CN116770142A - Preparation method and product of titanium alloy particle reinforced rare earth magnesium-based composite material - Google Patents
Preparation method and product of titanium alloy particle reinforced rare earth magnesium-based composite material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C23/00—Alloys based on magnesium
- C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F3/03—Press-moulding apparatus therefor
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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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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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Abstract
本发明涉及一种钛合金颗粒增强稀土镁基复合材料的制备方法及产品，属于镁合金材料技术领域。该方法具体为：首先将TC4钛合金球形粉末与Mg‑Gd‑Zn‑Zr合金粉末在保护气氛下球磨，获得混合粉末；然后将混合粉末置于模具后热压烧结，获得坯料；最后将坯料固溶、时效处理后冷却至室温，即可。选用TC4颗粒作为增强体，结合热压烧结工艺及热处理工艺，最终制得具有较高的综合力学性能的稀土镁合金。该制备工艺流程简单，能耗更少且生产耗时短，成本低，有利于工业化大规模生产，具有良好的应用前景和经济效益。
The invention relates to a preparation method and product of titanium alloy particle-reinforced rare earth magnesium-based composite materials, and belongs to the technical field of magnesium alloy materials. The specific method is as follows: first, ball-mill TC4 titanium alloy spherical powder and Mg-Gd-Zn-Zr alloy powder under a protective atmosphere to obtain a mixed powder; then place the mixed powder in a mold and hot-press and sinter it to obtain a billet; finally, the billet is After solid solution and aging treatment, it can be cooled to room temperature. Using TC4 particles as reinforcement, combined with hot pressing sintering process and heat treatment process, a rare earth magnesium alloy with high comprehensive mechanical properties is finally produced. The preparation process is simple, consumes less energy, is short in production time, has low cost, is conducive to industrial large-scale production, and has good application prospects and economic benefits.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy materials, and particularly relates to a preparation method and a product of a titanium alloy particle reinforced rare earth magnesium-based composite material.
Background
Magnesium alloy is the lightest metal structural material applicable at present, but compared with metal structural materials such as steel, aluminum alloy and the like, the absolute strength and rigidity of the magnesium alloy are lower, so that the application of the magnesium alloy is limited. Because of the solid solution strengthening and precipitation strengthening effects of rare earth elements, the rare earth magnesium alloy has higher strength than general (AZ series and the like) magnesium alloy, is expected to meet the requirements of aerospace and other fields on high strength and light weight of materials, but the plasticity of the rare earth magnesium alloy can be further improved on the basis of ensuring the strength so as to improve the comprehensive mechanical property of the rare earth magnesium alloy.
The mechanical properties of the material can be further improved by adding second phase particles into the alloy, and the reinforcing phase particles of the second phase which are commonly used at present mainly comprise nonmetallic particles and metal particles, wherein the nonmetallic particles (such as SiC, tiC, al 2 O 3 、TiB 2 、B 4 C. AlN, etc.) can effectively improve the strength and rigidity of the magnesium alloy, but the plasticity is generally poor because the wettability of the ceramic particles and the magnesium matrix is poor, and good interface bonding is difficult to form, so that the stress at the interface is highly concentrated, thereby causing the premature fracture of the material. The metal particles (such as Ti particles) have a crystal structure similar to that of a magnesium matrix, have good wettability, and can coordinate the deformation of the matrix, so that the strength of the material can be improved on the premise of not greatly sacrificing the plasticity. But currently utilize the firstThe research on improving the mechanical properties of the rare earth magnesium alloy by the two-phase particles is relatively less, and the search for the second-phase particles capable of improving the comprehensive mechanical properties of the rare earth magnesium alloy is particularly important.
Disclosure of Invention
In view of the above, one of the objects of the present invention is to provide a method for preparing a titanium alloy particle reinforced rare earth magnesium-based composite material; and the second aim is to provide a titanium alloy particle reinforced rare earth magnesium-based composite material.
In order to achieve the above purpose, the present invention provides the following technical solutions:
1. a preparation method of a titanium alloy particle reinforced rare earth magnesium-based composite material comprises the following steps:
s1, proportioning according to mass percentages: 2-10wt.% of TC4 titanium alloy spherical powder and the balance of Mg-Gd-Zn-Zr alloy powder, and ball milling the TC4 titanium alloy spherical powder and the Mg-Gd-Zn-Zr alloy powder under a protective atmosphere to obtain mixed powder;
s2, placing the mixed powder into a die, and hot-pressing and sintering to obtain a blank;
s3, carrying out solid solution and aging treatment on the blank, and cooling to room temperature.
Preferably, in the step S1, the Mg-Gd-Zn-Zr alloy powder comprises the following components in percentage by mass: 5-15wt.% Gd, 1-2% zn, 0.1-0.5% zr, the balance Mg and unavoidable impurities.
Preferably, in step S1, the ball milling under the protective atmosphere specifically includes: ball milling is carried out for 3-5h at the rotating speed of 50-100rpm according to the ball-material ratio of 5-10:1 under the argon atmosphere.
Preferably, in step S2, the hot press sintering specifically includes: placing the die in a vacuum hot-pressing furnace, vacuumizing to be less than or equal to 20Pa, pre-pressurizing a hot-pressing head to be 5MPa, pressurizing to be 80-100MPa, heating to 390-420 ℃ at the heating rate of 80-100 ℃/min, heating to 485-495 ℃ at the heating rate of 20-35 ℃/min, heating to 500 ℃ at the heating rate of less than or equal to 1 ℃/min, preserving heat and pressure for 5-10min, cooling and releasing pressure, and cooling to room temperature.
Preferably, the cooling is furnace cooling.
Preferably, in step S3, the solid solution is specifically: solid-dissolving at 480-520 deg.C for 10-12 hr.
Preferably, in step S3, the aging is specifically: aging at 200deg.C for 1-128h.
Preferably, in step S1, the cooling is water quenching cooling or air cooling.
Preferably, the granularity of the TC4 titanium alloy spherical powder is smaller than 25 mu m, and the granularity of the Mg-Gd-Zn-Zr alloy powder is 50-100 mu m.
2. The titanium alloy particle reinforced rare earth magnesium-based composite material prepared by the method.
The invention has the beneficial effects that: the invention provides a preparation method and a product of a titanium alloy particle reinforced rare earth magnesium-based composite material, wherein TC4 (Ti-6 Al-4V alloy) particles are selected as a reinforcing body in the method, and as titanium and magnesium are in a hexagonal structure, magnesium and titanium atoms are easier to combine, so that a good magnesium-titanium interface is formed, the transmission of load between the magnesium-based body and titanium particles is facilitated, the material fracture caused by stress concentration at the interface is reduced, and in addition, the transmission of load from the magnesium-based body to the titanium particles is facilitated to exert the synergistic deformation effect of the titanium particles, so that the plasticity of the composite material is improved. More importantly, TC4 particles can promote the generation of beta phase and LPSO phase in the rare earth magnesium alloy, so that more beta phase and LPSO phase appear in the rare earth magnesium alloy matrix, the two phases are firstly dissolved back into the matrix in a solid solution process in the later period, more nano precipitated phases can be precipitated in aging, on the one hand, dislocation movement in the deformation process can be blocked by the nano precipitated phases, dislocation plug sets are caused, and thus work hardening is caused. In addition, dislocations bypass or cut the nano-precipitates requiring additional energy or stress, thereby increasing the material strength. And through reasonable control of the dosage of TC4 particles, the uniform distribution of the TC4 particles in the matrix can be ensured, and the stacking trend of the TC4 particles in the matrix can be weakened to the greatest extent, because if the content of the TC4 particles is too small, the strengthening effect on the matrix is poor, and the content of the TC4 particles is too large, the TC4 particles are not easy to disperse uniformly in the ball milling process, thereby causing the agglomeration of the TC4 particles and deteriorating the mechanical property of the material. In addition, TC4 can be uniformly dispersed in a matrix by adopting a powder metallurgy process, and a hot-pressing sintering process is adopted, so that on one hand, a blank with higher density can be obtained, on the other hand, more beta phases can be presented in a granular form, and less beta phases are presented in a grid form, so that the obtained blank has better mechanical properties, because the beta phases can be broken along the grain boundary in the deformation process too early after forming a grid structure after being separated along the grain boundary, the mechanical properties of the material are not beneficial to being improved, and the granular beta phases can block dislocation movement in the deformation process, so that the strength of the material is improved. The preparation process is simple in flow, less in energy consumption, short in production time, low in cost, beneficial to industrial mass production, and good in application prospect and economic benefit.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objects and other advantages of the invention may be realized and obtained by means of the instrumentalities and combinations particularly pointed out in the specification.
Drawings
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in the following preferred detail with reference to the accompanying drawings, in which:
FIG. 1 is a SEM image at 200 times of a blank of the titanium alloy particle-reinforced rare earth magnesium-based composite material prepared in example 1;
FIG. 2 is an SEM image at 2000 times of a blank of the titanium alloy particle-reinforced rare earth magnesium-based composite material prepared in example 1;
FIG. 3 is an SEM image at 2000 times of a blank of the rare earth magnesium-based material prepared in comparative example 1;
FIG. 4 is a TEM image of the rare earth magnesium-based materials prepared in example 1 and comparative example 1;
fig. 5 is a graph showing the results of mechanical property tests of the rare earth magnesium-based materials and blanks thereof prepared in example 1 and comparative example 1.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
Example 1
Preparation of titanium alloy particle reinforced rare earth magnesium base composite material
S1, proportioning according to mass percentages: 5wt.% of TC4 (Ti-6 Al-4V) titanium alloy spherical powder with the granularity smaller than 25 mu m and the balance of Mg-15Gd-1Zn-0.5Zr alloy powder with the granularity distributed at 50-100 mu m, and mechanically ball-milling the TC4 titanium alloy spherical powder and the Mg-15Gd-1Zn-0.5Zr alloy powder for 5 hours in an argon atmosphere according to the ball-to-material ratio of 10:1 and the rotating speed of 80rpm to obtain mixed powder;
s2, placing the mixed powder obtained in the step S1 into a graphite mold, placing the mold into a vacuum hot-pressing furnace, vacuumizing to 20Pa, pre-pressurizing a hot-pressing head to 5MPa, pressurizing to 100MPa, heating to 400 ℃ at a heating rate of 80 ℃/min, heating to 495 ℃ at a heating rate of 30 ℃/min, heating to 500 ℃ at a heating rate of 1 ℃/min, preserving heat and pressure for 5min, cooling and releasing pressure, and cooling to room temperature along with the furnace to obtain a blank;
s3, after the blank obtained in the step S2 is subjected to solid solution for 12 hours at 520 ℃, aging for 80 hours at 200 ℃, and air-cooling to room temperature, so that the finished product is obtained.
Example 2
Preparation of titanium alloy particle reinforced rare earth magnesium base composite material
S1, proportioning according to mass percentages: 2wt.% of TC4 (Ti-6 Al-4V) titanium alloy spherical powder with the granularity smaller than 25 mu m, and the balance of Mg-10Gd-2Zn-0.3Zr alloy powder with the granularity distributed at 50-100 mu m, and mechanically ball-milling the TC4 titanium alloy spherical powder and the Mg-10Gd-2Zn-0.3Zr alloy powder for 4 hours at the rotating speed of 100rpm according to the ball-to-material ratio of 5:1 in the argon atmosphere to obtain mixed powder;
s2, placing the mixed powder obtained in the step S1 into a graphite mold, placing the mold into a vacuum hot-pressing furnace, vacuumizing to 15Pa, pre-pressurizing a hot-pressing head to 5MPa, pressurizing to 90MPa, heating to 390 ℃ at a heating rate of 90 ℃/min, heating to 485 ℃ at a heating rate of 20 ℃/min, heating to 500 ℃ at a heating rate of 0.8 ℃/min, preserving heat and pressure for 8min, cooling and releasing pressure, and cooling to room temperature along with the furnace to obtain a blank;
s3, after the blank obtained in the step S2 is subjected to solid solution at 480 ℃ for 11 hours, aging at 200 ℃ for 128 hours, and air-cooling to room temperature.
Example 3
Preparation of titanium alloy particle reinforced rare earth magnesium base composite material
S1, proportioning according to mass percentages: 10wt.% of TC4 (Ti-6 Al-4V) titanium alloy spherical powder with the granularity smaller than 25 mu m and the balance of Mg-5Gd-1.5Zn-0.1Zr alloy powder with the granularity distributed at 50-100 mu m, and mechanically ball-milling the TC4 titanium alloy spherical powder and the Mg-5Gd-1.5Zn-0.1Zr alloy powder for 3 hours in an argon atmosphere according to a ball-to-material ratio of 8:1 and a rotating speed of 50rpm to obtain mixed powder;
s2, placing the mixed powder obtained in the step S1 into a graphite mold, placing the mold into a vacuum hot-pressing furnace, vacuumizing to 10Pa, pre-pressurizing a hot-pressing head to 5MPa, pressurizing to 80MPa, heating to 420 ℃ at a heating rate of 100 ℃/min, heating to 490 ℃ at a heating rate of 35 ℃/min, heating to 500 ℃ at a heating rate of 0.5 ℃/min, preserving heat and pressure for 10min, cooling and releasing pressure, and cooling to room temperature along with the furnace to obtain a blank;
s3, after the blank obtained in the step S2 is subjected to solid solution for 10 hours at 500 ℃, aging for 60 hours at 200 ℃, and air-cooling to room temperature, so that the finished product is obtained.
Comparative example 1
The difference from example 1 is that TC4 (Ti-6 Al-4V) titanium alloy spherical powder was not added.
The billets (TC 4/GZ151K billets) of the titanium alloy particle-reinforced rare earth magnesium-based composite material prepared in example 1 were observed at 200 times and 2000 times, respectively, using an electron scanning microscope, and the results are shown in fig. 1 and 2; the ingot (GZ 151K ingot) of the rare earth magnesium-based material prepared in comparative example 1 was observed at 2000 times, and the result is shown in fig. 3. As can be seen from FIG. 1, the spherical TC4 particles in the TC4/GZ151K blank are uniformly distributed in the matrix, no agglomeration phenomenon exists, the interface between TC4 and the magnesium matrix is well combined, no obvious gaps or hollows exist in the matrix, and coarse chain-shaped second phases are not precipitated. From fig. 2 and 3, the results of statistics of the beta phase and the LPSO phase in the TC4/GZ151K blank and the GZ151K blank are shown in table 1, and it is clear from fig. 2, 3 and 1 that the amounts of the beta phase and the LPSO phase in the TC4/GZ151K blank are significantly greater than those in the GZ151K blank, and that a plurality of granular beta phases, a few grid beta phases and a large number of lamellar LPSO structures are present in the TC4/GZ151K blank, which indicates that the addition of TC4 particles can promote precipitation of the beta phases and the LPSO structures.
Table 1 statistical results of beta phase and LPSO phase in billets of rare earth magnesium-based materials prepared in example 1 and comparative example 1
As a result of testing the rare earth magnesium-based materials prepared in example 1 and comparative example 1 by using a transmission electron microscope, as shown in fig. 4 and table 2, it is apparent from fig. 4 that the rare earth magnesium-based material (TC 4/GZ 151K) prepared in example 1 has more, more dispersed, finer nano-precipitated phases (β' precipitated phases) precipitated in the matrix than the rare earth magnesium-based material (GZ 151K) prepared in comparative example 1. As is clear from table 2, the number of β 'precipitated phases in TC4/GZ151K are higher in surface density and area ratio than GZ151K, and further, it is described that a larger number of β' precipitated phases are present in TC4/GZ 151K.
TABLE 2 statistical results of beta' -precipitate phases in rare earth magnesium-based materials prepared in example 1 and comparative example 1
As shown in fig. 5 and table 3, the results of mechanical property tests on the rare earth magnesium-based materials and the blanks thereof prepared in example 1 and comparative example 1, respectively, show that the plasticity and strength of the TC4/GZ151K blank are superior to those of the GZ151K blank, the strength of TC4/GZ151K is superior to that of GZ151K, and the plasticity is slightly inferior to that of GZ151K, but the overall has higher plasticity. In the sintering process, TC4 particles promote the precipitation of beta-phase and LPSO structures, and a plurality of granular beta-phase, a few grid beta-phase and a plurality of lamellar LPSO structures exist in the TC4/GZ151K blank, so that the strength and the plasticity of the blank are improved. After solid solution and aging treatment, the beta phase and LPSO structure in the blank are converted into nano precipitated phases, and dislocation movement in the deformation process can be blocked by the nano precipitated phases, so that dislocation plug sets are caused, and work hardening is caused. In addition, dislocations bypass or cut the nano-precipitates requiring additional energy or stress, thereby increasing the material strength. The strength of the TC4/GZ151K is improved and the plasticity is sacrificed, so that the plasticity of the TC4/GZ151K is slightly lower than that of the GZ151K, but the addition of TC4 particles can form a good magnesium-titanium interface, which is beneficial to the transmission of load between a magnesium matrix and titanium particles, thereby being beneficial to exerting the cooperative deformation effect of the titanium particles, and finally ensuring that the TC4/GZ151K still maintains higher plasticity.
Table 3 test results of mechanical properties of rare earth magnesium-based materials and blanks thereof prepared in example 1 and comparative example 1
Finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the present invention, which is intended to be covered by the claims of the present invention.
Claims (10)
1. The preparation method of the titanium alloy particle reinforced rare earth magnesium-based composite material is characterized by comprising the following steps of:
s1, proportioning according to mass percentages: 2-10wt.% of TC4 titanium alloy spherical powder and the balance of Mg-Gd-Zn-Zr alloy powder, and ball milling the TC4 titanium alloy spherical powder and the Mg-Gd-Zn-Zr alloy powder under a protective atmosphere to obtain mixed powder;
s2, placing the mixed powder into a die, and hot-pressing and sintering to obtain a blank;
s3, carrying out solid solution and aging treatment on the blank, and cooling to room temperature.
2. The preparation method of claim 1, wherein in step S1, the Mg-Gd-Zn-Zr alloy powder comprises the following components in percentage by mass: 5-15wt.% Gd, 1-2% zn, 0.1-0.5% zr, the balance Mg and unavoidable impurities.
3. The preparation method according to claim 1, wherein in step S1, ball milling under the protective atmosphere specifically comprises: ball milling is carried out for 3-5h at the rotating speed of 50-100rpm according to the ball-material ratio of 5-10:1 under the argon atmosphere.
4. The method according to claim 1, wherein in step S2, the hot press sintering is specifically: placing the die in a vacuum hot-pressing furnace, vacuumizing to be less than or equal to 20Pa, pre-pressurizing a hot-pressing head to be 5MPa, pressurizing to be 80-100MPa, heating to 390-420 ℃ at the heating rate of 80-100 ℃/min, heating to 485-495 ℃ at the heating rate of 20-35 ℃/min, heating to 500 ℃ at the heating rate of less than or equal to 1 ℃/min, preserving heat and pressure for 5-10min, cooling and releasing pressure, and cooling to room temperature.
5. The method of claim 4, wherein the cooling is furnace cooling.
6. The method according to claim 1, wherein in step S3, the solid solution is specifically: solid-dissolving at 480-520 deg.C for 10-12 hr.
7. The method according to claim 1, wherein in step S3, the aging is specifically: aging at 200deg.C for 1-128h.
8. The method according to claim 1, wherein in step S1, the cooling is water quenching or air cooling.
9. The method of any one of claims 1 to 8, wherein the TC4 titanium alloy spherical powder has a particle size of less than 25 μm and the Mg-Gd-Zn-Zr alloy powder has a particle size of 50 to 100 μm.
10. A titanium alloy particle-reinforced rare earth magnesium-based composite material prepared by the method of any one of claims 1-9.
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