CN113528916A - Rare earth-containing heat-resistant high-strength magnesium alloy material and preparation method thereof - Google Patents

Rare earth-containing heat-resistant high-strength magnesium alloy material and preparation method thereof Download PDF

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CN113528916A
CN113528916A CN202110826588.6A CN202110826588A CN113528916A CN 113528916 A CN113528916 A CN 113528916A CN 202110826588 A CN202110826588 A CN 202110826588A CN 113528916 A CN113528916 A CN 113528916A
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magnesium alloy
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CN113528916B (en
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吴玉娟
薛艳婷
邓庆琛
武千业
陈凯
常治宇
宿宁
彭立明
丁文江
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Shanghai Jiaotong University
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    • C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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Abstract

The invention provides a rare earth-containing heat-resistant high-strength magnesium alloy material and a preparation method thereof, belonging to the technical field of magnesium alloy. The preparation method comprises the following steps: A. coating the heat-resistant enhanced phase powder on the surface of the rare earth magnesium alloy powder through mechanical modification and fusion treatment; B. b, drying the powder treated in the step A; C. carrying out selective laser melting molding on the dried powder to obtain SLM-state magnesium alloy; the heat-resistant reinforcing phase is at least one of Mo, V, Sm, Sn and Nb. The invention utilizes mechanical fusion modification treatment to coat a layer of heat-resistant reinforcing phase powder on the surface of magnesium alloy powder and uses SLM technology to prepare the high-strength heat-resistant magnesium alloy. The invention can uniformly distribute the nanoscale heat-resistant reinforcing phase on the surface of the magnesium alloy substrate, effectively solves the bottleneck problems of easy softening and low tensile strength of the magnesium alloy in the high-temperature stretching process, and expands the application field of the heat-resistant magnesium alloy under the high-temperature service condition.

Description

Rare earth-containing heat-resistant high-strength magnesium alloy material and preparation method thereof
Technical Field
The invention belongs to the technical field of alloy material preparation, and particularly relates to a rare earth-containing heat-resistant high-strength magnesium alloy material and a preparation method thereof.
Background
The magnesium alloy is a metal structure material with the lowest density, has higher specific strength and specific stiffness, is rich in resource reserves, low in price and wider in application range, and has been successfully applied to the fields of aerospace, traffic, communication and the like so far. With the increasingly tense international energy problem, the concept of environmental protection is in depth, and the recyclable characteristic and the light weight and high strength characteristic of the magnesium alloy greatly meet the light weight requirement of structural materials, so the magnesium alloy is called as green engineering materials in the 21 st century.
The magnesium alloy is divided into the magnesium alloy used below 120 ℃ and the magnesium alloy used above 120 ℃ according to the heat resistance, the magnesium alloy used above 120 ℃ is generally Mg-RE alloy, but the service temperature of the existing heat-resistant magnesium alloy such as QE22, EQ21, WE54 and WE43 is generally not higher than 250 ℃.
With the development of aerospace, the requirement on the heat-resistant temperature of the magnesium alloy is further improved, and the performance of the heat-resistant magnesium alloy is further required. In order to improve the high-temperature performance of the magnesium alloy and expand the application range of the magnesium alloy, the common practice at present is to add a heat-resistant reinforcing phase into the magnesium alloy, but when the heat-resistant reinforcing phase is added into the magnesium alloy through the traditional casting process, the heat-resistant reinforcing phase is difficult to be uniformly distributed in a magnesium alloy matrix, so that segregation is easily caused (even the problem that the heat-resistant phase cannot be added into the alloy is solved), the heat-resistant reinforcing phase which is not uniformly distributed can become a tensile crack source of the magnesium alloy, and the room-temperature and high-temperature mechanical properties of the magnesium alloy are greatly reduced.
At present, the emergence of selective laser melting molding (SLM) provides a new idea and method for adding a heat-resistant reinforcing phase in magnesium alloy.
The SLM uses laser as an energy source, and is sintered in a specific area of a material through computer program control, and parts are formed by overlapping layer by layer; the selective laser melting technology takes a high-power and fine-spot laser beam as a heat source and has the intrinsic forming characteristic of point-line-surface-body, so that the selective laser melting has the characteristic of finely forming metal parts with complex structures. In addition, the high-power laser beam provided by the SLM can completely melt powder particles, the material melt can be uniformly combined with the matrix, and gaps existing in the forming process are fully filled, so that a sample prepared by the SLM has higher compactness.
SLM (selective laser melting) is also more and more important for preparing composite materials, but the simple mechanical mixing of powder easily causes uneven distribution of an addition phase in a matrix, has a local agglomeration phenomenon and has adverse effects on material properties. The mixing by ball milling can narrow the particle size range to some extent, but the problem of individual large particles still remains.
In patent document CN110681869A in the past by the inventor, a method for preparing a high-toughness magnesium rare earth alloy by a selective laser melting additive manufacturing technology is described, but the magnesium alloy prepared by the method is used in a room temperature environment, and has a defect in performance at a high temperature of 300 ℃.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a rare earth-containing heat-resistant high-strength magnesium alloy material and a preparation method thereof. The preparation method comprises the steps of coating a layer of nanoscale heat-resistant strengthening phase powder on the surface of a matrix by adopting a coating process of a mechanical modification fusion method, and then preparing the heat-resistant high-strength rare earth magnesium alloy by adopting an SLM (selective laser melting) process.
The purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of a rare earth-containing heat-resistant high-strength magnesium alloy, which comprises the following steps:
A. coating the heat-resistant enhanced phase powder on the surface of the rare earth magnesium alloy powder through mechanical modification and fusion treatment;
B. b, drying the powder treated in the step A to remove residual moisture in the powder;
C. carrying out selective laser melting molding on the dried powder to obtain SLM-state magnesium alloy;
in the step A, the heat-resistant reinforcing phase is at least one of Mo, V, Sm, Sn and Nb;
the mechanical modification fusion treatment adopts the following specific parameters: the power is 1.8-2 kw, the current is 9.5-9.7A, the rotating speed is 1300-1600 rpm, and the processing time is 15-18 min.
Preferably, in the step a, the alloy composition of the rare earth magnesium alloy powder includes the following components by mass percent: gd: 6-15 wt.%; y: 0-5 wt.%; zn: 0-3 wt.%; mn: 0-1 wt.%; zr: 0-1 wt.%; the balance being Mg and unavoidable impurities; the rare earth magnesium alloy powder is prepared by a gas atomization method;
in the rare earth heat-resistant high-strength magnesium alloy, the content of a heat-resistant reinforcing phase is 0.2-10 wt.%; the heat-resistant reinforcing phase powder is nanoscale powder.
More preferably, the heat-resistant reinforcing phase is contained in the rare earth heat-resistant high-strength magnesium alloy in an amount of 1 to 5 wt.%, and most preferably in an amount of 2.5 to 5 wt.%.
Preferably, the heat-resistant reinforcing phase Mo has a relatively high melting point, and it is relatively easy to prepare a nano-sized powder.
Preferably, in the step B, the drying treatment is carried out under vacuum, the drying temperature is 100-300 ℃, and the drying time is 1-3 hours.
Preferably, in step C, before the powder is subjected to selective laser melting molding, inert gas is introduced to keep the oxygen content in the molding chamber below 100 ppm. More preferably, the inert gas is argon.
Preferably, in the step C, the substrate needs to be preheated before the selective laser melting molding; the preheating temperature is 50-400 ℃.
Preferably, in the step C, the dried powder is firstly added into a powder bed, and the height of the powder bed is adjusted after compaction treatment, so that powder paving treatment in the subsequent selective laser melting forming process is facilitated.
Preferably, in step C, the printing parameters for performing the selective laser melting molding are as follows: the power is 80-160 w, the scanning distance is 50-100 μm, and the scanning speed is 400-1000 mm/s.
Preferably, in the step C, the laser scanning strategy adopted for the selective laser melting molding is a belt scanning strategy, the belt width is 4-8mm, and the interlayer rotation angle is 85-90 °.
Preferably, after the step C, the method further comprises the step of carrying out solid solution treatment and aging treatment on the magnesium alloy in the SLM state.
Preferably, the conditions of the solution treatment are: the solid solution temperature is 400-520 ℃, and the time is 1-6 h; quenching after the solution treatment, wherein the quenching temperature is 25-80 ℃;
the aging treatment conditions are as follows: the aging temperature is 150-225 ℃, and the time is 32-256 h.
The invention also provides a rare earth-containing heat-resistant high-strength magnesium alloy prepared by the method, which comprises the following components in percentage by mass: gd: 6-15 wt.%; y: 0-5 wt.%; zn: 0-3 wt.%; mn: 0-1 wt.%; zr: 0-1 wt.%; heat resistant reinforcing phase: 0.2-10 wt.%; the balance being Mg and unavoidable impurities; the heat-resistant reinforcing phase is at least one of Mo, V, Sm, Sn and Nb.
Compared with the prior art, the invention has the following beneficial effects:
1. the rare earth-containing heat-resistant high-strength magnesium alloy prepared by the invention can realize that the nanoscale heat-resistant reinforcing phase is uniformly coated on the surface of the rare earth magnesium alloy powder by utilizing the mechanical modification fusion machine, can be uniformly distributed in an alloy matrix in the selective laser melting forming process, and can play an effective high-temperature reinforcing effect.
2. The invention adopts the selective laser melting technology to form the parts with any complex shape, and has short forming period and good product stability.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a morphology chart of a magnesium alloy prepared in example 1 of the present invention; wherein FIG. 1(a) is an SLM-state magnesium alloy, and FIG. 1(b) is an SLM-T4-state magnesium alloy;
FIG. 2 is an SEM topography of an SLM magnesium alloy prepared by comparative example 1 of the present invention.
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 provides a rare earth-containing heat-resistant high-strength magnesium alloy and a preparation method thereof, and the method specifically comprises the following steps:
1) the rare earth-containing heat-resistant high-strength magnesium alloy consists of the following components in percentage by mass: gd: 10 wt.%; y: 3 wt.%; zn: 1 wt.%; mn: 0.4 wt.%, heat resistant reinforcing phase Mo: 5 wt.%; the balance being Mg and unavoidable impurities.
2) Preparing Mg-10Gd-3Y-1Zn-0.4Mn (wt.%) alloy powder by a conventional gas atomization method;
3) the method for preparing the mixed powder of Mg-10Gd-3Y-1Zn-0.4Mn (wt.%) and nano-grade Mo by utilizing mechanical modification fusion comprises the following specific steps: wrapping 5 wt.% of nano-grade Mo powder on the surface of Mg-10Gd-3Y-1Zn-0.4Mn (wt.%) magnesium alloy powder by using a mechanical modification fusion machine (model is NOB130), wherein the power of the mechanical modification fusion machine is 1.8kw, the current is 9.5A, the rotating speed is 1300rpm, and the powder mixing time is 18 min;
4) drying the mixed powder prepared in the step 3) at 100 ℃ for 3 h; transferring the cooled powder into a powder bed, and introducing Ar gas into an SLM (selective laser melting) chamber for protection until the oxygen content is reduced to 100 ppm;
5) the substrate is preheated to 200 ℃ and then begins to be printed, the laser power adopted by selective laser melting molding is 160W, the scanning speed is 1000mm/s, the scanning interval is 50 mu m, the scanning strategy is a belt-shaped scanning strategy, the width of each belt is 4mm, and the interlayer rotation angle is 85 degrees;
6) subjecting the SLM-state magnesium alloy prepared in the step 5) to solution treatment (T4 treatment): the method is carried out in an air resistance furnace, and adopts a single-step solution treatment: dissolving in water at 500 deg.C for 2 hr, and quenching in warm water at 50 deg.C;
7) further aging treatment (T6 treatment) is carried out on the SLM-T4 state magnesium alloy obtained in the step 6): carrying out aging treatment in an oil bath pan: aging at 175 deg.C for 64 h. Thus obtaining the rare earth-containing heat-resistant high-strength magnesium alloy Mg-10Gd-3Y-1Zn-0.4Mn-5Mo (wt.%).
The structure of the SLM-state magnesium alloy prepared in the above step 5) is shown in fig. 1 (a): the typical rapid solidification characteristic is presented, the crystal grains are fine and uniform, and the nano-grade Mo powder is uniformly distributed in the matrix without obvious agglomeration. The structure of the SLM-T4 state magnesium alloy prepared by the step 6) treatment is shown in figure 1 (b): after the treatment of T4, the boundary of the molten pool disappears, namely, the fine columnar crystal growing vertically along the molten pool is converted into fine isometric crystal by the treatment of T4.
The tensile strength of the SLM-state magnesium alloy at the high temperature of 300 ℃ is 203MPa, and the elongation is 12.8%. After T4 treatment, the tensile strength at 300 ℃ is 252MPa, and the elongation is 6.7%. After T6 treatment, the tensile strength at 300 ℃ is 307MPa, and the elongation is 6%.
Example 2:
the embodiment provides a rare earth-containing heat-resistant high-strength magnesium alloy and a preparation method thereof, and the method specifically comprises the following steps:
1) the rare earth-containing heat-resistant high-strength magnesium alloy consists of the following components in percentage by mass: gd: 6 wt.%; heat-resistant reinforcing phase V: 0.2 wt.%; the balance being Mg and unavoidable impurities.
2) Preparing Mg-6Gd (wt.%) alloy powder by a conventional gas atomization method;
3) preparing mixed powder of Mg-6Gd (wt.%) and nano-grade V by using mechanical modification fusion, which comprises the following steps: wrapping 0.2 wt.% of nano-grade V powder on the surface of Mg-6Gd (wt.%) alloy powder by using a mechanical modification fusion machine (model is NOB130), wherein the power of the mechanical modification fusion machine is 2kw, the current is 9.7A, the rotating speed is 1600rpm, and the powder mixing time is 15 min;
4) drying the prepared mixed powder at 200 ℃ for 1 h; transferring the cooled powder into a powder bed, and introducing Ar gas into an SLM (selective laser melting) chamber for protection until the oxygen content is reduced to 100 ppm;
5) the substrate is preheated to 50 ℃ and then begins to be printed, the laser power adopted by selective laser melting molding is 80W, the scanning speed is 400mm/s, the distance between melting pools is 100 mu m, the scanning strategy is a belt-shaped scanning strategy, the width of each belt is 8mm, and the rotation angle between layers is 90 degrees;
6) subjecting the SLM-state magnesium alloy prepared in the step 5) to solution treatment (T4 treatment): the method is carried out in an air resistance furnace, and adopts a single-step solution treatment: dissolving in water at 400 deg.C for 6 hr, and quenching in 25 deg.C warm water;
7) further aging treatment (T6 treatment) is carried out on the SLM-T4 state magnesium alloy obtained in the step 6): carrying out aging treatment in an oil bath pan: aging at 200 deg.C for 64 h. The rare earth-containing heat-resistant high-strength magnesium alloy Mg-6Gd-0.2Mo (wt.%) is prepared.
The SLM-state magnesium alloy prepared in the step 5) has tensile strength of 151MPa at a high temperature of 300 ℃ and elongation of 8%. After T4 treatment, the tensile strength at 300 ℃ is 213MPa, and the elongation is 3.4%. After T6 treatment, the tensile strength at 300 ℃ is 263MPa, and the elongation is 3.1%.
Example 3:
the embodiment provides a rare earth-containing heat-resistant high-strength magnesium alloy and a preparation method thereof, and the method specifically comprises the following steps:
1) the rare earth-containing heat-resistant high-strength magnesium alloy consists of the following components in percentage by mass: gd: 15 wt.%; y: 5 wt.%; zn: 3 wt.%; mn: 1 wt.%, heat-resistant reinforcing phase Sm: 10 wt.%; the balance being Mg and unavoidable impurities.
2) Preparing Mg-15Gd-5Y-3Zn-1Mn (wt.%) alloy powder by a conventional gas atomization method;
3) the method for preparing the mixed powder of Mg-15Gd-5Y-3Zn-1Mn (wt.%) and nanoscale Sm by utilizing mechanical modification fusion comprises the following specific steps: wrapping 10 wt.% of nano-scale Sm powder on the surface of Mg-15Gd-5Y-3Zn-1Mn (wt.%) alloy powder by using a mechanical modification fusion machine (model is NOB130), wherein the power of the mechanical modification fusion machine is 1.9kw, the current is 9.6A, the rotating speed is 1500rpm, and the powder mixing time is 16 min;
4) drying the prepared mixed powder at 150 ℃ for 2 h; transferring the cooled powder into a powder bed, and introducing Ar gas into an SLM (selective laser melting) chamber for protection until the oxygen content is reduced to 100 ppm;
5) the substrate is preheated to 100 ℃ and then begins to be printed, the laser power adopted by selective laser melting molding is 100W, the scanning speed is 600mm/s, the distance between melting pools is 50 mu m, the scanning strategy is a belt-shaped scanning strategy, the width of each belt is 6mm, and the rotation angle between layers is 88 degrees;
6) subjecting the SLM-state magnesium alloy prepared in the step 5) to solution treatment (T4 treatment): the method is carried out in an air resistance furnace, and adopts a single-step solution treatment: dissolving in water at 520 deg.C for 2 hr, and quenching in 80 deg.C warm water;
7) further aging treatment (T6 treatment) is carried out on the SLM-T4 state magnesium alloy obtained in the step 6): carrying out aging treatment in an oil bath pan: aging at 150 deg.C for 128 h. Thus obtaining the rare earth-containing heat-resistant high-strength magnesium alloy Mg-15Gd-5Y-3Zn-1Mn-10Mo (wt.%).
The SLM-state magnesium alloy prepared in the step 5) has the tensile strength of 164MPa at the high temperature of 300 ℃ and the elongation of 19.1%. After T4 treatment, the tensile strength at 300 ℃ is 217MPa, and the elongation is 7.9%. After T6 treatment, the tensile strength at 300 ℃ is 252MPa, and the elongation is 6.5%.
Example 4:
the embodiment provides a rare earth-containing heat-resistant high-strength magnesium alloy and a preparation method thereof, and the method specifically comprises the following steps:
1) the rare earth-containing heat-resistant high-strength magnesium alloy consists of the following components in percentage by mass: gd: 8 wt.%; y: 3 wt.%; zn: 1 wt.%; zr: 0.5 wt.%, heat resistant additive phase Sn: 2.5 wt.%; the balance being Mg and unavoidable impurities.
2) Preparing Mg-8Gd-3Y-1Zn-0.5Zr (wt.%) alloy powder by a conventional gas atomization method;
3) preparing mixed powder of Mg-8Gd-3Y-1Zn-0.5Zr (wt.%) and nanoscale Sn by utilizing mechanical modification fusion, and specifically comprising the following steps: wrapping 2.5 wt.% of nano-grade Sn powder on the surface of Mg-8Gd-3Y-1Zn-0.5Zr (wt.%) alloy powder by using a mechanical modification fusion machine (model is NOB130), wherein the power of the mechanical modification fusion machine is 1.8kw, the current is 9.6A, the rotating speed is 1400rpm, and the powder mixing time is 17 min;
4) drying the prepared mixed powder at 300 ℃ for 1 h; transferring the cooled powder into a powder bed, and introducing Ar gas into an SLM (selective laser melting) chamber for protection until the oxygen content is reduced to 100 ppm;
5) the substrate is preheated to 150 ℃ and then begins to be printed, the laser power adopted by selective laser melting molding is 80W, the scanning speed is 800mm/s, the distance between melting pools is 100 mu m, the scanning strategy is a belt-shaped scanning strategy, the width of each belt is 7mm, and the rotation angle between layers is 89 degrees;
6) subjecting the SLM-state magnesium alloy prepared in the step 5) to solution treatment (T4 treatment): the method is carried out in an air resistance furnace, and adopts a single-step solution treatment: dissolving in water at 480 deg.C for 1 hr, and quenching in 35 deg.C warm water;
7) further aging treatment (T6 treatment) is carried out on the SLM-T4 state magnesium alloy obtained in the step 6): carrying out aging treatment in an oil bath pan: aging at 225 deg.C for 32 h. Thus obtaining the rare earth-containing heat-resistant high-strength magnesium alloy Mg-8Gd-3Y-1Zn-0.5Zr-2.5Sn (wt.%).
The SLM-state magnesium alloy prepared in the step 5) has the tensile strength of 159MPa at the high temperature of 300 ℃ and the elongation of 17.5%. After T4 treatment, the tensile strength at 300 ℃ is 196MPa, and the elongation is 8.9%. After T6 treatment, the tensile strength at 300 ℃ is 250MPa, and the elongation is 7.8%.
Example 5:
the embodiment provides a rare earth-containing heat-resistant high-strength magnesium alloy and a preparation method thereof, and the method specifically comprises the following steps:
1) the rare earth-containing heat-resistant high-strength magnesium alloy consists of the following components in percentage by mass: gd: 8 wt.%; y: 3 wt.%; zn: 1 wt.%; zr: 1 wt.%, heat resistant additive phase Nb: 2.5 wt.%; the balance being Mg and unavoidable impurities.
2) Preparing Mg-8Gd-3Y-1Zn-1Zr (wt.%) alloy powder by a conventional gas atomization method;
3) preparing mixed powder of Mg-8Gd-3Y-1Zn-1Zr (wt.%) and nano-grade Nb by utilizing mechanical modification fusion, and specifically comprising the following steps: wrapping 2.5 wt.% of nano-scale Nb powder on the surface of Mg-8Gd-3Y-1Zn-1Zr (wt.%) alloy powder by using a mechanical modification fusion machine (model is NOB130), wherein the power of the mechanical modification fusion machine is 1.9kw, the current is 9.5A, the rotating speed is 1400rpm, and the powder mixing time is 18 min;
4) drying the prepared mixed powder at 200 ℃ for 2 h; transferring the cooled powder into a powder bed, and introducing Ar gas into an SLM (selective laser melting) chamber for protection until the oxygen content is reduced to 100 ppm;
5) preheating a substrate to 400 ℃, and then starting printing, wherein the laser power adopted by selective laser melting molding is 120W, the scanning speed is 1000mm/s, the molten pool interval is 75 mu m, the scanning strategy is a belt-shaped scanning strategy, the belt-dividing width is 7mm, and the interlayer rotation angle is 87 degrees;
6) subjecting the SLM-state magnesium alloy prepared in the step 5) to solution treatment (T4 treatment): the method is carried out in an air resistance furnace, and adopts a single-step solution treatment: dissolving in water at 440 deg.C for 4h, and quenching in 65 deg.C warm water;
7) further aging treatment (T6 treatment) is carried out on the SLM-T4 state magnesium alloy obtained in the step 6): carrying out aging treatment in an oil bath pan: aging at 200 deg.C for 256 h. Thus obtaining the rare earth-containing heat-resistant high-strength magnesium alloy Mg-8Gd-3Y-1Zn-1Zr-2.5Nb (wt.%).
The SLM-state magnesium alloy prepared in the step 5) has the tensile strength of 225MPa at the high temperature of 300 ℃ and the elongation of 15.7%. After T4 treatment, the tensile strength at 300 ℃ is 280MPa, and the elongation is 9.8%. After T6 treatment, the tensile strength at 300 ℃ and high temperature is 300MPa, and the elongation is 6.5%.
Example 6:
the embodiment provides a rare earth-containing heat-resistant high-strength magnesium alloy and a preparation method thereof, and the specifically adopted steps are basically the same as those of embodiment 1, except that: in step 3), the present embodiment employs nano-sized Mo with a mass fraction of 1 wt.%.
The SLM-state magnesium alloy prepared in the embodiment has the tensile strength of 180MPa at the high temperature of 300 ℃ and the elongation of 16.9%. After T4 treatment, the tensile strength at 300 ℃ is 230MPa, and the elongation is 13.7%. After T6 treatment, the tensile strength at 300 ℃ is 270MPa, and the elongation is 9.4%.
Example 7:
the embodiment provides a rare earth-containing heat-resistant high-strength magnesium alloy and a preparation method thereof, and the specifically adopted steps are basically the same as those of embodiment 1, except that: in step 3), the present example employs 2.5 wt.% of nano-sized Mo.
The SLM-state magnesium alloy prepared in the embodiment has the tensile strength of 190MPa at the high temperature of 300 ℃ and the elongation of 14.5%. After T4 treatment, the tensile strength at 300 ℃ is 240MPa, and the elongation is 9.7%. After T6 treatment, the tensile strength at 300 ℃ is 285MPa, and the elongation is 7.0%.
Example 8:
the embodiment provides a rare earth-containing heat-resistant high-strength magnesium alloy and a preparation method thereof, and the specifically adopted steps are basically the same as those of embodiment 1, except that: in step 3), the present embodiment employs nanoscale V with a mass fraction of 5 wt.%.
The SLM-state magnesium alloy prepared in the embodiment has a tensile strength of 196MPa and an elongation of 12.7% at a high temperature of 300 ℃. After T4 treatment, the tensile strength at 300 ℃ is 245MPa, and the elongation is 9.9%. After T6 treatment, the tensile strength at 300 ℃ is 295MPa, and the elongation is 6.0%.
Comparative example 1:
this comparative example provides a method of producing a magnesium rare earth alloy using a selective laser melting additive manufacturing technique, substantially the same as example 1, except that: in the comparative example, nano-sized Mo was not added, i.e., the Mg-10Gd-3Y-1Zn-0.4Mn (wt.%) magnesium alloy powder prepared in step 2) was directly subjected to the processes of steps 4) -7), and the printing parameters used were adjusted accordingly according to the actual printing.
The SEM organizational chart of the SLM-state magnesium alloy prepared by the comparative example is shown in FIG. 2, magnesium alloy powder is ablated under the action of laser, obvious holes are left on the surface of the alloy, and the performance of the alloy is greatly influenced; the tensile strength at 300 ℃ and the elongation are 72MPa and 42.1 percent respectively.
Comparative example 2:
this comparative example provides a method for preparing a magnesium rare earth alloy by gravity casting, which is different from example 1 in that: in this comparative example, the preparation method used was gravity casting, and no nano-sized Mo powder was added to the alloy composition.
Compared with the magnesium alloy prepared by SLM, the gravity casting Mg-10Gd-3Y-1Zn-0.4Mn (wt.%) magnesium alloy has larger grain size, and the excessive grain size has adverse effect on the tensile property in the high-temperature stretching process; compared with the SLM preparation method, Mg-10Gd-3Y-1Zn-0.4Mn (wt.%) and Mo powder can be uniformly mixed, and in the gravity casting process, the Mo has high density and cannot be sufficiently mixed with Mg-10Gd-3Y-1Zn-0.4Mn (wt.%) magnesium alloy, so that the Mg-10Gd-3Y-1Zn-0.4Mn (wt.%) + Mo alloy with uniform components cannot be prepared.
The tensile strength of the cast sample is 127MPa and the elongation is 23% at the high temperature of 300 ℃; after the solution treatment (520 ℃ multiplied by 12h), the tensile strength of the T4 state is 172MPa and the elongation is 18.9% at the high temperature of 300 ℃; after solution treatment and aging heat treatment (520 ℃ C.. times.12 h +200 ℃ C.. times.64 h), the tensile strength was 189MPa and the elongation was 21.5% in the T6 state at a high temperature of 300 ℃.
Comparative example 3:
this comparative example provides a method of producing a magnesium rare earth alloy using a selective laser melting additive manufacturing technique, substantially the same as example 1, except that: the added heat-resistant reinforcing phase is Si3N4And the powder is mixed by a common mechanical ball milling method instead of a mechanical modified fusion method.
The tensile strength of the prepared SLM-state magnesium alloy at the high temperature of 300 ℃ is 120MPa, the elongation is 18%, and the tensile strength and the plasticity are both obviously lower than those of the SLM-state magnesium alloy prepared in the embodiment 1. The reason is that Si3N4The powders were not mixed by mechanical modified fusion resulting in Si3N4The powder agglomerates in the matrix, adversely affecting the sample.
Comparative example 4:
this comparative example provides a method of producing a magnesium rare earth alloy using a selective laser melting additive manufacturing technique, substantially the same as example 1, except that: and 3) mixing the nano-grade Mo powder with Mg-10Gd-3Y-1Zn-0.4Mn (wt.%) alloy powder by adopting a ball milling method.
The tensile strength of the prepared SLM-state magnesium alloy at the high temperature of 300 ℃ is 126MPa, the elongation is 18%, and the tensile strength and the plasticity are both obviously lower than those of the SLM-state magnesium alloy prepared in the embodiment 1.
Comparative example 5:
this comparative example provides a method of producing a magnesium rare earth alloy using a selective laser melting additive manufacturing technique, substantially the same as example 1, except that: the power of the mechanical modification fusion machine adopted in the step 3) is 1.5 kw.
The tensile strength of the prepared SLM-state magnesium alloy at the high temperature of 300 ℃ is 176MPa, the elongation is 14%, and the tensile strength and the plasticity are both obviously lower than those of the SLM-state magnesium alloy prepared in the embodiment 1.
Comparative example 6:
this comparative example provides a method of producing a magnesium rare earth alloy using a selective laser melting additive manufacturing technique, substantially the same as example 1, except that: the interlayer rotation angle adopted in the step 5) is 80 degrees.
The tensile strength of the prepared SLM-state magnesium alloy at the high temperature of 300 ℃ is 163MPa, the elongation is 16%, and the tensile strength and the plasticity are both obviously lower than those of the SLM-state magnesium alloy prepared in the embodiment 1.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (10)

1. The preparation method of the rare earth-containing heat-resistant high-strength magnesium alloy is characterized by comprising the following steps of:
A. coating the heat-resistant enhanced phase powder on the surface of the rare earth magnesium alloy powder through mechanical modification and fusion treatment;
B. b, drying the powder treated in the step A;
C. carrying out selective laser melting molding on the dried powder to obtain SLM-state magnesium alloy;
in the step A, the heat-resistant reinforcing phase is at least one of Mo, V, Sm, Sn and Nb;
the mechanical modification fusion treatment adopts the following specific parameters: the power is 1.8-2 kw, the current is 9.5-9.7A, the rotating speed is 1300-1600 rpm, and the processing time is 15-18 min.
2. The method for preparing the rare earth-containing heat-resistant high-strength magnesium alloy as claimed in claim 1, wherein in the step A, the alloy composition of the rare earth-containing magnesium alloy powder comprises the following components in percentage by mass: gd: 6-15 wt.%; y: 0-5 wt.%; zn: 0-3 wt.%; mn: 0-1 wt.%; zr: 0-1 wt.%; the balance being Mg and unavoidable impurities;
in the rare earth heat-resistant high-strength magnesium alloy, the content of a heat-resistant reinforcing phase is 0.2-10 wt.%; the heat-resistant reinforcing phase powder is nanoscale powder.
3. The method for preparing the rare earth-containing heat-resistant high-strength magnesium alloy according to claim 1, wherein in the step B, the drying treatment is performed under vacuum at a temperature of 100-300 ℃ for 1-3 hours.
4. The method for preparing the rare earth-containing heat-resistant high-strength magnesium alloy as claimed in claim 1, wherein in the step C, before the powder is subjected to selective laser melting molding, an inert gas is introduced to keep the oxygen content in the molding chamber below 100 ppm.
5. The method for preparing the rare earth-containing heat-resistant high-strength magnesium alloy as claimed in claim 1, wherein in the step C, the substrate is preheated before the selective laser melting molding; the preheating temperature is 50-400 ℃.
6. The method for preparing the rare earth-containing heat-resistant high-strength magnesium alloy as claimed in claim 1, wherein in the step C, the selective laser melting molding is performed with the following printing parameters: the power is 80-160 w, the scanning distance is 50-100 μm, and the scanning speed is 400-1000 mm/s.
7. The method for preparing the rare earth-containing heat-resistant high-strength magnesium alloy as claimed in claim 1, wherein in the step C, the laser scanning strategy adopted for the selective laser melting forming is a belt scanning strategy, the belt width is 4-8mm, and the interlayer rotation angle is 85-90 °.
8. The method for preparing the rare earth-containing heat-resistant high-strength magnesium alloy as claimed in claim 1, further comprising the step of subjecting the SLM-state magnesium alloy to solution treatment and aging treatment after step C.
9. The method for preparing the rare earth-containing heat-resistant high-strength magnesium alloy as claimed in claim 8, wherein the conditions of the solution treatment are as follows: the solid solution temperature is 400-520 ℃, and the time is 1-6 h; quenching after the solution treatment, wherein the quenching temperature is 25-80 ℃;
the aging treatment conditions are as follows: the aging temperature is 150-225 ℃, and the time is 32-256 h.
10. The rare earth-containing heat-resistant high-strength magnesium alloy prepared by the method according to any one of claims 1 to 9, which is characterized by comprising the following components in percentage by mass: gd: 6-15 wt.%; y: 0-5 wt.%; zn: 0-3 wt.%; mn: 0-1 wt.%; zr: 0-1 wt.%; heat resistant reinforcing phase: 0.2-10 wt.%; the balance being Mg and unavoidable impurities; the heat-resistant reinforcing phase is at least one of Mo, V, Sm, Sn and Nb.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113174519A (en) * 2021-03-23 2021-07-27 山东科技大学 Superfine vanadium particle reinforced fine-grain magnesium-based composite material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003129161A (en) * 2001-08-13 2003-05-08 Honda Motor Co Ltd Heat resistant magnesium alloy
CN110681869A (en) * 2019-10-15 2020-01-14 上海交通大学 Method for preparing high-strength and high-toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology
CN112795818A (en) * 2020-12-30 2021-05-14 上海交通大学 High-strength heat-resistant rare earth aluminum alloy manufactured by laser additive manufacturing and preparation method thereof
CN113073244A (en) * 2021-03-19 2021-07-06 中北大学 High-strength and high-toughness rare earth heat-resistant magnesium alloy and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003129161A (en) * 2001-08-13 2003-05-08 Honda Motor Co Ltd Heat resistant magnesium alloy
CN110681869A (en) * 2019-10-15 2020-01-14 上海交通大学 Method for preparing high-strength and high-toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology
CN112795818A (en) * 2020-12-30 2021-05-14 上海交通大学 High-strength heat-resistant rare earth aluminum alloy manufactured by laser additive manufacturing and preparation method thereof
CN113073244A (en) * 2021-03-19 2021-07-06 中北大学 High-strength and high-toughness rare earth heat-resistant magnesium alloy and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113174519A (en) * 2021-03-23 2021-07-27 山东科技大学 Superfine vanadium particle reinforced fine-grain magnesium-based composite material and preparation method thereof
CN113174519B (en) * 2021-03-23 2022-04-29 山东科技大学 Superfine vanadium particle reinforced fine-grain magnesium-based composite material and preparation method thereof

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