WO2021073404A1 - 选区激光熔化增材制造技术制备高强韧镁稀土合金的方法 - Google Patents

选区激光熔化增材制造技术制备高强韧镁稀土合金的方法 Download PDF

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WO2021073404A1
WO2021073404A1 PCT/CN2020/118093 CN2020118093W WO2021073404A1 WO 2021073404 A1 WO2021073404 A1 WO 2021073404A1 CN 2020118093 W CN2020118093 W CN 2020118093W WO 2021073404 A1 WO2021073404 A1 WO 2021073404A1
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laser melting
selective laser
alloy
rare earth
strength
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French (fr)
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吴玉娟
邓庆琛
彭立明
罗远航
宿宁
常治宇
薛晓瑜
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上海交通大学
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Priority to US17/769,325 priority Critical patent/US20240123499A1/en
Priority to EP20876620.4A priority patent/EP4029629B1/en
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    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
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    • B33Y10/00—Processes of additive manufacturing
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    • 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
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    • B33Y80/00—Products made by additive manufacturing
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C1/0408—Light metal alloys
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
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    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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    • Y02P10/25—Process efficiency

Definitions

  • the invention relates to the technical field of preparation of non-ferrous metal alloys, in particular to a method for preparing high-strength and tough magnesium rare earth alloys by selective laser melting additive manufacturing technology.
  • magnesium alloy As the lightest metal structural material, magnesium alloy has the advantages of low density, high specific strength and high specific rigidity. It has very broad application prospects in the fields of rail transit, aerospace and 3C products.
  • the commercial magnesium alloys on the market mainly include Mg-Al series and Mg-Zn series, but these magnesium alloys have low absolute strength and poor plasticity, which limits the further expansion of the application range of magnesium alloys.
  • the Mg-RE series magnesium alloy has excellent solid solution strengthening and age hardening effects, which brings great possibilities for the development of high strength and toughness magnesium alloys.
  • the addition of Zn to Mg-RE alloys can not only control the ageing precipitation structure of the alloys, but also introduce long-period stacking order structure (LPSO structure) under appropriate addition amount and process conditions.
  • LPSO structure long-period stacking order structure
  • Adding a small amount of Zr element is mainly to provide heterogeneous nucleation particles to refine crystal grains.
  • SLM Selective laser melting
  • SLM helps to improve the performance of parts required by the aerospace, automotive industry and so on.
  • the SLM technology of magnesium alloys will be one of the very promising methods to control the structure and properties of magnesium alloys and develop high-performance magnesium alloys and components.
  • the alloy s thermal conductivity, solidification temperature range, thermal expansion coefficient, and solidification shrinkage
  • the SLM process parameters of the above-mentioned reported alloys are not suitable for Mg-RE (including Gd) alloys, and it is necessary to develop SLM process parameters suitable for Mg-RE (including Gd) alloys.
  • the Mg-RE (containing Gd) alloy prepared by SLM technology has fine grains and second phase, and the area fraction of the second phase is small.
  • the solid solubility in the ⁇ -Mg matrix is high, which can produce significant fine grain strengthening.
  • solid solution strengthening effect, microstructure morphology and mechanical properties are better than traditional gravity casting methods.
  • the selective laser melting process is used for the preparation of Mg-RE-(Zn)-Zr alloy, and a suitable forming process and subsequent heat treatment process for Mg-RE-(Zn)-Zr alloy are found, it is expected to develop high strength and toughness Magnesium rare earth alloys, and provide theoretical support for magnesium alloy parts in aerospace, automotive and other fields.
  • the purpose of the present invention is to fill the gap of the existing Mg-RE-(Zn)-Zr alloy in the field of selective laser melting preparation, and to provide a method for preparing high-strength and tough magnesium rare earth alloys by selective laser melting additive manufacturing technology, which overcomes traditional casting Magnesium alloy grains and eutectic phase are coarse, composition segregation, defects such as porosity, shrinkage cavity, inclusions and other key problems and poor mechanical properties.
  • the Mg-RE-(Zn)-Zr alloy spherical powder is prepared by gas atomization, and an efficient and flexible additive manufacturing method—selected laser melting technology is selected to prepare high-strength and tough magnesium rare-earth alloys, and the subsequent heat treatment is optimized.
  • the process (T6 or T5) further improves the mechanical properties of the alloy.
  • the SLM process parameters of the present invention are the results of a large number of experiments summarized by the inventor in the early stage.
  • the laser power is selected from 80 to 160W, because higher laser power will produce serious magnesium powder evaporation and splashing, which affects the stability of the molding process and is lower.
  • the power cannot achieve the interlayer metallurgical bonding of magnesium alloy; the laser scanning rate of 100 ⁇ 1000mm/s is selected to match the laser power to obtain the laser energy density required for magnesium alloy SLM forming.
  • the partitioned island scanning strategy is also applied for the first time
  • the Mg-RE-(Zn)-Zr alloy reduces the thermal stress during the forming process and weakens the cracking phenomenon.
  • the subsequent heat treatment of the Mg-RE-(Zn)-Zr alloy in the SLM state is also the first case, because the pure Mg reported in the literature , Mg-Al series and Mg-Zn series alloys do not have the outstanding age hardening potential of Mg-RE-(Zn)-Zr alloy.
  • the SLM process parameters and the subsequent heat treatment process parameters of the present invention are specially designed for the specific alloy composition of Mg-RE-(Zn)-Zr, which belongs to the first research application.
  • the invention prepares a new morphology of a magnesium rare earth alloy with a small content of grain boundary ⁇ phase and fine and dispersed distribution, and the prepared SLM state Mg-RE-(Zn)-Zr alloy structure has fine ⁇ -Mg matrix crystal grains
  • the characteristics of uniform and supersaturated, small content of grain boundary ⁇ phase, fine dispersion distribution, no pores and unfused defects, T6 and T5 Mg-RE-(Zn)-Zr alloy structures have dense and finely dispersed prismatic precipitates
  • Zn-containing alloys will also produce stacking faults or LPSO phases on the basal surface, which have a composite strengthening and toughening effect with the aging precipitation phase on the prism surface.
  • the invention aims to adjust the gas atomization powdering process to prepare magnesium rare earth alloy spherical powder with a specific composition of suitable particle size distribution, and to adjust the crystal grains of the magnesium rare earth alloy by adjusting the process parameters of the selected laser melting and the subsequent heat treatment process parameters
  • the size, the number and shape of the grain boundary ⁇ phase, and the size and number of the aging precipitated phase can be used to prepare a high-strength and toughness magnesium rare-earth alloy that is superior to traditional gravity casting in strength and plasticity.
  • the present invention provides a method for preparing high-strength and toughness magnesium rare-earth alloy by selective laser melting additive manufacturing technology, and the method includes the following steps:
  • the Mg-RE-(Zn)-Zr alloy spherical powder is subjected to selective laser melting and forming to obtain a high-strength and tough magnesium rare-earth alloy with fine grains (1 ⁇ 3 ⁇ m), uniform structure and high density;
  • step B Heat the magnesium alloy prepared in step B to further improve the mechanical properties: solution + aging treatment (T6) or directly aging treatment (T5).
  • the specific composition magnesium rare earth alloy spherical powder contains the following elements in weight percentage: RE10-20%, Zn0-2%, Zr0-0.5%, the balance is Mg and unavoidable impurities, The total amount of impurities is less than 0.02%; the RE includes Gd, and other rare earth elements such as Y can also be added.
  • the Zr content in the magnesium rare earth alloy spherical powder is 0.3-0.5%.
  • step B 200-300 mesh (average particle size of 61 ⁇ m), 300-500 mesh (average particle size of 42 ⁇ m) or 500 mesh or more (average particle size of 34 ⁇ m) of Mg-RE-(Zn) -Zr alloy spherical powder undergoes selective laser melting and forming. If the particle size of the powder is too large, it will not be suitable for molding.
  • the invention regulates and controls the alloy by adjusting the laser power, scanning speed, scanning distance, spot diameter, layer thickness, interlayer rotation angle, substrate preheating temperature, zone width, overlap zone width, and subsequent heat treatment process temperature and time of laser melting in the selected area.
  • this method has the advantages of high processing efficiency, high processing precision, adjustable product structure, high cooling rate leading to uniform and small structure, etc., thereby greatly improving mechanical properties.
  • the spherical powder prepared in step A should be dried in a vacuum drying oven at 100-200°C for 1 to 5 hours before performing selective laser melting and molding to remove water vapor in the powder and improve powder agglomeration Block phenomenon to enhance the fluidity of the powder.
  • the laser-related parameters used in the selective laser melting molding are as follows: laser power is 80-160 W, scanning speed is 100-1000 mm/s, scanning interval is 50-100 ⁇ m, and spot diameter is 65-150 ⁇ m.
  • the laser scanning strategy adopted in the selected area laser melting molding is as follows: the partitioned island scanning strategy is to reduce the thermal stress concentration, the partition width is 3-6mm, and the width of the overlap area between different partitions is 0.1 ⁇ 0.3mm to increase the density of the molded parts to improve the mechanical properties, and the interlayer rotation angle is 70-75° to weaken the anisotropy of the mechanical properties of the manufactured components.
  • step B other process parameters used in the selective laser melting molding are as follows: the layer thickness is 20-40 ⁇ m to ensure the metallurgical bonding between the layers, and the substrate preheating temperature is 25-200°C to reduce the molding process.
  • the temperature gradient reduces thermal stress.
  • step B the selective laser melting molding is performed under the protection of inert gas argon to avoid oxidation, and the oxygen and water vapor content in the molding chamber during the molding process is less than 100 ppm.
  • the temperature of the solution treatment is 450-520°C, and the time is 15min-2h.
  • the temperature of the aging treatment is 175-225°C, and the time is 0-512h.
  • the temperature of the aging treatment is 200° C. and the time is 64 h.
  • the present invention also provides a high-strength and toughness magnesium rare earth alloy prepared according to the foregoing method, and the magnesium rare earth alloy is a Mg-RE-(Zn)-Zr alloy.
  • the Mg-RE-(Zn)-Zr alloy contains the following elements in weight percentage: RE10-20%, Zn0-2%, Zr0-0.5%, the balance is Mg and unavoidable impurities, wherein The total amount of impurities is less than 0.02%, the RE must contain Gd, and other rare earth elements such as Y can also be added.
  • the present invention has the following beneficial effects:
  • the laser melting process of the present invention has a short molding cycle, and can directly mold parts of any complex shape.
  • the molded parts have high density, good product stability and high repeatability.
  • the laser melting process of the selected area of the present invention is carried out under the protection of argon gas to avoid violent oxidation of the powder.
  • the structure of the product prepared by the present invention is improved: the ⁇ -Mg matrix crystal grains are fine and uniform and supersaturated, the grain boundary ⁇ phase content is small and the fine dispersion distribution, nano-level stacking faults, no holes and no fusion defects.
  • the SLM state product prepared by the present invention has good mechanical properties: the room temperature tensile yield strength of the Mg-11.16Gd-1.72Zn-0.44Zr (wt.%) alloy SLM state is 252MPa, the tensile strength is 275MPa, and the elongation is At 4.3%, the strength and plasticity are better than the room temperature tensile properties of the same composition alloy in the semi-continuous casting state (yield strength of 163MPa, tensile strength of 210MPa, and elongation of 3.6%). Compared with the semi-continuous casting state, the SLM state Yield strength increased by 54.6%, tensile strength increased by 31.0%, and elongation increased by 19.4%.
  • the mechanical properties of the SLM product prepared by the present invention are further improved after subsequent heat treatment: after solid solution + aging heat treatment, the room temperature tensile yield strength of the T6 state is as high as 260MPa, the tensile strength is 346MPa, and the elongation is 4.8%, which is significant
  • the room temperature tensile properties (yield strength of 186 MPa, tensile strength of 258 MPa, and elongation of 4.6%) are better than that of semi-continuous casting T6 temper. Compared with semi-continuous casting T6 temper, the yield strength of SLM-T6 temper is increased by 39.8%.
  • the tensile strength is increased by 34.1%, and the elongation is increased by 4.3%; the strength of the alloy is greatly increased after direct aging treatment, but the plasticity is poor.
  • the room temperature tensile yield strength of T5 temper is as high as 382MPa, the tensile strength is 385MPa, and the elongation is 0.4%.
  • the yield strength of the SLM-T5 state is increased by 51.6%, the tensile strength is increased by 40%, and the elongation rate is decreased by 90.7%.
  • Figure 1 is the OM structure diagram (a) and SEM structure diagram (b) of the SLM state Mg-11.16Gd-1.72Zn-0.44Zr (wt.%) alloy prepared in Example 1 of the present invention;
  • Example 2 is a comparison diagram of room temperature tensile properties of Mg-11.16Gd-1.72Zn-0.44Zr (wt.%) alloys prepared in Example 1 and Comparative Example 1 of the present invention in different states;
  • Fig. 3 is the OM structure diagram (a) and SEM structure diagram (b) of the semi-continuous as-cast Mg-11.16Gd-1.72Zn-0.44Zr (wt.%) alloy prepared in Comparative Example 1 of the present invention.
  • This embodiment provides a method for preparing high-strength and toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology, which specifically adopts the following steps:
  • the laser power used in the selective laser melting molding is 80W
  • the scanning speed is 500mm/s
  • the scanning distance is 100 ⁇ m
  • the spot diameter is 100 ⁇ m
  • the layer thickness is 30 ⁇ m
  • the interlayer rotation angle is 73°
  • the scanning strategy is the partition island scanning strategy.
  • the width of the partition is 5mm
  • the width of the overlap area between different partitions is 0.2mm.
  • the T4 magnesium alloy prepared in the above 4) is artificially aged T6 in a constant temperature oil bath furnace, and a single-step aging treatment is adopted: the aging temperature is 200°C for 64h, and then quenched in cold water at 20°C.
  • T5 treatment is performed on the SLM magnesium alloy prepared in 3) above: in a constant temperature oil bath furnace, a single-step aging treatment is adopted: the aging temperature is 200°C for 64h, and then quenched in cold water at 20°C.
  • the SLM state, T4 state, T6 state, and T5 state magnesium alloy prepared in the above 3), 4), 5), and 6) are subjected to room temperature tensile experiments.
  • the tensile machine is a Zwick BTC-Z100 electronic universal material testing machine ,
  • the tensile test rate is 0.5mm/min.
  • the structure of the obtained alloy in the SLM state is shown in Figure 1: It presents the typical characteristics of rapid solidification, the ⁇ -Mg matrix has fine and uniform grains (1 ⁇ 3 ⁇ m), the content of the grain boundary ⁇ phase is small and the distribution is fine and dispersed.
  • the room temperature tensile properties of Mg-11.16Gd-1.72Zn-0.44Zr (wt.%) alloys (SLM, SLM-T4, SLM-T6, SLM-T5) in different states are shown in Figure 2.
  • the room temperature tensile properties of SLM state The yield strength is 252MPa, the tensile strength is 275MPa, and the elongation is 4.3%; the strength and plasticity are improved after solution + aging heat treatment.
  • the room temperature tensile yield strength of T6 is as high as 260MPa, the tensile strength is 346MPa, and the elongation is 4.8%; After direct aging treatment, the strength of the alloy is greatly improved but the plasticity is poor.
  • the room temperature tensile yield strength of T5 temper is as high as 365MPa, the tensile strength is 385MPa, and the elongation is 2.3%.
  • This embodiment provides a method for preparing high-strength and toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology, which specifically adopts the following steps:
  • the laser power used in the selective laser melting molding is 80W
  • the scanning speed is 100mm/s
  • the scanning distance is 100 ⁇ m
  • the spot diameter is 100 ⁇ m
  • the layer thickness is 2 ⁇ m
  • the interlayer rotation angle is 70°
  • the scanning strategy is the partition island scanning strategy.
  • the width of the partition is 4mm
  • the width of the overlap area between different partitions is 0.3mm.
  • the T4 magnesium alloy prepared in the above 4) is artificially aged T6 in a constant temperature oil bath furnace, and a single-step aging treatment is adopted: the aging temperature is 200°C for 64h, and then quenched in cold water at 20°C.
  • T5 treatment is performed on the SLM magnesium alloy prepared in 3) above: in a constant temperature oil bath furnace, a single-step aging treatment is adopted: the aging temperature is 200°C for 64h, and then quenched in cold water at 20°C.
  • the SLM state, T4 state, T6 state, and T5 state magnesium alloy prepared in the above 3), 4), 5), and 6) are subjected to room temperature tensile experiments.
  • the tensile machine is a Zwick BTC-Z100 electronic universal material testing machine ,
  • the tensile test rate is 0.5mm/min.
  • the obtained SLM alloy presents the typical characteristics of rapid solidification and fine grains.
  • the ⁇ -Mg matrix grains are small and uniform (1 ⁇ 3 ⁇ m), the content of grain boundary ⁇ phase is small and the distribution is fine and dispersed.
  • the room temperature tensile yield strength of the SLM state is 306MPa, the tensile strength is 310MPa, and the elongation rate is 0.7%;
  • the room temperature tensile yield strength of the T6 state is as high as 308MPa, the tensile strength is 337MPa, and the elongation rate is 0.3%;
  • the room temperature of the T5 state The tensile yield strength is as high as 340MPa, the tensile strength is 343MPa, and the elongation is 0.4%.
  • This embodiment provides a method for preparing high-strength and toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology, which specifically adopts the following steps:
  • Mg-19.89Gd (wt.%) alloy powder is prepared by aerosolization method, and the alloy powder is sieved, and powders with 500 meshes or more (average particle size of 34 ⁇ m) are selected for selective laser melting molding.
  • the laser power used in the selective laser melting molding is 160W
  • the scanning speed is 1000mm/s
  • the scanning distance is 50 ⁇ m
  • the spot diameter is 65 ⁇ m
  • the layer thickness is 40 ⁇ m
  • the interlayer rotation angle is 75°
  • the scanning strategy is the partition island scanning strategy.
  • the width of the partition is 3mm
  • the width of the overlap area between different partitions is 0.1mm.
  • the T4 magnesium alloy prepared in 4) is artificially aged T6 in a constant temperature oil bath furnace, and a single-step aging treatment is adopted: the aging temperature is 175°C for 512h, and then quenched in cold water at 20°C.
  • T5 treatment is performed on the SLM magnesium alloy prepared in the above 3): in a constant temperature oil bath furnace, a single-step aging treatment is adopted: the aging temperature is 175°C for 512h, and then quenched in cold water at 20°C.
  • the SLM state, T4 state, T6 state, and T5 state magnesium alloy prepared in the above 3), 4), 5), and 6) are subjected to room temperature tensile experiments.
  • the tensile machine is a Zwick BTC-Z100 electronic universal material testing machine ,
  • the tensile test rate is 0.5 mm/min.
  • the obtained SLM alloy presents the typical characteristics of rapid solidification and fine grains.
  • the ⁇ -Mg matrix grains are small and uniform (1 ⁇ 3 ⁇ m), the content of grain boundary ⁇ phase is small and the distribution is fine and dispersed.
  • the room temperature tensile yield strength of SLM state is 358MPa, the tensile strength is 362MPa, and the elongation rate is 0.7%;
  • the room temperature tensile yield strength of T6 state is as high as 365MPa, the tensile strength is 374MPa, and the elongation rate is 0.5%;
  • the room temperature of T5 state is
  • the tensile yield strength is as high as 410MPa, the tensile strength is 418MPa, and the elongation is 0.3%.
  • This embodiment provides a method for preparing high-strength and toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology, which specifically adopts the following steps:
  • the laser power used in the selective laser melting molding is 120W
  • the scanning speed is 300mm/s
  • the scanning distance is 100 ⁇ m
  • the spot diameter is 90 ⁇ m
  • the layer thickness is 30 ⁇ m
  • the interlayer rotation angle is 71°
  • the scanning strategy is the partition island scanning strategy.
  • the width of the partition is 6mm
  • the width of the overlap area between different partitions is 0.2mm.
  • the T4 magnesium alloy prepared in the above 4) is artificially aged T6 in a constant temperature oil bath furnace, and a single-step aging treatment is adopted: the aging temperature is 200°C for 64h, and then quenched in cold water at 20°C.
  • T5 treatment is performed on the SLM magnesium alloy prepared in 3) above: in a constant temperature oil bath furnace, a single-step aging treatment is adopted: the aging temperature is 200°C for 64h, and then quenched in cold water at 20°C.
  • the SLM state, T4 state, T6 state, and T5 state magnesium alloy prepared in the above 3), 4), 5), and 6) are subjected to room temperature tensile experiments.
  • the tensile machine is a Zwick BTC-Z100 electronic universal material testing machine ,
  • the tensile test rate is 0.5mm/min.
  • the obtained SLM structure of the alloy presents typical characteristics of rapid solidification.
  • the ⁇ -Mg matrix has fine and uniform grains (1 ⁇ 3 ⁇ m), a small content of grain boundary ⁇ phase and fine dispersion distribution.
  • the room temperature tensile yield strength of SLM state is 245MPa, the tensile strength is 246MPa, and the elongation rate is 0.1%;
  • the room temperature tensile yield strength of T6 state is as high as 296MPa, the tensile strength is 365MPa, and the elongation rate is 0.4%;
  • the room temperature of T5 state is
  • the tensile yield strength is as high as 302MPa, the tensile strength is 363MPa, and the elongation is 0.3%.
  • This embodiment provides a method for preparing high-strength and toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology, which specifically adopts the following steps:
  • the laser power used in the selective laser melting molding is 160W
  • the scanning speed is 700mm/s
  • the scanning distance is 70 ⁇ m
  • the spot diameter is 100 ⁇ m
  • the layer thickness is 20 ⁇ m
  • the interlayer rotation angle is 74°
  • the scanning strategy is the partition island scanning strategy.
  • the width of the partition is 4mm
  • the width of the overlap area between different partitions is 0.2mm.
  • the T4 magnesium alloy prepared in the above 4) is artificially aged T6 in a constant temperature oil bath furnace, and a single-step aging treatment is adopted: the aging temperature is 200°C for 64h, and then quenched in cold water at 20°C.
  • T5 treatment is performed on the SLM magnesium alloy prepared in 3) above: in a constant temperature oil bath furnace, a single-step aging treatment is adopted: the aging temperature is 200°C for 64h, and then quenched in cold water at 20°C.
  • the SLM state, T4 state, T6 state, and T5 state magnesium alloy prepared in the above 3), 4), 5), and 6) are subjected to room temperature tensile experiments.
  • the tensile machine is a Zwick BTC-Z100 electronic universal material testing machine ,
  • the tensile test rate is 0.5mm/min.
  • the obtained SLM structure of the alloy presents typical characteristics of rapid solidification.
  • the ⁇ -Mg matrix has fine and uniform grains (1 ⁇ 3 ⁇ m), a small content of grain boundary ⁇ phase and fine dispersion distribution.
  • the room temperature tensile yield strength of SLM state is 353MPa, the tensile strength is 388MPa, and the elongation rate is 1.4%;
  • the room temperature tensile yield strength of T6 state is as high as 315MPa, the tensile strength is 393MPa, and the elongation rate is 3.0%;
  • the room temperature of T5 state is
  • the tensile yield strength is as high as 374MPa, the tensile strength is 396MPa, and the elongation is 0.9%.
  • This embodiment provides a method for preparing high-strength and toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology, which specifically adopts the following steps:
  • the laser power used in the selective laser melting molding is 80W
  • the scanning speed is 350mm/s
  • the scanning distance is 90 ⁇ m
  • the spot diameter is 100 ⁇ m
  • the layer thickness is 30 ⁇ m
  • the interlayer rotation angle is 73°
  • the scanning strategy is the partition island scanning strategy.
  • the width of the partition is 6mm
  • the width of the overlap area between different partitions is 0.3mm.
  • the T4 magnesium alloy prepared in the above 4) is artificially aged T6 in a constant temperature oil bath furnace, and a single-step aging treatment is adopted: the aging temperature is 175°C for 128 hours, and then quenched in cold water at 20°C.
  • T5 treatment is performed on the SLM magnesium alloy prepared in 3) above: in a constant temperature oil bath furnace, a single-step aging treatment is adopted: the aging temperature is 175°C, the time is 128h, and then quenched in cold water at 20°C.
  • the SLM state, T4 state, T6 state, and T5 state magnesium alloy prepared in the above 3), 4), 5), and 6) are subjected to room temperature tensile experiments.
  • the tensile machine is a Zwick BTC-Z100 electronic universal material testing machine ,
  • the tensile test rate is 0.5mm/min.
  • the obtained SLM structure of the alloy presents typical characteristics of rapid solidification.
  • the ⁇ -Mg matrix has fine and uniform grains (1 ⁇ 3 ⁇ m), a small content of grain boundary ⁇ phase and fine dispersion distribution.
  • the room temperature tensile yield strength of SLM state is 194MPa, the tensile strength is 253MPa, and the elongation rate is 6.2%;
  • the room temperature tensile yield strength of T6 state is as high as 217MPa, the tensile strength is 298MPa, and the elongation rate is 4.5%;
  • the room temperature of T5 state is
  • the tensile yield strength is as high as 243MPa, the tensile strength is 306MPa, and the elongation rate is 3.4%.
  • This embodiment provides a method for preparing high-strength and toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology, which specifically adopts the following steps:
  • the laser power used in the selective laser melting molding is 80W
  • the scanning speed is 800mm/s
  • the scanning distance is 100 ⁇ m
  • the spot diameter is 150 ⁇ m
  • the layer thickness is 40 ⁇ m
  • the interlayer rotation angle is 74°
  • the scanning strategy is the partition island scanning strategy.
  • the width of the partition is 6mm
  • the width of the overlap area between different partitions is 0.3mm.
  • the T4 magnesium alloy prepared in the above 4) is artificially aged T6 in a constant temperature oil bath furnace, and a single-step aging treatment is adopted: the aging temperature is 175°C for 128 hours, and then quenched in cold water at 20°C.
  • T5 treatment is performed on the SLM magnesium alloy prepared in 3) above: in a constant temperature oil bath furnace, a single-step aging treatment is adopted: the aging temperature is 175°C, the time is 128h, and then quenched in cold water at 20°C.
  • the SLM state, T4 state, T6 state, and T5 state magnesium alloy prepared in the above 3), 4), 5), and 6) are subjected to room temperature tensile experiments.
  • the tensile machine is a Zwick BTC-Z100 electronic universal material testing machine ,
  • the tensile test rate is 0.5mm/min.
  • the obtained SLM structure of the alloy presents typical characteristics of rapid solidification.
  • the ⁇ -Mg matrix has fine and uniform grains (1 ⁇ 3 ⁇ m), a small content of grain boundary ⁇ phase and fine dispersion distribution.
  • the room temperature tensile yield strength of the SLM state is 187MPa, the tensile strength is 243MPa, and the elongation rate is 5.7%;
  • the room temperature tensile yield strength of the T6 state is as high as 208MPa, the tensile strength is 285MPa, and the elongation rate is 4.3%;
  • the room temperature of the T5 state is
  • the tensile yield strength is as high as 235MPa, the tensile strength is 297MPa, and the elongation is 3.1%.
  • This embodiment provides a method for preparing high-strength and toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology, which specifically adopts the following steps:
  • the laser power used in the selective laser melting molding is 80W
  • the scanning speed is 300mm/s
  • the scanning distance is 100 ⁇ m
  • the spot diameter is 90 ⁇ m
  • the layer thickness is 20 ⁇ m
  • the interlayer rotation angle is 71°
  • the scanning strategy is a partitioned island scanning strategy.
  • the width of the partition is 3mm
  • the width of the overlap area between different partitions is 0.1mm.
  • T4 treatment of the SLM magnesium alloy prepared in the above 3) in an air resistance furnace, and put the SO 2 gas released by thermal decomposition of pyrite to protect the alloy from flame retardancy, and take a single step solid solution Treatment: Solid solution at 500°C for 2h, then quenched in cold water at 20°C.
  • the T4 magnesium alloy prepared in 4) is artificially aged T6 in a constant temperature oil bath furnace, and a single-step aging treatment is adopted: the aging temperature is 225°C for 64 hours, and then quenched in cold water at 20°C.
  • T5 treatment is performed on the SLM magnesium alloy prepared in the above 3): in a constant temperature oil bath furnace, a single-step aging treatment is adopted: the aging temperature is 225°C for 64h, and then quenched in cold water at 20°C.
  • the SLM state, T4 state, T6 state, and T5 state magnesium alloy prepared in the above 3), 4), 5), and 6) are subjected to room temperature tensile experiments.
  • the tensile machine is a Zwick BTC-Z100 electronic universal material testing machine ,
  • the tensile test rate is 0.5mm/min.
  • the obtained SLM alloy presents the typical characteristics of rapid solidification and fine grains.
  • the ⁇ -Mg matrix grains are small and uniform (1 ⁇ 3 ⁇ m), the content of grain boundary ⁇ phase is small and the distribution is fine and dispersed.
  • the room temperature tensile yield strength of the SLM state is 356MPa, the tensile strength is 389MPa, and the elongation rate is 3.9%;
  • the room temperature tensile yield strength of the T6 state is as high as 367MPa, the tensile strength is 423MPa, and the elongation rate is 4.7%;
  • the room temperature of the T5 state The tensile yield strength is as high as 411MPa, the tensile strength is 432MPa, and the elongation rate is 1.8%.
  • This comparative example provides a magnesium rare earth alloy prepared by gravity casting.
  • the alloy composition is basically the same as that of Example 1, except that: in this comparative example, the preparation method adopted is gravity casting.
  • the OM structure and SEM structure of the semi-continuous as-cast Mg-11.16Gd-1.72Zn-0.44Zr (wt.%) alloy prepared in this comparative example are shown in Figure 3.
  • the grain size is about ⁇ 50 ⁇ m, and the grain boundary ⁇ phase It is lamellar, relatively coarse, and presents typical eutectic reaction characteristics.
  • the room temperature tensile properties of Mg-11.16Gd-1.72Zn-0.44Zr (wt.%) alloy in different states (As-cast, As-cast T6) are shown in Figure 2.
  • the room temperature tensile yield strength of the as-cast state is 163MPa, The tensile strength is 210MPa, and the elongation is 3.6%; after solution + aging heat treatment (480°C-12h+200°C-32h), the room temperature tensile yield strength of T6 is as high as 186MPa, the tensile strength is 258MPa, and the elongation is It is 4.6%.
  • the strength and plasticity of the alloy prepared by gravity casting are lower than those of the same state alloy prepared by selective laser melting. The reason for the difference is that the cooling rate of gravity casting is much lower than that of laser melting in the selected area, and the ⁇ -Mg matrix grains and the grain boundary ⁇ phase are coarse.
  • This comparative example provides a method for preparing high-strength and tough magnesium rare earth alloys by selective laser melting additive manufacturing technology, which is basically the same as Example 1, except that: in this comparative example, the laser scanning speed used in selective laser melting molding It is 1500mm/s.
  • the room temperature tensile yield strength of the SLM state is 119 MPa, the tensile strength is 122 MPa, and the elongation rate is 0.3%.
  • the strength and plasticity of the SLM state alloy are significantly lower than those of the SLM state alloy prepared in Example 1. The reason for the difference lies in the fact that the laser scanning speed is too large and the laser action time is too short, and the laser energy density is too low to completely melt all the powder, resulting in a large number of unfused defects.
  • This comparative example provides a method for preparing high-strength and tough magnesium rare earth alloys by selective laser melting additive manufacturing technology, which is basically the same as Example 1, except that: in this comparative example, the laser scanning distance used in selective laser melting molding It is 150 ⁇ m.
  • the room temperature tensile yield strength of the SLM state is 204 MPa, the tensile strength is 221 MPa, and the elongation rate is 1.3%.
  • the strength and plasticity of the SLM state are significantly lower than those of the SLM state alloy prepared in Example 1. The reason for the difference is that the laser scanning distance is too large, which leads to the overlap between the scan tracks, and there are a lot of non-fusion defects in the overlap area of the scan tracks.
  • This comparative example provides a magnesium rare earth alloy prepared by gravity casting.
  • the alloy composition is basically the same as that of Example 2, except that: in this comparative example, the preparation method adopted is gravity casting.
  • the room temperature tensile yield strength of the as-cast state is 169MPa, the tensile strength is 251MPa, and the elongation rate is 5.7%; after solution + aging heat treatment (520°C-12h+200°C-64h), the room temperature tensile yield strength of T6 It is as high as 232MPa, the tensile strength is 296MPa, and the elongation is 0.6%.
  • the strength of the alloy prepared by gravity casting is lower than that of the alloy in the same state prepared by selective laser melting, but the plasticity. The reason for the difference is that the cooling rate of gravity casting is much lower than that of laser melting in the selected area, and the ⁇ -Mg matrix grains and the grain boundary ⁇ phase are coarse.
  • This comparative example provides a method for preparing high-strength and toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology, which is basically the same as Example 2, except that: in this comparative example, the laser power used for selective laser melting is 40W.

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Abstract

本发明提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，包含如下步骤：A、通过气雾化的方法制备出Mg-RE-(Zn)-Zr合金球形粉末；B、将Mg-RE-(Zn)-Zr合金球形粉末进行选区激光熔化成型得到高强韧镁稀土合金；C、将步骤B制得的镁稀土合金进行热处理：固溶+时效处理或直接进行时效处理，即可。本发明通过调控选区激光熔化的工艺参数(激光功率、扫描速度、扫描间距、光斑直径、层厚、层间转角、基板预热温度、分区宽度和搭接区宽度)和后续热处理的工艺参数(温度和时间)来调控合金的微观组织和力学性能，首次使用选区激光熔化工艺制备出高强韧Mg-RE-(Zn)-Zr合金。

Description

选区激光熔化增材制造技术制备高强韧镁稀土合金的方法 技术领域
本发明涉及有色金属合金制备的技术领域，具体为一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法。
背景技术
镁合金作为最轻的金属结构材料，具有密度低、比强度和比刚度高等优点，在轨道交通、航空航天和3C产品等领域有着非常广阔的应用前景。目前市场上商业化的镁合金主要包括Mg-Al系和Mg-Zn系两大类，但是这些镁合金的绝对强度较低和塑性较差，因此限制了进一步扩大镁合金的应用范围。Mg-RE系镁合金具有优异的固溶强化和时效硬化效应，为开发高强韧镁合金带来了巨大可能。此外，往Mg-RE系合金中添加Zn元素，不仅能够调控该合金系的时效析出组织，而且在适当的加入量以及工艺条件下会引入长周期堆垛有序结构(LPSO结构)，大量研究表明LPSO结构可以进一步提高合金的强度和塑性。添加微量的Zr元素主要是提供异质形核质点以细化晶粒。
选区激光熔化(SLM)是目前比较有前景的激光辅助增材制造方法之一，能够逐层沉积任意复杂形状的金属部件，可实现传统铸造难以实现甚至不能实现的高质量复杂部件制备，非常适合小批量、复杂构件的个性化定制。另一方面，快速扫描激光束产生微小熔池和热影响区，且极高的冷却速率(10 4～10 6K/s)可导致微观组织的细化和固溶度的扩大，从而产生显著的细晶强化和固溶强化效应，使得SLM制备的构件的力学性能显著高于铸件，接近锻件的性能，故SLM有助于改善航空航天、汽车工业等所需部件的性能。随着环境与能源问题的日益突出，镁合金的SLM技术将是调控镁合金组织性能，并开发出高性能镁合金及部件的非常有前景的方法之一。
目前，国内外针对镁合金的SLM工艺研究仅有少量报道，涉及纯Mg、Mg-Al系、Mg-Zn系，但是还未见Mg-RE(含Gd)系合金的SLM报道。Mg-RE(含Gd)系合金的室温和高温拉伸性能、抗蠕变性能、刚度等都明显优于上述已报道合金，同时该合金的导热系数、凝固温度区间、热膨胀系数、凝固收缩率等参数有别于上述已报道合金，故上述已报道合金的SLM工艺参数并不适合Mg-RE(含Gd)系合金，需要开发适合 Mg-RE(含Gd)系合金的SLM工艺参数。此外，采用SLM技术制备的Mg-RE(含Gd)系合金晶粒和第二相都细小，第二相面积分数小，ɑ-Mg基体内的固溶度高，能够产生显著的细晶强化和固溶强化效应，微观组织形态和力学性能都优于传统重力铸造方式。因此，如果将选区激光熔化工艺用于Mg-RE-(Zn)-Zr合金的制备上，并且找到适合Mg-RE-(Zn)-Zr合金的成型工艺及后续热处理工艺，有望研发出高强韧的镁稀土合金，并为航空航天、汽车等领域镁合金部件提供理论支持。
发明内容
本发明的目的在于补全现有Mg-RE-(Zn)-Zr合金在选区激光熔化制备领域的空白，提供一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，克服传统铸造镁合金晶粒和共晶相粗大、成分偏析、易产生疏松、缩孔、夹杂等缺陷及力学性能较差的关键问题。通过气雾化的方法制备出Mg-RE-(Zn)-Zr合金球形粉末，选用一种高效灵活的增材制造手段——选区激光熔化技术来制备高强韧镁稀土合金，并通过优化后续热处理工艺(T6或T5)进一步提高合金的力学性能。
本发明的SLM工艺参数是发明人前期大量实验总结的结果，例如，激光功率选取80～160W，是因为更高的激光功率会产生严重的镁粉蒸发飞溅现象而影响成型过程稳定性和更低的功率无法实现镁合金的层间冶金结合；激光扫描速率选取100～1000mm/s是和激光功率相匹配的以得到镁合金SLM成型所需的激光能量密度，分区岛状扫描策略也是首次应用于Mg-RE-(Zn)-Zr合金以减小成型过程的热应力而减弱开裂现象，对SLM态的Mg-RE-(Zn)-Zr合金进行后续热处理也是首例，因为文献报道的纯Mg、Mg-Al系和Mg-Zn系等合金都不具有Mg-RE-(Zn)-Zr合金这样出众的时效硬化潜力。综上，本发明的SLM工艺参数和后续热处理工艺参数都是针对Mg-RE-(Zn)-Zr这一特定合金成分而专门设计的，属于首次研究应用。
本发明制得一种镁稀土合金中晶界β相含量少且细小弥散分布的一种新形貌，制备的SLM态Mg-RE-(Zn)-Zr合金组织具有ɑ-Mg基体晶粒细小均匀且过饱和、晶界β相含量少且细小弥散分布、无孔洞和未熔合缺陷的特点，T6和T5态Mg-RE-(Zn)-Zr合金组织具有密集细小弥散分布的棱柱面析出相的特点，此外，含Zn合金还会产生基面层错或LPSO相，与棱柱面时效析出相产生复合强韧化的作用。
本发明旨在调整气雾化制粉工艺制备出具有合适粒径分布的特定成分的镁稀土合金球形粉末，并通过调整选区激光熔化的工艺参数和后续热处理工艺参数来调控镁稀土合金的晶粒大小、晶界β相的数量与形态、时效析出相的大小和数量以制备出强度和塑 性都优于传统重力铸造的高强韧镁稀土合金。
本发明的目的是通过以下技术方案实现的：
本发明提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，所述方法包含如下步骤：
A、通过气雾化的方法制备出Mg-RE-(Zn)-Zr合金球形粉末；
B、将Mg-RE-(Zn)-Zr合金球形粉末进行选区激光熔化成型得到晶粒细小(1～3μm)、组织均匀、高致密度的高强韧镁稀土合金；
C、将步骤B制得的镁合金进行热处理以进一步改善力学性能：固溶+时效处理(T6)或直接进行时效处理(T5)，即可。
优选地，步骤A中，所述特定成分镁稀土合金球形粉末中包含如下重量百分数的各元素：RE10～20％、Zn0～2％、Zr0～0.5％、余量为Mg和不可避免的杂质，其中杂质的总量小于0.02％；所述RE包括Gd，还可添加Y等其他稀土元素。
更优选地，所述镁稀土合金球形粉末中，Zr含量为0.3～0.5％。
优选地，步骤B中，选用200～300目(平均粒径为61μm)、300～500目(平均粒径为42μm)或500目以上(平均粒径为34μm)的Mg-RE-(Zn)-Zr合金球形粉末进行选区激光熔化成型。若粉末的粒径过大，将不适合成型。
本发明通过调控选区激光熔化的激光功率、扫描速度、扫描间距、光斑直径、层厚、层间转角、基板预热温度、分区宽度、搭接区宽度和后续热处理工艺的温度和时间来调控合金的组织，同现有的镁合金成型方式相比，该方法具有加工效率高、加工精度高、产品的组织可调控、冷却速度高导致组织均匀细小等优点，从而大幅度提升力学性能。
优选地，步骤B中，步骤A制得的球形粉末进行选区激光熔化成型之前要在真空干燥箱中进100～200℃，1～5h的干燥处理以去除粉末中的水蒸气和改善粉末团聚结块现象以增强粉末的流动性。
优选地，步骤B中，所述选区激光熔化成型采用的激光相关参数如下：激光功率为80～160W，扫描速度为100～1000mm/s，扫描间距为50～100μm，光斑直径为65～150μm。
优选地，步骤B中，所述选区激光熔化成型采用的激光扫描策略如下：分区岛状扫描策略以减小热应力集中，分区宽度为3～6mm，不同分区之间的搭接区宽度为0.1～0.3mm以提高成型零件的致密度从而提高力学性能，层间转角为70～75°以减弱制得构件力学性能的各向异性。
优选地，步骤B中，所述选区激光熔化成型采用的其他工艺参数如下：层厚为 20～40μm以保证层间的冶金结合，基板预热温度为25～200℃以减小成型的过程的温度梯度从而减小热应力。
优选地，步骤B中，所述选区激光熔化成型在惰性气体氩气保护下进行以避免氧化，成型过程中成型舱室内氧和水蒸气含量低于100ppm。
优选地，步骤C中，所述固溶处理的温度为450～520℃，时间为15min～2h。
优选地，步骤C中，所述时效处理的温度为175～225℃，时间为0～512h。
更优选地，所述时效处理的温度为200℃，时间为64h。
本发明还提供了一种根据前述方法制备的高强韧镁稀土合金，所述镁稀土合金为Mg-RE-(Zn)-Zr合金。
优选地，所述Mg-RE-(Zn)-Zr合金中包含如下重量百分数的各元素：RE10～20％、Zn0～2％、Zr0～0.5％、余量为Mg和不可避免的杂质，其中杂质的总量小于0.02％，所述RE一定包含Gd，还可添加Y等其他稀土元素。
与现有技术相比，本发明具有如下的有益效果：
1、本发明选区激光熔化过程成型周期短，可直接成型任意复杂形状零件，成型零件致密度高，产品稳定性好，重复性高。
2、本发明选区激光熔化过程在氩气保护下进行，避免粉末剧烈氧化。
3、本发明制备的产品组织得到改善：ɑ-Mg基体晶粒细小均匀且过饱和、晶界β相含量少且细小弥散分布、纳米级基面层错、无孔洞和未熔合缺陷。
4、本发明制备的SLM态产品具有良好的力学性能：Mg-11.16Gd-1.72Zn-0.44Zr(wt.％)合金SLM态的室温拉伸屈服强度为252MPa，抗拉强度为275MPa，延伸率为4.3％，强度和塑性都优于同样成分合金半连续铸造态的室温拉伸性能(屈服强度为163MPa，抗拉强度210MPa，延伸率为3.6％)，相比于半连续铸造态，SLM态屈服强度提升54.6％，抗拉强度提升31.0％，延伸率提升19.4％。
5、本发明制备的SLM态产品经过后续热处理后力学性能进一步提升：进行固溶+时效热处理后，T6态的室温拉伸屈服强度高达260MPa，抗拉强度为346MPa，延伸率为4.8％，显著优于半连续铸造T6态的室温拉伸性能(屈服强度为186MPa，抗拉强度258MPa，延伸率为4.6％)，相比于半连续铸造T6态，SLM-T6态屈服强度提升39.8％，抗拉强度提升34.1％，延伸率提升4.3％；直接进行时效处理后合金的强度大幅度提升但塑性较差，T5态的室温拉伸屈服强度高达382MPa，抗拉强度为385MPa，延伸率为0.4％，相比于SLM态，SLM-T5态屈服强度提升51.6％，抗拉强度提升40％，延伸率下降90.7％。
附图说明
通过阅读参照以下附图对非限制性实施例所作的详细描述，本发明的其它特征、目的和优点将会变得更明显：
图1是本发明实施例1制备的SLM态Mg-11.16Gd-1.72Zn-0.44Zr(wt.％)合金的OM组织图(a)和SEM组织图(b)；
图2是本发明实施例1和对比例1制备的Mg-11.16Gd-1.72Zn-0.44Zr(wt.％)合金不同状态的室温拉伸性能对比图；
图3是本发明对比例1制备的半连续铸造态Mg-11.16Gd-1.72Zn-0.44Zr(wt.％)合金的OM组织图(a)和SEM组织图(b)。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明，但不以任何形式限制本发明。应当指出的是，对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变化和改进。这些都属于本发明的保护范围。
实施例1
本实施例提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，具体采用以下步骤：
1)通过气雾化的方法制备出Mg-11.16Gd-1.72Zn-0.44Zr(wt.％)合金粉末，并对合金粉末进行筛分，选用300～500目(平均粒径为42μm)的粉末进行选区激光熔化成型。
2)将粉末在真空干燥箱中进200℃/5h的干燥处理后装入选区激光熔化设备的粉床内，并预热基板到200℃，通入保护气体氩气进行气体循环，待成型舱室内氧和水蒸气含量低于100ppm开始进行选区激光熔化成型。
3)选区激光熔化成型采用的激光功率为80W，扫描速度为500mm/s，扫描间距为100μm，光斑直径为100μm，层厚为30μm，层间转角为73°，扫描策略为分区岛状扫描策略，分区宽度为5mm，不同分区之间的搭接区宽度为0.2mm。
4)将上述3)制备的SLM态镁合金进行T4处理：在空气电阻炉中进行，并放入硫铁矿以热分解释放出的SO 2气体对合金加以阻燃保护，采取单步固溶处理:480℃下固溶1h，随后在20℃冷水中淬火。
5)将上述4)制备的T4态镁合金在恒温油浴炉中进行人工时效T6处理，采取单步时效处理：时效温度为200℃，时间为64h，随后在20℃冷水中淬火。
6)将上述3)制备的SLM态镁合金进行T5处理：在恒温油浴炉中进行，采取单步时效处理：时效温度为200℃，时间为64h，随后在20℃冷水中淬火。
7)将上述3)、4)、5)、6)制备的SLM态、T4态、T6态、T5态镁合金进行室温拉伸实验，拉伸机为Zwick BTC—Z100型电子万能材料试验机，拉伸测试速率为0.5mm/min。
所得合金SLM态的组织如图1所示：呈现典型的快速凝固的特点，ɑ-Mg基体晶粒细小均匀(1～3μm)、晶界β相含量少且细小弥散分布。Mg-11.16Gd-1.72Zn-0.44Zr(wt.％)合金(SLM、SLM-T4、SLM-T6、SLM-T5)不同状态的室温拉伸性能如图2所示，SLM态的室温拉伸屈服强度为252MPa，抗拉强度为275MPa，延伸率为4.3％；进行固溶+时效热处理后强度和塑性都提升，T6态的室温拉伸屈服强度高达260MPa，抗拉强度为346MPa，延伸率为4.8％；直接进行时效处理后合金的强度大幅度提升但塑性较差，T5态的室温拉伸屈服强度高达365MPa，抗拉强度为385MPa，延伸率为2.3％。
实施例2
本实施例提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，具体采用以下步骤：
1)通过气雾化的方法制备出Mg-14.92Gd-0.30Zr(wt.％)合金粉末，并对合金粉末进行筛分，选用300～500目(平均粒径为42μm)的粉末进行选区激光熔化成型。
2)将粉末在真空干燥箱中进200℃/5h的干燥处理后装入选区激光熔化设备的粉床内，并预热基板到150℃，通入保护气体氩气进行气体循环，待成型舱室内氧和水蒸气含量低于100ppm开始进行选区激光熔化成型。
3)选区激光熔化成型采用的激光功率为80W，扫描速度为100mm/s，扫描间距为100μm，光斑直径为100μm，层厚为2μm，层间转角为70°，扫描策略为分区岛状扫描策略，分区宽度为4mm，不同分区之间的搭接区宽度为0.3mm。
4)将上述3)制备的SLM态镁合金进行T4处理：在空气电阻炉中进行，并放入硫铁矿以热分解释放出的SO 2气体对合金加以阻燃保护，采取单步固溶处理:520℃下固溶15min，随后在20℃冷水中淬火。
5)将上述4)制备的T4态镁合金在恒温油浴炉中进行人工时效T6处理，采取单步时效处理：时效温度为200℃，时间为64h，随后在20℃冷水中淬火。
6)将上述3)制备的SLM态镁合金进行T5处理：在恒温油浴炉中进行，采取单步时效处理：时效温度为200℃，时间为64h，随后在20℃冷水中淬火。
7)将上述3)、4)、5)、6)制备的SLM态、T4态、T6态、T5态镁合金进行室温拉伸实验，拉伸机为Zwick BTC—Z100型电子万能材料试验机，拉伸测试速率为0.5mm/min。
所得SLM态合金呈现典型的快速凝固细小晶粒的特点，ɑ-Mg基体晶粒细小均匀(1～3μm)、晶界β相含量少且细小弥散分布。SLM态的室温拉伸屈服强度为306MPa，抗拉强度为310MPa，延伸率为0.7％；T6态的室温拉伸屈服强度高达308MPa，抗拉强度为337MPa，延伸率为0.3％；T5态的室温拉伸屈服强度高达340MPa，抗拉强度为343MPa，延伸率为0.4％。
实施例3
本实施例提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，具体采用以下步骤：
1)通过气雾化的方法制备出Mg-19.89Gd(wt.％)合金粉末，并对合金粉末进行筛分，选用500目以上(平均粒径为34μm)的粉末进行选区激光熔化成型。
2)将粉末在真空干燥箱中进150℃/4h的干燥处理后装入选区激光熔化设备的粉床内，并预热基板到100℃，通入保护气体氩气进行气体循环，待成型舱室内氧和水蒸气含量低于100ppm开始进行选区激光熔化成型。
3)选区激光熔化成型采用的激光功率为160W，扫描速度为1000mm/s，扫描间距为50μm，光斑直径为65μm，层厚为40μm，层间转角为75°，扫描策略为分区岛状扫描策略，分区宽度为3mm，不同分区之间的搭接区宽度为0.1mm。
4)将上述3)制备的SLM态镁合金进行T4处理：在空气电阻炉中进行，并放入硫铁矿以热分解释放出的SO 2气体对合金加以阻燃保护，采取单步固溶处理:520℃下固溶2h，随后在20℃冷水中淬火。
5)将上述4)制备的T4态镁合金在恒温油浴炉中进行人工时效T6处理，采取单步时效处理：时效温度为175℃，时间为512h，随后在20℃冷水中淬火。
6)将上述3)制备的SLM态镁合金进行T5处理：在恒温油浴炉中进行，采取单步时效处理：时效温度为175℃，时间为512h，随后在20℃冷水中淬火。
7)将上述3)、4)、5)、6)制备的SLM态、T4态、T6态、T5态镁合金进行室温拉伸实验，拉伸机为Zwick BTC—Z100型电子万能材料试验机，拉伸测试速率为0.5 mm/min。
所得SLM态合金呈现典型的快速凝固细小晶粒的特点，ɑ-Mg基体晶粒细小均匀(1～3μm)、晶界β相含量少且细小弥散分布。SLM态的室温拉伸屈服强度为358MPa，抗拉强度为362MPa，延伸率为0.7％；T6态的室温拉伸屈服强度高达365MPa，抗拉强度为374MPa，延伸率为0.5％；T5态的室温拉伸屈服强度高达410MPa，抗拉强度为418MPa，延伸率为0.3％。
实施例4
本实施例提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，具体采用以下步骤：
1)通过气雾化的方法制备出Mg-14.92Gd-0.30Zr(wt.％)合金粉末，并对合金粉末进行筛分，选用200～300目(平均粒径为61μm)的粉末进行选区激光熔化成型。
2)将粉末在真空干燥箱中进100℃/1h的干燥处理后装入选区激光熔化设备的粉床内，并预热基板到180℃，通入保护气体氩气进行气体循环，待成型舱室内氧和水蒸气含量低于100ppm开始进行选区激光熔化成型。
3)选区激光熔化成型采用的激光功率为120W，扫描速度为300mm/s，扫描间距为100μm，光斑直径为90μm，层厚为30μm，层间转角为71°，扫描策略为分区岛状扫描策略，分区宽度为6mm，不同分区之间的搭接区宽度为0.2mm。
4)将上述3)制备的SLM态镁合金进行T4处理：在空气电阻炉中进行，并放入硫铁矿以热分解释放出的SO 2气体对合金加以阻燃保护，采取单步固溶处理:520℃下固溶0.5h，随后在20℃冷水中淬火。
5)将上述4)制备的T4态镁合金在恒温油浴炉中进行人工时效T6处理，采取单步时效处理：时效温度为200℃，时间为64h，随后在20℃冷水中淬火。
6)将上述3)制备的SLM态镁合金进行T5处理：在恒温油浴炉中进行，采取单步时效处理：时效温度为200℃，时间为64h，随后在20℃冷水中淬火。
7)将上述3)、4)、5)、6)制备的SLM态、T4态、T6态、T5态镁合金进行室温拉伸实验，拉伸机为Zwick BTC—Z100型电子万能材料试验机，拉伸测试速率为0.5mm/min。
所得合金SLM态的组织呈现典型的快速凝固的特点，ɑ-Mg基体晶粒细小均匀(1～3μm)、晶界β相含量少且细小弥散分布。SLM态的室温拉伸屈服强度为245MPa，抗拉强度为246MPa，延伸率为0.1％；T6态的室温拉伸屈服强度高达296MPa，抗拉强 度为365MPa，延伸率为0.4％；T5态的室温拉伸屈服强度高达302MPa，抗拉强度为363MPa，延伸率为0.3％。
实施例5
本实施例提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，具体采用以下步骤：
1)通过气雾化的方法制备出Mg-14.24Gd-0.76Zn-0.32Zr(wt.％)合金粉末，并对合金粉末进行筛分，选用200～300目(平均粒径为61μm)的粉末进行选区激光熔化成型。
2)将粉末在真空干燥箱中进100℃/4h的干燥处理后装入选区激光熔化设备的粉床内，并预热基板到130℃，通入保护气体氩气进行气体循环，待成型舱室内氧和水蒸气含量低于100ppm开始进行选区激光熔化成型。
3)选区激光熔化成型采用的激光功率为160W，扫描速度为700mm/s，扫描间距为70μm，光斑直径为100μm，层厚为20μm，层间转角为74°，扫描策略为分区岛状扫描策略，分区宽度为4mm，不同分区之间的搭接区宽度为0.2mm。
4)将上述3)制备的SLM态镁合金进行T4处理：在空气电阻炉中进行，并放入硫铁矿以热分解释放出的SO 2气体对合金加以阻燃保护，采取单步固溶处理:520℃下固溶2h，随后在20℃冷水中淬火。
5)将上述4)制备的T4态镁合金在恒温油浴炉中进行人工时效T6处理，采取单步时效处理：时效温度为200℃，时间为64h，随后在20℃冷水中淬火。
6)将上述3)制备的SLM态镁合金进行T5处理：在恒温油浴炉中进行，采取单步时效处理：时效温度为200℃，时间为64h，随后在20℃冷水中淬火。
7)将上述3)、4)、5)、6)制备的SLM态、T4态、T6态、T5态镁合金进行室温拉伸实验，拉伸机为Zwick BTC—Z100型电子万能材料试验机，拉伸测试速率为0.5mm/min。
所得合金SLM态的组织呈现典型的快速凝固的特点，ɑ-Mg基体晶粒细小均匀(1～3μm)、晶界β相含量少且细小弥散分布。SLM态的室温拉伸屈服强度为353MPa，抗拉强度为388MPa，延伸率为1.4％；T6态的室温拉伸屈服强度高达315MPa，抗拉强度为393MPa，延伸率为3.0％；T5态的室温拉伸屈服强度高达374MPa，抗拉强度为396MPa，延伸率为0.9％。
实施例6
本实施例提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，具 体采用以下步骤：
1)通过气雾化的方法制备出Mg-10.02Gd-0.18Zn-0.34Zr(wt.％)合金粉末，并对合金粉末进行筛分，选用200～300目(平均粒径为61μm)的粉末进行选区激光熔化成型。
2)将粉末在真空干燥箱中进100℃/5h的干燥处理后装入选区激光熔化设备的粉床内，并预热基板到170℃，通入保护气体氩气进行气体循环，待成型舱室内氧和水蒸气含量低于100ppm开始进行选区激光熔化成型。
3)选区激光熔化成型采用的激光功率为80W，扫描速度为350mm/s，扫描间距为90μm，光斑直径为100μm，层厚为30μm，层间转角为73°，扫描策略为分区岛状扫描策略，分区宽度为6mm，不同分区之间的搭接区宽度为0.3mm。
4)将上述3)制备的SLM态镁合金进行T4处理：在空气电阻炉中进行，并放入硫铁矿以热分解释放出的SO 2气体对合金加以阻燃保护，采取单步固溶处理:450℃下固溶1h，随后在20℃冷水中淬火。
5)将上述4)制备的T4态镁合金在恒温油浴炉中进行人工时效T6处理，采取单步时效处理：时效温度为175℃，时间为128h，随后在20℃冷水中淬火。
6)将上述3)制备的SLM态镁合金进行T5处理：在恒温油浴炉中进行，采取单步时效处理：时效温度为175℃，时间为128h，随后在20℃冷水中淬火。
7)将上述3)、4)、5)、6)制备的SLM态、T4态、T6态、T5态镁合金进行室温拉伸实验，拉伸机为Zwick BTC—Z100型电子万能材料试验机，拉伸测试速率为0.5mm/min。
所得合金SLM态的组织呈现典型的快速凝固的特点，ɑ-Mg基体晶粒细小均匀(1～3μm)、晶界β相含量少且细小弥散分布。SLM态的室温拉伸屈服强度为194MPa，抗拉强度为253MPa，延伸率为6.2％；T6态的室温拉伸屈服强度高达217MPa，抗拉强度为298MPa，延伸率为4.5％；T5态的室温拉伸屈服强度高达243MPa，抗拉强度为306MPa，延伸率为3.4％。
实施例7
本实施例提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，具体采用以下步骤：
1)通过气雾化的方法制备出Mg-10.08Gd-0.37Zr(wt.％)合金粉末，并对合金粉末进行筛分，选用500目以上(平均粒径为34μm)的粉末进行选区激光熔化成型。
2)将粉末在真空干燥箱中进100℃/3h的干燥处理后装入选区激光熔化设备的粉床 内，不预热基板使基板保持室温25℃，通入保护气体氩气进行气体循环，待成型舱室内氧和水蒸气含量低于100ppm开始进行选区激光熔化成型。
3)选区激光熔化成型采用的激光功率为80W，扫描速度为800mm/s，扫描间距为100μm，光斑直径为150μm，层厚为40μm，层间转角为74°，扫描策略为分区岛状扫描策略，分区宽度为6mm，不同分区之间的搭接区宽度为0.3mm。
4)将上述3)制备的SLM态镁合金进行T4处理：在空气电阻炉中进行，并放入硫铁矿以热分解释放出的SO 2气体对合金加以阻燃保护，采取单步固溶处理:450℃下固溶1h，随后在20℃冷水中淬火。
5)将上述4)制备的T4态镁合金在恒温油浴炉中进行人工时效T6处理，采取单步时效处理：时效温度为175℃，时间为128h，随后在20℃冷水中淬火。
6)将上述3)制备的SLM态镁合金进行T5处理：在恒温油浴炉中进行，采取单步时效处理：时效温度为175℃，时间为128h，随后在20℃冷水中淬火。
7)将上述3)、4)、5)、6)制备的SLM态、T4态、T6态、T5态镁合金进行室温拉伸实验，拉伸机为Zwick BTC—Z100型电子万能材料试验机，拉伸测试速率为0.5mm/min。
所得合金SLM态的组织呈现典型的快速凝固的特点，ɑ-Mg基体晶粒细小均匀(1～3μm)、晶界β相含量少且细小弥散分布。SLM态的室温拉伸屈服强度为187MPa，抗拉强度为243MPa，延伸率为5.7％；T6态的室温拉伸屈服强度高达208MPa，抗拉强度为285MPa，延伸率为4.3％；T5态的室温拉伸屈服强度高达235MPa，抗拉强度为297MPa，延伸率为3.1％。
实施例8
本实施例提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，具体采用以下步骤：
1)通过气雾化的方法制备出Mg-10Gd-3Y-1Zn-0.40Zr(wt.％)合金粉末，并对合金粉末进行筛分，选用300～500目(平均粒径为42μm)的粉末进行选区激光熔化成型。
2)将粉末在真空干燥箱中进150℃/3h的干燥处理后装入选区激光熔化设备的粉床内，并预热基板到200℃，通入保护气体氩气进行气体循环，待成型舱室内氧和水蒸气含量低于100ppm开始进行选区激光熔化成型。
3)选区激光熔化成型采用的激光功率为80W，扫描速度为300mm/s，扫描间距为100μm，光斑直径为90μm，层厚为20μm，层间转角为71°，扫描策略为分区岛状扫描 策略，分区宽度为3mm，不同分区之间的搭接区宽度为0.1mm。
4)将上述3)制备的SLM态镁合金进行T4处理：在空气电阻炉中进行，并放入硫铁矿以热分解释放出的SO 2气体对合金加以阻燃保护，采取单步固溶处理:500℃下固溶2h，随后在20℃冷水中淬火。
5)将上述4)制备的T4态镁合金在恒温油浴炉中进行人工时效T6处理，采取单步时效处理：时效温度为225℃，时间为64h，随后在20℃冷水中淬火。
6)将上述3)制备的SLM态镁合金进行T5处理：在恒温油浴炉中进行，采取单步时效处理：时效温度为225℃，时间为64h，随后在20℃冷水中淬火。
7)将上述3)、4)、5)、6)制备的SLM态、T4态、T6态、T5态镁合金进行室温拉伸实验，拉伸机为Zwick BTC—Z100型电子万能材料试验机，拉伸测试速率为0.5mm/min。
所得SLM态合金呈现典型的快速凝固细小晶粒的特点，ɑ-Mg基体晶粒细小均匀(1～3μm)、晶界β相含量少且细小弥散分布。SLM态的室温拉伸屈服强度为356MPa，抗拉强度为389MPa，延伸率为3.9％；T6态的室温拉伸屈服强度高达367MPa，抗拉强度为423MPa，延伸率为4.7％；T5态的室温拉伸屈服强度高达411MPa，抗拉强度为432MPa，延伸率为1.8％。
对比例1
本对比例提供了一种重力铸造制备的镁稀土合金，合金成分与实施例1基本相同，不同之处仅在于：本对比例中，采用的制备方法为重力铸造。
本对比例制备的半连续铸造态Mg-11.16Gd-1.72Zn-0.44Zr(wt.％)合金的OM组织图和SEM组织图如图3所示，晶粒大小约～50μm，晶界β相呈层片状，较为粗大，呈现典型的共晶反应特征。Mg-11.16Gd-1.72Zn-0.44Zr(wt.％)合金不同状态(As-cast、As-cast T6)的室温拉伸性能如图2所示，铸态的室温拉伸屈服强度为163MPa，抗拉强度为210MPa，延伸率为3.6％；进行固溶+时效热处理(480℃-12h+200℃-32h)后，T6态的室温拉伸屈服强度高达186MPa，抗拉强度为258MPa，延伸率为4.6％。无论是铸态还是T6态，重力铸造制备的合金的强度和塑性都低于采用选区激光熔化制备的相同状态的合金。其差别原因在于重力铸造相比于选区激光熔化的冷却速度要小很多，ɑ-Mg基体晶粒和晶界β相粗大。
对比例2
本对比例提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法， 与实施例1基本相同，不同之处仅在于：本对比例中，选区激光熔化成型采用的激光扫描速度为1500mm/s。
SLM态的室温拉伸屈服强度为119MPa，抗拉强度为122MPa，延伸率为0.3％，强度和塑性都显著低于实施例1制备的SLM态合金。其差别原因在于激光扫描速度过大导致激光作用时间过短，激光能量密度低不足以完全熔化所有的粉末，产生大量未熔合缺陷。
对比例3
本对比例提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，与实施例1基本相同，不同之处仅在于：本对比例中，选区激光熔化成型采用的激光扫描间距为150μm。
SLM态的室温拉伸屈服强度为204MPa，抗拉强度为221MPa，延伸率为1.3％，强度和塑性都显著低于实施例1制备的SLM态合金。其差别原因在于激光扫描间距过大导致扫描道之间搭接不上，扫描道的搭接区域存在大量未熔合缺陷。
对比例4
本对比例提供了一种重力铸造制备的镁稀土合金，合金成分与实施例2基本相同，不同之处仅在于：本对比例中，采用的制备方法为重力铸造。
铸态的室温拉伸屈服强度为169MPa，抗拉强度为251MPa，延伸率为5.7％；进行固溶+时效热处理(520℃-12h+200℃-64h)后，T6态的室温拉伸屈服强度高达232MPa，抗拉强度为296MPa，延伸率为0.6％。无论是铸态还是T6态，重力铸造制备的合金的强度都低于采用选区激光熔化制备的相同状态的合金但塑性。其差别原因在于重力铸造相比于选区激光熔化的冷却速度要小很多，ɑ-Mg基体晶粒和晶界β相粗大。
对比例5
本对比例提供了一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，与实施例2基本相同，不同之处仅在于：本对比例中，选区激光熔化成型采用的激光功率为40W。
成型过程中粉末发生严重的球化现象，零件发生翘曲导致破坏铺粉刮刀使成型实验被迫停止，相邻打印层之间未能实现冶金结合导致成型零件基本没有结合强度。其差别原因在于激光功率过低无法完全熔透粉末，粉末只是部分熔化，粉末与粉末之间未发生冶金结合。
以上对本发明的具体实施例进行了描述。需要理解的是，本发明并不局限于上述特 定实施方式，本领域技术人员可以在权利要求的范围内做出各种变化或修改，这并不影响本发明的实质内容。在不冲突的情况下，本申请的实施例和实施例中的特征可以任意相互组合。

Claims (10)

  1. 一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，其特征在于，所述方法包含如下步骤：
    A、通过气雾化的方法制备出Mg-RE-(Zn)-Zr合金球形粉末；
    B、将Mg-RE-(Zn)-Zr合金球形粉末进行选区激光熔化成型得到高强韧镁稀土合金；
    C、将步骤B制得的镁稀土合金进行热处理：固溶+时效处理或直接进行时效处理，即可。
  2. 根据权利要求1所述的一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，其特征在于：步骤A中，所述Mg-RE-(Zn)-Zr合金球形粉末中包含如下重量百分数的各元素：RE10～20％、Zn0～2％、Zr0～0.5％、余量为Mg和不可避免的杂质，其中杂质的总量小于0.02％；所述RE包括Gd。
  3. 根据权利要求1所述的一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，其特征在于：步骤B中，选用200～300目、300～500目或500目以上的Mg-RE-(Zn)-Zr合金球形粉末进行选区激光熔化成型。
  4. 根据权利要求1所述的一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，其特征在于：步骤B中，所述Mg-RE-(Zn)-Zr合金球形粉末进行选区激光熔化成型之前先在100～200℃下干燥处理1～5h。
  5. 根据权利要求1所述的一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，其特征在于：步骤B中，所述选区激光熔化成型采用的激光相关参数如下：激光功率为80～160W，扫描速度为100～1000mm/s，扫描间距为50～100μm，光斑直径为65～150μm。
  6. 根据权利要求1所述的一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，其特征在于：步骤B中，所述选区激光熔化成型采用的激光扫描策略如下：分区岛状扫描策略，分区宽度为3～6mm，不同分区之间的搭接区宽度为0.1～0.3mm，层间转角为70～75°。
  7. 根据权利要求1所述的一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，其特征在于：步骤B中，所述选区激光熔化成型采用的其他工艺参数如下：层厚为20～40μm，基板预热温度为25～200℃。
  8. 根据权利要求1所述的一种选区激光熔化增材制造技术制备高强韧镁稀土合金 的方法，其特征在于：步骤B中，所述选区激光熔化成型在惰性气体氩气保护下进行，成型过程中成型舱室内氧和水蒸气含量均低于100ppm。
  9. 根据权利要求1所述的一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，其特征在于：步骤C中，所述固溶处理的温度为450～520℃，时间为15min～2h。
  10. 根据权利要求1所述的一种选区激光熔化增材制造技术制备高强韧镁稀土合金的方法，其特征在于：步骤C中，所述时效处理的温度为175～225℃，时间为0～512h。
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