CN113600792A - Spatial two-phase continuous structure Ti2AlC/Mg-based composite material and pressureless infiltration preparation method thereof - Google Patents
Spatial two-phase continuous structure Ti2AlC/Mg-based composite material and pressureless infiltration preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
- B22D23/04—Casting by dipping
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- C22C1/10—Alloys containing non-metals
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- C22C1/1068—Making hard metals based on borides, carbides, nitrides, oxides or silicides
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- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
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- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
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- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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Abstract
Spatial two-phase continuous structure Ti2AlC/Mg-based composite material and a pressureless infiltration preparation method thereof. In the material Ti2The volume content of AlC is 30-80 vol.%, and the balance is Mg alloy. The microstructure of the material is ceramic phase Ti2AlC and metal phase Mg are respectively in three-dimensional continuous network cross distribution, and the interface combination of the AlC and the metal phase Mg is firm. The preparation method of the material comprises the following steps: in-situ synthesis of Ti with different porosities2Placing the AlC preform in an alumina crucible, placing a Mg alloy ingot above the AlC preform, and heating to 700 ℃ at a speed of 10-30 ℃/min under vacuumAnd (3) preserving the heat at 750 ℃ for 30-120 min, and cooling to room temperature along with the furnace. The material has the remarkable characteristics of low density, high strength, high rigidity, wear resistance, self lubrication and the like, and can be widely used for manufacturing lightweight parts in the fields of vehicles, aerospace and the like.
Description
Technical Field
The invention relates to a spatial two-phase continuous structure Ti2AlC/Mg-based composite material and a pressureless infiltration preparation method thereof.
Background
Magnesium alloy is the lightest metal structure material in the world, and has important application value and wide development prospect in the competitive field of light weight and low emission in the automobile industry (reference: Wu culture, Chinese energy, 2007,29[10]: P.19-22). Meanwhile, the magnesium alloy has the advantages of high specific strength and specific stiffness, strong electromagnetic shielding performance, strong damping and shock absorbing performance and the like, and has good prospects in the fields of aerospace, electronics and the like (reference documents: R.Oakley, R.Cochrane, and R.Stevens, Key Engineering Materials,1995,104: P.387-416). However, magnesium alloys have low absolute strength, especially poor high temperature performance, which limits their applications in engine parts and transmission parts, such as cylinder liners, bearing bushes, etc.
Research has shown that the only way to pursue magnesium alloys that are heat resistant and have wear resistant properties is through compounding (ref: A. Mortensen, J. Llorca, Materials Today,2010,9[6]: P.1-16). Namely, the 'reinforcement/functional body' is added in the magnesium alloy, and the performance of the material is comprehensively improved by reasonably regulating and controlling the interface, the tissue structure and the like on the basis of utilizing the intrinsic performance of different material components. The magnesium-based composite material not only inherits the advantages of low density, high specific strength and specific stiffness, electromagnetic shielding performance, damping performance and the like of the magnesium alloy, but also improves the absolute strength, high-temperature performance, friction performance, plasticity and the like. These excellent properties make it considered to be a light metal composite material which is extremely influential after the aluminum-based composite material. As most of cylinder liners of automobile and motorcycle cylinders are made of cast iron materials, the density of the cylinder liners is far greater than that of magnesium alloy, and in order to realize the light weight of engine cylinders, development of Mg-based composite materials with high strength, high rigidity, excellent damping, shock absorption and noise reduction performance and wear-resisting self-lubricating characteristics becomes a research hotspot.
SiC, TiC and Al2O3Granules, B4C and C nanotube whiskers and fibers, etc. are widely used as Mg-based composite reinforcements (ref: R.Oakley, R.Cochrane, and R.Stevens, Key Engineering Materials,1995,104: P.387-416). Among them, the most studied SiC — Mg based composite materials have been applied to propellers, missile empennages and internally reinforced cylinders by Textron corporation in the united states. Tensile experiments show that the failure mechanism of the composite material is caused by the separation of the SiC and Mg matrix interface to form cracks and further propagation. In addition, it has been found that high hot extrusion ratios are prone to cracking of the hard and brittle SiC. For the traditional SiC reinforced Mg-based composite material, Saravanan (reference: R. Saravanan, M. Surappa, Materials Science and Engineering: A,2000.276[1 ]]P.108-116) found that 30 vol.% SiC-Mg in the composite had improved wear resistance by two orders of magnitude over pure magnesium, but the hard and brittle SiC ceramic particles were easily dislodged from the Mg matrix causing severe "furrowing" scratching of the matrix surface. Meanwhile, the hard and brittle SiC reinforcement body which does not have damping capacity is not beneficial to damping shock absorption of the whole composite material. In view of this, Das et al (reference: A.das, S.P.Harimkar, Journal of Materials Science&Technology,2014,30[11]P.1059-1070.) this phenomenon was overcome by the preparation of SiC-Graphene reinforced Mg-based composites by introducing carbon materials with high damping capacity and self-lubricating properties. However, graphite, which acts as a self-lubricating and damping capacity enhancing feature, is susceptible to oxidative failure in oxidizing environments above 350 ℃. Therefore, the traditional magnesium-based composite material reinforcement has the following defects: the ductility and toughness and damage tolerance of the material are low; ② and Mg groupThe formed interface has low binding force, hard and brittle particles are easy to fall off to cause Mg matrix scratching, and the introduced carbon material for overcoming the phenomenon is easy to lose efficacy by high-temperature oxidation; and thirdly, the hard and brittle particles are easy to be broken by later processing, such as hot extrusion.
Ti2AlC is a new type of ternary layered cermet material that can be machined and belongs to the hexagonal system with Mg. The polycrystalline block has Vickers hardness of 4.5GPa, Young's modulus of 277GPa, room-temperature compression strength of 540MPa and thermal expansion coefficient of 0.82 multiplied by 10-5K-1Conductivity at room temperature 2.7 (. mu.OMEGA. m)-1(reference: M.W. Barsum, et al, Metallurgical and Materials transformations A,2000,31[7 ]]P.1857-1865). Further, Ti2The AZ91D magnesium alloy reinforced by AlC has excellent tribological properties: the friction coefficient of the composite material is less than 0.34, and the specific wear rate is less than 5.0 multiplied by 10- 4mm3/(Nm) (ref: W.B.Yu, et al., Journal of materials science)&technology,2019,35[3]P.275-284). Meanwhile, MAX phase and metals such as Mg, Ti, Zr and Zn belong to a close-packed hexagonal system and have a micro plastic deformation mechanism, namely Incipient Knk Band (IKB) is formed inside, and the energy from the outside can be greatly absorbed in the cyclic compression process (reference: M.W.Barsum, et al., Nature Materials,2003,2[2 ]]P.107-111). Therefore, the MAX material can become a reinforcement for preparing composite materials with high damping, self-lubricating, wear-resistant and damage tolerance characteristics.
A space two-phase continuous structure cermet material is a structural form of a ceramic/metal composite material developed in the 80 s of the 20 th century, namely a ceramic phase and a metal phase are three-dimensional continuous and form a network cross structure in space. Compared with the fiber reinforced material, the structure has the characteristic of isotropy in the whole structure; it has the characteristic of being continuous with each other with respect to the particle or whisker reinforcing material. Spatially two-phase continuous structure Ti2The AlC/Mg-based composite material can be Ti2The AlC ceramic and the Mg-based alloy are both distributed continuously, the ceramic framework is toughened due to the toughness of the metal phase, the metal phase is enhanced due to the rigid bearing effect of the ceramic framework, and the ceramic framework and the metal phase are supported and reinforced mutually and support the framework mutually. At the same time, itThe material has more unique mechanical property, friction and abrasion resistance, vibration reduction performance and thermal performance, and has wide application prospect in the industrial fields of aerospace, transportation, mechanical manufacturing and the like.
Disclosure of Invention
The invention aims to provide a porous Ti2Ti with a space biphase continuous structure prepared from AlC prefabricated bodies (with the porosity of 30-80%) and Mg-based alloy serving as raw materials2AlC/Mg-based composite material and a pressureless infiltration preparation method thereof.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
spatial two-phase continuous structure Ti2The AlC/Mg-based composite material and the pressureless infiltration preparation method thereof are characterized in that:
(1) the Ti with the space biphase continuous structure prepared by the method2The AlC/Mg-based composite material comprises the following components: ti2The volume content of AlC is 20-70 vol.%, and the balance is Mg-based alloy;
(2) the Ti with the space biphase continuous structure prepared by the method2The AlC/Mg-based composite material is characterized in that: the Ti2Ceramic phase Ti in microstructure of AlC/Mg-based composite material2AlC and metal phase Mg-based alloy are respectively in three-dimensional continuous space distribution and in a network cross structure in space;
(3) the method comprises the following steps:
step 1, marking Mg-based alloy bars at intervals of 10-20 mm, placing the marked bars into a precision cutting machine, fixing the bars by using a clamp according to marks reserved on the bars, setting a tool, setting a cutting speed of 0.05-0.1 mm/s and a cutting stroke of 100-200 mm, starting a program, and taking out Mg-based alloy ingots after the cutting is finished;
step 2, paving a layer of thin graphite paper in the alumina crucible, and synthesizing Ti in situ with porosity of 30-80 percent2Placing the AlC prefabricated body in an alumina crucible, placing a pre-cut Mg-based alloy ingot above or below the AlC prefabricated body, and covering an alumina cover;
step 3, putting the alumina crucible into a vacuum sintering furnaceHeating to 700-750 ℃ at a rate of 10-30 ℃/min under vacuum. Wherein, the vacuumizing is stopped at 300 ℃, meanwhile, argon is introduced into the furnace, the atmosphere pressure is 9-15KPa, the temperature is increased to 700-750 ℃, then the temperature is kept for 30-120 min, and the temperature is cooled to room temperature along with the furnace, so that the Ti with the space biphase continuous structure is obtained2AlC/Mg based composite material.
The invention has the following beneficial effects:
the spatial two-phase continuous structure Ti of the invention2AlC/Mg based composite material having compressive strength, maximum strain rate and Vickers hardness depending on initial Ti2The porosity of AlC preforms varies. The spatial two-phase continuous structure Ti of the invention2The highest compressive yield strength of the AlC/Mg-based composite material can reach 630MPa, the highest compressive strength can reach 870MPa, and the highest Vickers hardness is 2.1 GPa. Spatially biphasic continuous structure Ti for the purposes of the invention2The pressureless infiltration preparation method of the AlC/Mg-based composite material has the main advantages of simple process and easy operation, and is suitable for manufacturing wear-resistant self-lubricating parts needing light weight, good conductivity, high specific strength and rigidity.
The spatial two-phase continuous structure Ti of the invention2The AlC/Mg-based composite material can be widely applied to the fields of transportation, aerospace, mechanical manufacturing and the like, such as automobile parts of automobile engine cylinder bodies, automobile connecting rods and the like, and can also be used for manufacturing devices of radiating fins of electronic equipment and the like.
Drawings
FIG. 1 is an in situ synthesis of porous Ti for use in the present invention2AlC preform
FIG. 2A spatially two-phase continuous structure Ti of the present invention2Microstructure of AlC/Mg-based composite material with Ti as light gray part2An AlC reinforcing phase, a dark grey fraction of Mg-based alloy.
FIG. 3 shows a spatially two-phase continuous structure Ti of the present invention2And (3) three-dimensional reconstruction of the AlC/Mg-based composite material.
Detailed Description
The invention provides a spatial two-phase continuous structure Ti2AlC/Mg-based composite material and pressureless infiltration preparation method thereof, the invention is described below by combining the accompanying drawings and examplesThe present invention will be described in detail, but the present invention is not limited thereto.
Implementation mode one
Marking Mg-based alloy bars at intervals of 10mm, putting the marked bars into a precision cutting machine, fixing the bars by using a clamp according to marks reserved on the bars, setting a cutter, setting the cutting speed to be 0.05mm/s and the cutting stroke to be 100mm, starting a program, and taking out Mg-based alloy ingots after the cutting is finished. Laying a layer of thin graphite paper in an alumina crucible, and putting porous in-situ Ti with the porosity of 30 percent2The AlC preform is placed in an alumina crucible, Mg-based alloy ingots cut in advance are placed above and below the AlC preform, and an alumina lid is covered. The alumina crucible is placed in a vacuum sintering furnace and heated to 750 ℃ at a rate of 10 ℃/min under vacuum. Stopping vacuumizing when the temperature reaches 300 ℃, simultaneously introducing argon into the furnace, keeping the atmospheric pressure at 9KPa, keeping the temperature for 30min after the temperature is raised to the corresponding temperature, and cooling to room temperature along with the furnace to obtain the Ti with the spatial two-phase continuous structure2AlC/Mg based composite material.
The above-mentioned space two-phase continuous structure Ti2Processing the AlC/Mg-based composite material into a cylinder with the diameter of 5mm and the length of 8mm, and loading on a universal testing machine at a loading speed of 0.5 mm/min; the yield strength was determined to be 630MPa, the compressive strength was 870MPa, the strain rate was 6.3%, and the Vickers hardness was 2.1 GPa.
Second embodiment
Marking Mg-based alloy bars at intervals of 15mm, putting the marked bars into a precision cutting machine, fixing the bars by using a clamp according to marks reserved on the bars, setting a cutter, setting the cutting speed to be 0.08mm/s and the cutting stroke to be 150mm, starting a program, and taking out Mg-based alloy ingots after the cutting is finished. Laying a layer of thin graphite paper in an alumina crucible, and putting porous in-situ Ti with porosity of 50%2The AlC preform is placed in an alumina crucible, Mg-based alloy ingots cut in advance are placed above and below the AlC preform, and an alumina lid is covered. The alumina crucible is put into a vacuum sintering furnace and heated to 750 ℃ at a speed of 20 ℃/min under vacuum. When the temperature reaches 300 ℃, stopping vacuumizing, and simultaneously introducing argon into the furnace, wherein the atmosphere pressure is 10KPa, and the temperature isHeating to corresponding temperature, keeping the temperature for 60min, and cooling to room temperature along with the furnace to obtain the spatial two-phase continuous structure Ti2AlC/Mg based composite material.
The above-mentioned space two-phase continuous structure Ti2Processing the AlC/Mg-based composite material into a cylinder with the diameter of 5mm and the length of 8mm, and loading on a universal testing machine at a loading speed of 0.5 mm/min; the yield strength was 545MPa, the compressive strength was 755MPa, the strain rate was 7.5%, and the Vickers hardness was 1.95 GPa.
Third embodiment
Marking Mg-based alloy bars at intervals of 20mm, putting the marked bars into a precision cutting machine, fixing the bars by using a clamp according to marks reserved on the bars, setting a cutter, setting the cutting speed to be 0.1mm/s and the cutting stroke to be 200mm, starting a program, and taking out Mg-based alloy ingots after the cutting is finished. Laying a layer of thin graphite paper in an alumina crucible, and putting porous in-situ Ti with the porosity of 60 percent2The AlC preform is placed in an alumina crucible, Mg-based alloy ingots cut in advance are placed above and below the AlC preform, and an alumina lid is covered. The alumina crucible is put into a vacuum sintering furnace and heated to 750 ℃ at 30 ℃/min under vacuum. Stopping vacuumizing when the temperature reaches 300 ℃, simultaneously introducing argon into the furnace, keeping the atmospheric pressure at 11KPa, keeping the temperature for 90min after the temperature is raised to the corresponding temperature, and cooling to room temperature along with the furnace to obtain the Ti with the spatial two-phase continuous structure2AlC/Mg based composite material.
The above-mentioned space two-phase continuous structure Ti2Processing the AlC/Mg-based composite material into a cylinder with the diameter of 5mm and the length of 8mm, and loading on a universal testing machine at a loading speed of 0.5 mm/min; the yield strength was found to be 457MPa, the compressive strength was found to be 623MPa, the strain rate was found to be 11.6%, and the Vickers hardness was found to be 1.67 GPa.
Claims (1)
1. Spatial two-phase continuous structure Ti2The AlC/Mg-based composite material and the pressureless infiltration preparation method thereof are characterized in that:
(1) the Ti with the space biphase continuous structure prepared by the method2The AlC/Mg-based composite material comprises the following components: ti2Volume of AlCThe content is 30-80 vol.%, and the balance is Mg-based alloy;
(2) the Ti with the space biphase continuous structure prepared by the method2The AlC/Mg-based composite material is characterized in that: the Ti2Ceramic phase Ti in microstructure of AlC/Mg-based composite material2AlC and metal phase Mg-based alloy are respectively in three-dimensional continuous space distribution and in a network cross structure in space;
(3) the method comprises the following steps:
step 1, marking Mg-based alloy bars at intervals of 10-20 mm, placing the marked bars into a precision cutting machine, fixing the bars by using a clamp according to marks reserved on the bars, setting a tool, setting a cutting speed of 0.05-0.1 mm/s and a cutting stroke of 100-200 mm, starting a program, and taking out Mg-based alloy ingots after the cutting is finished;
step 2, paving a layer of thin graphite paper in the alumina crucible, and synthesizing Ti in situ with porosity of 30-80 percent2Placing the AlC prefabricated body in an alumina crucible, placing a pre-cut Mg-based alloy ingot above or below the AlC prefabricated body, and covering an alumina cover;
and 3, putting the alumina crucible into a vacuum sintering furnace, heating to 700-750 ℃ at a speed of 10-30 ℃/min under vacuum, stopping vacuumizing at 300 ℃, introducing argon into the furnace at an atmosphere pressure of 9-15KPa, keeping the temperature for 30-120 min after the temperature is raised to a corresponding temperature, and cooling to room temperature along with the furnace to obtain the Ti with the spatial two-phase continuous structure2AlC/Mg based composite material.
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