluminum copper alloy, aluminum scandium alloy, aluminum zirconium alloy, aluminum manganese alloy and aluminum titanium alloy were weighed, and table 1 shows the chemical element content in each metal material in examples 1 to 4.
TABLE 1 formulation of the metal raw materials in examples 1-4 (after burning)
The production process of the aluminum alloy wire comprises the following steps:
(1) preparing materials: weighing metal raw materials and proportioning so as to enable the metal raw materials to meet the chemical elements and contents in the table 1;
(2) vacuum smelting: adding the metal raw material obtained by burdening into a crucible in a vacuum melting furnace, vacuumizing at the vacuum degree of 3Pa and the melting temperature of 760 ℃ after adding, and obtaining a molten raw material;
(3) casting: standing the melted raw materials for 15min, casting into a water-cooling mold with phi 120mm x 400mm, and rapidly cooling for molding, wherein the cooling rate of the water-cooling mold can reach 100K/s. The casting temperature was 740 ℃ to obtain an ingot.
Metallographic analysis is carried out on the cast ingot after water cooling treatment, an obtained photo is shown in figure 1, the grain size is basically distributed at 40-60 mu m, and raw material oxidation and slag inclusion can be avoided by adopting vacuum melting; the high-temperature melt is rapidly cooled and formed, so that crystal grains can be effectively refined, and the plasticity of the material is improved.
(4) Homogenizing: placing the ingot into an annealing furnace for homogenization treatment, heating to 380 ℃, preserving heat, discharging and cooling to obtain a homogenized ingot; the incubation time was 12 hours.
Metallographic analysis was performed on the ingot after the homogenization treatment, and the obtained photograph was as shown in fig. 2, in which the chemical components in the ingot were uniform. The homogenization treatment can ensure that the unbalanced eutectic structure in the cast ingot is distributed in the matrix to be uniform, and supersaturated solid solution elements are precipitated from the solid solution, so as to achieve the purposes of eliminating casting stress, improving the plasticity of the cast ingot and improving the structure and the performance of a processed product.
(5) Post-treatment of the surface of the cast ingot: and cutting off the bottom of the cap opening of the ingot, turning the ingot from phi 120 mm/400 mm to phi 116 mm/400 mm by using a lathe, and simultaneously ensuring that the surface roughness of the ingot is superior to Ra3.2 to obtain a photo of the ingot after surface post-treatment, wherein the surface of the ingot is smooth and flat as shown in figure 3.
(6) Wire drawing treatment: extruding the cast ingot after surface treatment into an extrusion rod with the diameter of 10mm by an extruder at the extrusion speed of 10mm/s, rolling into a wire with the diameter of 4mm by 6 rolling procedures, preparing the wire with the diameter of 1.2mm by a scraping and drawing procedure, and finally obtaining the Al-Zn-Mg-Sc aluminum alloy finished wire with the diameter of 1.2mm by ultrasonic cleaning and fine coiling procedures. The prepared wire is subjected to electron microscope detection and metallographic analysis respectively, wherein the picture 4 is a SEM 200X picture of the core structure of the wire, the picture 5 is a 200X metallographic picture of the surface of the wire, and the picture 6 is a 200X metallographic picture of the surface of the wire.
The wire prepared in the embodiment 1 is respectively printed into a printed part by using 3D printing equipment at home and abroad (two foreign countries and one domestic), the printed part is respectively subjected to metallographic analysis and mechanical property test according to the GB/T228-. The properties of the printed parts are shown in Table 2, wherein the tensile strength is 475-511MPa, the yield strength is 380-405MPa, and the elongation is 9-12%.
TABLE 2 mechanical property test results of domestic 1 and foreign 1-2 prints
The wire materials prepared in examples 1 to 4 were subjected to sample printing using a laser fuse 3D printing apparatus, and processed into test pieces after heat treatment. The mechanical property test of the printed part is carried out according to the GB/T228-.
TABLE 3 mechanical Property test results of printed Material
According to the data table 3, better Al-Zn-Mg-Sc aluminum alloy wire is obtained by adjusting Zn and Mg and adding certain amounts of Zr and Sc elements, parts printed by using the Al-Zn-Mg-Sc aluminum alloy wire have more excellent mechanical properties, and the Al-Zn-Mg-Sc aluminum alloy wire disclosed by the invention is more suitable for 3D printing of the wire.
Claims (8)
1. A preparation method of an Al-Zn-Mg-Sc aluminum alloy wire for 3D printing is characterized by comprising the following steps: (1) preparing materials: weighing metal raw materials and proportioning, wherein the metal raw materials comprise the following chemical elements in percentage by weight: 6.5-7.5% of Zn, 2.5-3% of Mg, 0.3-0.8% of Mn, 0.05-0.25% of Zr, 0.3-0.8% of Cu, 0.1-0.5% of Sc, 0.03-0.06% of Ti, less than or equal to 0.3% of impurities and the balance of Al; (2) vacuum smelting: vacuum melting is carried out on the metal raw material obtained by burdening, the vacuum degree is more than 0Pa and less than 5Pa, and the melting temperature is 720-800 ℃, so as to obtain a melted raw material; (3) casting: standing the melted raw materials, and casting the melted raw materials into a water-cooled mold at the casting temperature of 720 ℃ and 740 ℃ to obtain a cast ingot; (4) homogenizing: placing the ingot into an annealing furnace for homogenization treatment, heating to 350-400 ℃, preserving heat, discharging and cooling to obtain a homogenized ingot; (5) post-treatment of the surface of the cast ingot: turning the surface of the ingot after the homogenization treatment to ensure that the surface roughness of the ingot is less than Ra3.2 to obtain the ingot after the surface treatment; (6) wire drawing treatment: extruding the cast ingot after surface treatment into an extrusion rod with the thickness of 8-12mm by an extruder at the extrusion speed of 8-12mm/s, rolling into a wire with the thickness of 3-5mm by 5-7 rolling processes, preparing the wire with the thickness of 1-1.4mm by a scraping and drawing process, and finally obtaining the Al-Zn-Mg-Sc aluminum alloy finished wire by an ultrasonic cleaning-fine disc process;
the metal raw materials in the step (1) comprise pure aluminum, pure zinc, pure magnesium, aluminum-copper alloy, aluminum-scandium alloy, aluminum-zirconium alloy, aluminum-manganese alloy and aluminum-titanium alloy;
and (4) the cooling rate in the water-cooling mould in the step (3) is 80-100K/s.
2. The method of claim 1, wherein: in the step (1), the metal raw materials comprise impurities Fe and Si, wherein Fe is less than or equal to 0.2 percent, and Si is less than or equal to 0.1 percent; and (2) sequentially adding pure aluminum, pure zinc, pure magnesium, an aluminum-copper alloy, an aluminum-scandium alloy, an aluminum-zirconium alloy, an aluminum-manganese alloy and an aluminum-titanium alloy into a vacuum smelting furnace for vacuum smelting.
3. The method of claim 1, wherein: and (4) standing for 10-20min in the step (3).
4. The method of claim 1, wherein: the heat preservation time in the step (4) is 10-12 hours.
5. The production method according to any one of claims 1 to 4, characterized in that: the size of the water-cooling mould in the step (3) is (110-.
6. The production method according to any one of claims 1 to 4, characterized in that: and (5) cutting off two ends of the ingot after the homogenization treatment.
7. An Al-Zn-Mg-Sc series aluminum alloy wire for 3D metal printing is characterized by being prepared by the method of any one of claims 1 to 6, and the aluminum alloy wire is used for 3D metal printing of a product, wherein the tensile strength of the product is 470-520MPa, the yield strength of the product is 370-410MPa, and the elongation of the product is 9-12%.
8. The wire of claim 7, wherein: the diameter of the aluminum alloy wire is 1.0-2.0 mm.
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| CN113862534B (en) * | 2021-10-08 | 2022-07-29 | 上海交通大学 | Method for regulating and controlling tissue inheritance of aluminum alloy material and method for preparing 7085 aluminum alloy thick plate |
| CN114540675A (en) * | 2022-01-20 | 2022-05-27 | 山东南山铝业股份有限公司 | High-performance wrought aluminum alloy and manufacturing method thereof |
| CN116144993A (en) * | 2022-10-31 | 2023-05-23 | 沈阳航空航天大学 | 7-series aluminum alloy wire for arc additive manufacturing and preparation method and application thereof |
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| CA3059286A1 (en) * | 2017-04-05 | 2018-10-11 | Amag Casting Gmbh | Starting material, use thereof, and additive manufacturing process using said starting material |
| CN109266926A (en) * | 2018-11-19 | 2019-01-25 | 首都航天机械有限公司 | A kind of made of Al-Cu alloy silk and its preparation method and application |
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