CN111155015B - High-plasticity light alloy for three-dimensional printing and preparation method thereof - Google Patents

High-plasticity light alloy for three-dimensional printing and preparation method thereof Download PDF

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CN111155015B
CN111155015B CN202010083201.8A CN202010083201A CN111155015B CN 111155015 B CN111155015 B CN 111155015B CN 202010083201 A CN202010083201 A CN 202010083201A CN 111155015 B CN111155015 B CN 111155015B
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alloy
printing
intermediate alloy
powder
dimensional printing
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CN111155015A (en
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刘文才
李俊锋
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Suzhou Qingjin 3d Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/06Alloys based on magnesium with a rare earth metal 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • 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
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/04Alloys based on magnesium with zinc or cadmium as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon

Abstract

The invention discloses a high-plasticity light alloy for three-dimensional printing and a preparation method thereof, wherein the alloy comprises the following components in percentage by mass: 1-8 wt.% Zn, 1-7 wt.% Er, 0.2-5 wt.% Nd, 0.2-2 wt.% Mn, 0.1-1 wt.% Zr, and the balance Mg and unavoidable impurities. The preparation method comprises the following steps: the raw materials are made into spherical powder after composition design, metal powder is fully mixed, the mixed raw material powder is sintered and subjected to solution heat treatment, and then light alloy spherical powder is obtained through mechanical grinding and alloying. The finished product of the obtained material after three-dimensional printing has the advantages of high plasticity, light weight, good heat resistance and wear resistance on the premise of keeping higher strength.

Description

High-plasticity light alloy for three-dimensional printing and preparation method thereof
Technical Field
The invention belongs to the technical field of 3D printing materials, and particularly relates to a high-plasticity light alloy for three-dimensional printing and a preparation method thereof.
Background
The 3D printing technology is called additive manufacturing according to the manufacturing process, belongs to one of rapid prototyping technologies, and is characterized in that a product is finally directly printed by using a bondable material such as powdered metal or plastic in a multi-layer printing mode one layer by one layer to form digital manufacturing. The 3D printing technology originated from the photographic sculpture and the topographic formation technology studied in the united states at the end of the 19 th century, but was limited by the technological conditions at that time and had not made a breakthrough progress. In the last 80 th century, with the vigorous development of computer technology and new material technology, 3D printing technology has advanced a long time, but its commercialization and marketization process is slow. In the 21 st century, 3D printing technology has been rapidly developed, and its application fields are gradually extended from mold manufacturing, industrial design, and the like to aerospace, automobiles, medical treatment, and the like.
The magnesium alloy has a series of unique advantages of high specific strength and specific stiffness, good damping vibration attenuation, strong electromagnetic shielding and heat conducting properties, pressure resistance, good heat dissipation, easiness in casting and forming, easiness in cutting and processing, easiness in recycling and the like, and has great application potential in structural part industries of aerospace, automobiles, computers, communication, consumer electronics and the like. The magnesium alloy and the 3D printing technology are combined to serve the metal manufacturing industry, and the manufacturing industry can be promoted to develop towards low cost, short period and high efficiency. 3D printing metal powder generally requires high purity, good sphericity, narrow particle size distribution and low oxygen content. The metal raw materials for 3D printing are special, and must be capable of being liquefied and powdered, and simultaneously re-bonded in the printing process, and have physical and chemical properties meeting requirements.
However, the metal powder for 3D printing at present mainly includes titanium alloy, cobalt-chromium alloy, stainless steel, aluminum alloy material, and the like, and magnesium alloy is difficult to prepare due to its chemical activity and flammability, is still in the experimental stage, and is not widely applied to the field of 3D printing. The conventional method for three-dimensional printing of magnesium alloy comprises the steps of firstly preparing the magnesium alloy by smelting, then ball-milling the magnesium alloy into powder, and then carrying out three-dimensional printing. The whole preparation process has long working procedures, high energy consumption, easy increase of impurities and low material utilization rate.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention aims to provide a high-plasticity light alloy for three-dimensional printing and a preparation method thereof. In a first aspect, the Mg-Zn-Er-Nd-Mn-Zr magnesium alloy material provided by the invention comprises the following elements in percentage by weight: 1-8 wt.% Zn, 1-7 wt.% Er, 0.2-5 wt.% Nd, 0.2-2 wt.% Mn, 0.1-1 wt.% Zr, and the balance Mg and unavoidable impurities.
In a second aspect, the invention provides a preparation method of a high-plasticity light alloy for three-dimensional printing, wherein the Mg-Zn-Er-Nd-Mn-Zr magnesium alloy is prepared by combining raw materials (pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy and Mg-Zr intermediate alloy) with a traditional smelting process, and sequentially comprises the following steps:
(1) the raw materials of pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy and Mg-Zr intermediate alloy are prepared into spherical powder by a mechanical grinding process, the particle size is 30-140 mu m, and the oxygen content is 0.06-0.18.
(2) Weighing various raw material powders according to the specific contents of the elements of the Mg-Zn-Er-Nd-Mn-Zr magnesium alloy, and fully mixing the metal powders for 20-80 minutes.
(3) And sintering the mixed metal powder into a precast block and carrying out solution heat treatment, wherein the solution temperature is 350-570 ℃, and the solution time is 4-30 hours.
(4) The alloy prefabricated block is made into spherical powder by a mechanical grinding process, the particle size is 30-140 mu m, and the oxygen content is 0.06-0.18.
In a third aspect, the present invention provides a three-dimensionally printed part, which is made by three-dimensionally printing the Mg-Zn-Er-Nd-Mn-Zr magnesium alloy described in the first aspect or the Mg-Zn-Er-Nd-Mn-Zr magnesium alloy prepared by the method described in the first aspect.
The invention has the advantages and beneficial effects that:
(1) by applying the Mg-Zn-Er-Nd-Mn-Zr magnesium alloy powder material provided by the invention, the obtained parts have the advantages of high plasticity, good heat resistance and wear resistance on the premise of keeping higher strength.
(2) The Mg-Zn-Er-Nd-Mn-Zr magnesium alloy designed by the invention has excellent plasticity and heat resistance, the use temperature is increased to more than 300 ℃, the grain diameter is normally distributed, the structure crystal grains are fine, the Mg-Zn-Er-Nd-Mn-Zr magnesium alloy is free from contact with air in the preparation process, the oxygen content is low, the problems of easiness in smelting to prepare magnesium alloy ingots and easiness in preparing magnesium alloy powder by a subsequent atomization method are solved, and the Mg-Zn-Er-Nd-Mn-Zr magnesium alloy can be used for 3D printing related products.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment relates to a high-plasticity Mg-Zn-Er-Nd-Mn-Zr magnesium alloy material which comprises the following components in percentage by weight: 1wt.% Zn, 7wt.% Er, 0.2wt.% Nd, 2wt.% Mn, 0.1wt.% Zr, the balance Mg and unavoidable impurities. The Mg-1Zn-7Er-0.2Nd-2Mn-0.1Zr magnesium alloy is not prepared by combining raw materials (pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy and Mg-Zr intermediate alloy) with a traditional smelting process, but is sequentially prepared according to the following steps:
(1) the raw materials of pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy and Mg-Zr intermediate alloy are prepared into spherical powder by a mechanical grinding process, the particle size is 30-140 mu m, and the oxygen content is 0.06-0.18.
(2) Weighing various raw material powders according to the specific contents of the elements of the Mg-1Zn-7Er-0.2Nd-2Mn-0.1Zr magnesium alloy, and putting the powders into a powder mixer to be mixed for 20 minutes until the powders are uniformly mixed.
(3) And sintering the mixed metal powder into a precast block, and carrying out solid solution heat treatment at the solid solution temperature of 350 ℃ for 30 hours.
(4) The alloy prefabricated block is made into spherical powder by a mechanical grinding process, the particle size is 30-140 mu m, and the oxygen content is 0.06-0.18. Mechanical grinding alloying is a complex physical and chemical process which makes powder undergo repeated deformation, cold welding and crushing by high-energy ball milling so as to achieve the alloying of atoms between elements at the level.
(5) 3D printing is carried out by using the obtained finished product powder, and the printing parameters are as follows: building rate: 25cm3H, laser scanning speed: 12m/s, layer thickness: and 30 μm.
The high-plasticity Mg-1Zn-7Er-0.2Nd-2Mn-0.1Zr magnesium alloy material prepared by the method has the density of 1.82g/cm3The relative abrasion resistance ε was 10.8.
Room temperature mechanical properties: the yield strength is 225MPa, the tensile strength is 320MPa, and the elongation is 9%.
Mechanical properties at 300 ℃: the yield strength is 180MPa, the tensile strength is 235MPa, and the elongation is 35 percent.
Example 2
The embodiment relates to a high-plasticity Mg-Zn-Er-Nd-Mn-Zr magnesium alloy material which comprises the following components in percentage by weight: 8wt.% Zn, 1wt.% Er, 5wt.% Nd, 0.2wt.% Mn, 1wt.% Zr, the balance Mg and unavoidable impurities. The Mg-8Zn-1Er-5Nd-0.2Mn-1Zr magnesium alloy is not prepared by combining raw materials (pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy and Mg-Zr intermediate alloy) with a traditional smelting process, but is sequentially prepared according to the following steps:
(1) the raw materials of pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy and Mg-Zr intermediate alloy are prepared into spherical powder by a mechanical grinding process, the particle size is 30-140 mu m, and the oxygen content is 0.06-0.18.
(2) Weighing various raw material powders according to the specific contents of the elements of the Mg-8Zn-1Er-5Nd-0.2Mn-1Zr magnesium alloy, and putting the powders into a powder mixer to be mixed for 80 minutes until the powders are uniformly mixed.
(3) Sintering the mixed metal powder into a precast block and carrying out solid solution heat treatment, wherein the solid solution temperature is 570 ℃, and the solid solution time is 4 hours.
(4) The alloy prefabricated block is made into spherical powder by a mechanical grinding process, the particle size is 30-140 mu m, and the oxygen content is 0.06-0.18. Mechanical grinding alloying is a complex physical and chemical process which makes powder undergo repeated deformation, cold welding and crushing by high-energy ball milling so as to achieve the alloying of atoms between elements at the level.
(5) 3D printing is carried out by using the obtained finished product powder, and the printing parameters are as follows: building rate: 25cm3H, laser scanning speed: 12m/s, layer thickness: and 30 μm.
The high-plasticity Mg-8Zn-1Er-5Nd-0.2Mn-1Zr magnesium alloy material prepared by the method has the density of 1.91g/cm3The relative abrasion resistance ε was 11.7.
Room temperature mechanical properties: the yield strength is 238MPa, the tensile strength is 345MPa, and the elongation is 8 percent.
Mechanical properties at 300 ℃: the yield strength is 200MPa, the tensile strength is 265MPa, and the elongation is 30%.
Example 3
The embodiment relates to a high-plasticity Mg-Zn-Er-Nd-Mn-Zr magnesium alloy material which comprises the following components in percentage by weight: 4.5wt.% Zn, 4wt.% Er, 2.5wt.% Nd, 1wt.% Mn, 0.5wt.% Zr, the balance Mg and unavoidable impurities. The Mg-4.5Zn-4Er-2.5Nd-1Mn-0.5Zr magnesium alloy is not prepared by combining raw materials (pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy and Mg-Zr intermediate alloy) with a traditional smelting process, but is sequentially prepared according to the following steps:
(1) the raw materials of pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy and Mg-Zr intermediate alloy are prepared into spherical powder by a mechanical grinding process, the particle size is 30-140 mu m, and the oxygen content is 0.06-0.18.
(2) Weighing various raw material powders according to the specific contents of the elements of the Mg-4.5Zn-4Er-2.5Nd-1Mn-0.5Zr magnesium alloy, and putting the powders into a powder mixer to be mixed for 50 minutes until the powders are uniformly mixed.
(3) And sintering the mixed metal powder into a precast block, and carrying out solid solution heat treatment at the solid solution temperature of 500 ℃ for 16 hours.
(4) The alloy prefabricated block is made into spherical powder by a mechanical grinding process, the particle size is 30-140 mu m, and the oxygen content is 0.06-0.18. Mechanical grinding alloying is a complex physical and chemical process which makes powder undergo repeated deformation, cold welding and crushing by high-energy ball milling so as to achieve the alloying of atoms between elements at the level.
(5) 3D printing is carried out by using the obtained finished product powder, and the printing parameters are as follows: building rate: 25cm3H, laser scanning speed: 12m/s, layer thickness: and 30 μm.
The high-plasticity Mg-4.5Zn-4Er-2.5Nd-1Mn-0.5Zr magnesium alloy material prepared by the method has the density of 1.89g/cm3The relative abrasion resistance ε was 12.9.
Room temperature mechanical properties: the yield strength is 256MPa, the tensile strength is 360MPa, and the elongation is 10%.
Mechanical properties at 300 ℃: the yield strength is 208MPa, the tensile strength is 285MPa, and the elongation is 37 percent.
Comparative example 1
The comparative example is the comparative example of example 1, and provides a Mg-1Zn-7Er-0.2Nd-2Mn-0.1Zr magnesium alloy material, and is different from the magnesium alloy material involved in example 1 in that the Mg-1Zn-7Er-0.2Nd-2Mn-0.1Zr magnesium alloy is prepared by combining raw materials (pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy and Mg-Zr intermediate alloy) with a traditional smelting process.
The density of the magnesium alloy material is 1.83g/cm3The relative abrasion resistance ε was 9.9.
Room temperature mechanical properties: the yield strength is 211MPa, the tensile strength is 302MPa, and the elongation is 7%.
Mechanical properties at 300 ℃: the yield strength is 170MPa, the tensile strength is 222MPa, and the elongation is 28%.
Comparative example 2
The comparative example is the comparative example of example 2, and provides a Mg-8Zn-1Er-5Nd-0.2Mn-1Zr magnesium alloy material, and is different from the magnesium alloy material involved in example 2 in that the Mg-8Zn-1Er-5Nd-0.2Mn-1Zr magnesium alloy is prepared by combining raw materials (pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy and Mg-Zr intermediate alloy) with a traditional smelting process.
The density of the magnesium alloy material is 1.92g/cm3The relative abrasion resistance ε was 10.8.
Room temperature mechanical properties: the yield strength is 213MPa, the tensile strength is 330MPa, and the elongation is 6.5 percent.
Mechanical properties at 300 ℃: the yield strength is 180MPa, the tensile strength is 249MPa, and the elongation is 23%.
Comparative example 3
The present comparative example is the comparative example of example 3, and provides a Mg-4.5Zn-4Er-2.5Nd-1Mn-0.5Zr magnesium alloy material, which is different from the magnesium alloy material involved in example 3 in that the Mg-4.5Zn-4Er-2.5Nd-1Mn-0.5Zr magnesium alloy is prepared by combining raw materials (pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy, Mg-Zr intermediate alloy) with a conventional melting process.
The density of the magnesium alloy material is 1.90g/cm3The relative abrasion resistance ε was 11.7.
Room temperature mechanical properties: the yield strength is 239MPa, the tensile strength is 342MPa, and the elongation is 8.5 percent.
Mechanical properties at 300 ℃: the yield strength is 192MPa, the tensile strength is 268MPa, and the elongation is 29 percent.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.

Claims (2)

1. The high-plasticity light alloy for three-dimensional printing is characterized by comprising the following elements in percentage by weight: 4.5wt.% Zn, 4wt.% Er, 2.5wt.% Nd, 1wt.% Mn, 0.5wt.% Zr, the balance Mg and unavoidable impurities;
the high-plasticity light alloy for three-dimensional printing is prepared by combining raw materials with a traditional smelting process, and sequentially comprises the following steps:
(1) preparing raw materials of pure magnesium, pure zinc, Mg-Er intermediate alloy, Mg-Nd intermediate alloy, Mg-Mn intermediate alloy and Mg-Zr intermediate alloy into spherical powder by using a mechanical grinding process, wherein the particle size is 30-140 mu m, and the oxygen content is 0.06-0.18;
(2) weighing various raw material powders according to the specific contents of the elements of the Mg-Zn-Er-Nd-Mn-Zr magnesium alloy, and fully mixing the metal powders for 50 minutes;
(3) sintering the mixed metal powder into a precast block and carrying out solid solution heat treatment at the solid solution temperature of 500 ℃ for 16 hours;
(4) preparing the alloy prefabricated block into spherical powder by using a mechanical grinding process, wherein the particle size is 30-140 mu m, and the oxygen content is 0.06-0.18;
(5) 3D printing is carried out by using the obtained finished product powder, and the printing parameters are as follows: building rate: 25cm3H, laser scanning speed: 12m/s, layer thickness: and 30 μm.
2. A three-dimensionally printed part produced by three-dimensionally printing using the high-plasticity light alloy for three-dimensional printing according to claim 1.
CN202010083201.8A 2020-02-08 2020-02-08 High-plasticity light alloy for three-dimensional printing and preparation method thereof Active CN111155015B (en)

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CN112974837B (en) * 2021-02-09 2023-05-05 重庆大学 Process method for 3D printing two-step sintering of magnesium alloy material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004183062A (en) * 2002-12-04 2004-07-02 Sumitomo Denko Steel Wire Kk Magnesium-based alloy wire and manufacturing method therefor
CN104762541A (en) * 2015-03-17 2015-07-08 华南协同创新研究院 Rare earth magnesium-alloy material for 3D printing and preparation method of same
CN106148784A (en) * 2015-04-20 2016-11-23 中国科学院金属研究所 A kind of low cost room temperature high-ductility wrought magnesium alloy material and preparation technology thereof
CN106756240A (en) * 2017-02-07 2017-05-31 康硕电气集团有限公司 A kind of tungstenic 3D printing titanium-based alloy material and preparation method thereof
CN108515175A (en) * 2018-05-08 2018-09-11 东南大学 A kind of magnesium alloy slurry and its Method of printing

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004183062A (en) * 2002-12-04 2004-07-02 Sumitomo Denko Steel Wire Kk Magnesium-based alloy wire and manufacturing method therefor
CN104762541A (en) * 2015-03-17 2015-07-08 华南协同创新研究院 Rare earth magnesium-alloy material for 3D printing and preparation method of same
CN106148784A (en) * 2015-04-20 2016-11-23 中国科学院金属研究所 A kind of low cost room temperature high-ductility wrought magnesium alloy material and preparation technology thereof
CN106756240A (en) * 2017-02-07 2017-05-31 康硕电气集团有限公司 A kind of tungstenic 3D printing titanium-based alloy material and preparation method thereof
CN108515175A (en) * 2018-05-08 2018-09-11 东南大学 A kind of magnesium alloy slurry and its Method of printing

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