CN113308637A - MAX reinforced magnesium-based composite material and manufacturing method thereof - Google Patents

MAX reinforced magnesium-based composite material and manufacturing method thereof Download PDF

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CN113308637A
CN113308637A CN202110575078.6A CN202110575078A CN113308637A CN 113308637 A CN113308637 A CN 113308637A CN 202110575078 A CN202110575078 A CN 202110575078A CN 113308637 A CN113308637 A CN 113308637A
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dimensional porous
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composite material
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刘景申
王洋
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Hebei Runxia New Material Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—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
    • C22C32/0047—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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1005—Pretreatment of the non-metallic additives
    • C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1005—Pretreatment of the non-metallic additives
    • C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
    • C22C1/1021—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform the preform being ceramic
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C22C1/1068—Making hard metals based on borides, carbides, nitrides, oxides or silicides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—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
    • 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

Abstract

The embodiment of the invention discloses a MAX reinforced magnesium-based composite material and a manufacturing method thereof. The material is made of Ti2AlC or Ti3AlC2And a metal phase of Mg or Mg alloy, and the cermet phase exists in the form of a three-dimensional porous framework within the MAX reinforced magnesium matrix composite. The method comprises the following steps: step one, providing base powder, wherein the base powder is Ti2AlC powder or Ti3AlC2Powder; secondly, manufacturing a three-dimensional porous framework by using the base powder; step three, infiltrating the melted Mg or Mg alloy into the alloyAnd forming the MAX reinforced magnesium-based composite material in the three-dimensional porous framework. In the MAX reinforced magnesium-based composite material disclosed by the invention, the metal ceramic phase exists in a three-dimensional porous framework form, and the structure shows that the ceramic phase and the metal phase are respectively continuous in each direction and are three-dimensionally interlocked with each other, so that the problem of performance failure can be avoided, and the stable performance is ensured to reach the standard.

Description

MAX reinforced magnesium-based composite material and manufacturing method thereof
Technical Field
The invention relates to the technical field of metal ceramic materials, in particular to a MAX reinforced magnesium-based composite material and a manufacturing method thereof.
Background
As a light high-strength structural material, the ceramic has the advantages of high tensile strength, compressive strength, elastic modulus, hardness and the like, stable physical properties, wear resistance, acid and alkali resistance, corrosion resistance and the like, but is difficult to widely apply in some important fields due to high brittleness, low impact resistance, fragility, difficult processing and the like. Magnesium as metal is another light structural material, has high specific strength and specific stiffness, excellent casting performance and machining performance, and has wide application prospect. However, the magnesium alloy has low elastic modulus, limited high-temperature strength, poor wear resistance and poor corrosion resistance, and greatly limits the industrial application of the magnesium alloy.
From Ti2AlC/Ti3AlC2The composite material (MAX reinforced magnesium-based composite material) composed of MAX ceramics and magnesium metal can obtain the comprehensive performance which can not be achieved by a single composition phase through the complementation and the association of the performances of all the components on the premise of keeping the performance advantages of the two composition phases. At present, Ti2AlC/Ti3AlC2The preparation technology of the composite material consisting of-Mg is mainly to add MAX ceramic phase powder into Mg and Mg alloy semi-solid state and stir the mixture evenly to prepare a blank, and then extrude or pressurize the blank to obtain MAX reinforced magnesium-based composite material.
However, the MAX reinforced mg-based composite material produced in the prior art is difficult to be effectively controlled in structure, and is easy to have the problem of performance failure, so that the performance of the MAX reinforced mg-based composite material cannot meet the application requirement, and the MAX reinforced mg-based composite material is limited to a certain extent.
Disclosure of Invention
The present invention aims to provide a MAX reinforced magnesium-based composite material and a manufacturing method thereof, so as to solve the problems.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a MAX reinforced Mg-base composite material is prepared from Ti2AlC or Ti3AlC2And a metal phase of Mg or Mg alloy, said cermetThe phases exist in the form of a three-dimensional porous skeleton in the MAX reinforced magnesium-based composite material.
Preferably, the volume fraction of the cermet phase is not less than 30% -90%.
Preferably, the volume fraction of the cermet phase is between 50% and 90%.
Preferably, the diameter size of the unit ring of the three-dimensional porous framework is 10nm-100 mu m, and the diameter size of the metal phase is 10nm-100 mu m
A manufacturing method of a MAX reinforced magnesium-based composite material comprises the following steps:
step one, providing base powder, wherein the base powder is Ti2AlC powder or Ti3AlC2Powder;
secondly, manufacturing a three-dimensional porous framework by using the base powder;
and step three, infiltrating the melted Mg or Mg alloy into the three-dimensional porous framework to form the MAX reinforced magnesium-based composite material.
Preferably, the second step includes:
s21, manufacturing a three-dimensional porous framework blank by using a compression molding process or a powder grouting process;
and step S22, sintering the green body to form the three-dimensional porous framework.
Preferably, the process of manufacturing the three-dimensional porous skeleton blank by using the compression molding process comprises the following steps:
placing the base powder in a molding die;
applying pressure to 3-10 MPa;
keeping the constant pressure for 0.1h-2h to form the three-dimensional porous framework blank.
Preferably, the process of manufacturing the three-dimensional porous skeleton blank by using the powder grouting process comprises the following steps:
mixing the base powder with deionized water to form a powder slurry, wherein the base powder accounts for 40-70% of the mass of the powder slurry;
injecting the slip into a gypsum mold;
standing and curing to form the three-dimensional porous framework green body.
Preferably, the step S22 includes:
drying the three-dimensional porous framework blank to constant weight;
heating to 750-1200 ℃ in a protective atmosphere;
keeping the constant temperature for 0.5h-2h to form the three-dimensional porous framework.
Preferably, the second step includes:
placing the base powder in a hot-pressing mold;
heating to 750-1200 ℃ in protective atmosphere or vacuum environment, and pressurizing to 2-20 MPa;
keeping constant temperature and constant pressure for 0.5-3 h to form the three-dimensional porous skeleton.
Preferably, the third step includes:
placing solid Mg or a solid Mg alloy on the three-dimensional porous skeleton;
heating to a temperature higher than the melting point of solid Mg or a solid Mg alloy in a protective atmosphere or a vacuum environment to melt the solid Mg or the solid Mg alloy;
keeping the constant temperature for not less than 5min, so that the melted Mg or Mg alloy permeates into the three-dimensional porous framework;
and cooling and solidifying to form the MAX reinforced magnesium-based composite material.
In the MAX reinforced magnesium-based composite material disclosed by the invention, the metal ceramic phase exists in a three-dimensional porous framework form, and the structure shows that the ceramic phase and the metal phase are respectively continuous in each direction and are mutually interlocked in three dimensions, so that the problem of performance failure can be avoided, and the stable performance can be ensured to reach the standard.
Meanwhile, the MAX reinforced magnesium-based composite material manufacturing method provided by the invention prepares a three-dimensional porous framework with uniformly distributed pores in advance, and then infiltrates with Ti2AlC or Ti3AlC2The powder has better wettability of Mg or Mg alloy, so that the composite material prepared by the method has compact structure, uniform components and no obvious defects.
Further, the present inventionTi can also be expected by adjusting the pressure, time or the ratio of the powder slurry materials2AlC or Ti3AlC2And can adjust Ti in the material in a wide range2AlC or Ti3AlC2So that the performance thereof can be adjusted within a wide range to meet the performance requirements under different environments.
Particularly, in terms of performance, the MAX reinforced magnesium-based composite material prepared by the invention is obviously improved in hardness and strength, so that the MAX reinforced magnesium-based composite material prepared by the invention can be further applied to the field with higher requirements.
Drawings
FIG. 1 is a microstructure of a three-dimensional porous skeleton according to example 3 of the present invention;
FIG. 2 is a micro-topography of a MAX enhanced Mg-based composite material provided in embodiment 3 of the present invention;
fig. 3 is a bending stress-strain curve diagram of a MAX reinforced mg-based composite material provided in embodiment 3 of the present invention;
FIG. 4 is a microstructure of a three-dimensional porous skeleton according to example 4 of the present invention;
FIG. 5 is a micro-topography of a MAX enhanced Mg-based composite material provided in embodiment 4 of the present invention;
fig. 6 is a bending stress-strain curve of a MAX reinforced mg-based composite material provided in embodiment 4 of the present invention;
FIG. 7 is a microstructure of a three-dimensional porous skeleton according to example 6 of the present invention;
FIG. 8 is a micro-topography of a MAX enhanced Mg-based composite material provided in embodiment 6 of the present invention;
FIG. 9 is a microstructure of a three-dimensional porous skeleton provided in example 7 of the present invention;
FIG. 10 is a micro-topography of a MAX enhanced Mg-based composite material provided in embodiment 7 of the present invention;
FIG. 11 is a microstructure of a three-dimensional porous skeleton according to example 9 of the present invention;
fig. 12 is a micro-topography of a MAX enhanced mg-based composite material according to embodiment 9 of the present invention;
FIG. 13 is a three-dimensional porous scaffold microtopography provided in example 10 of the present invention;
fig. 14 is a micro-topography of a MAX enhanced mg-based composite material provided in embodiment 10 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
As described in the background art, the MAX reinforced mg-based composite material produced in the prior art is difficult to be effectively controlled in structure, and is prone to performance failure, so that the performance of the MAX reinforced mg-based composite material cannot meet the application requirements, and is limited to a certain extent.
The inventor has conducted extensive research on the existing materials and manufacturing processes, and found that the existing MAX reinforced Mg-based composite material has a structure in which most of Mg (metal phase) is continuous, but Ti is2AlC or Ti3AlC2It is the discontinuity (cermet phase) that leads to the problem of performance failure.
In addition, most of the existing MAX reinforced magnesium-based composite materials are cast and molded in the process, so that defects such as air holes and cracks are easily formed in the materials, and particularly when the content of ceramic is high, the defects are easily formed, so that the improvement of the performance of the composite materials is limited to a certain extent. Therefore, through composition analysis, the existing material has 5-50% of ceramic, more metal content and less ceramic content, the hardness is not more than 200HV, the strength is not more than 700MPa, and the material cannot be further applied in fields with higher requirements.
Based on the research, the invention discloses a MAX reinforced magnesium-based composite material and a manufacturing method thereof.
Wherein the MAX reinforced magnesium-based composite material is prepared from Ti2AlC or Ti3AlC2And a metal phase of Mg or Mg alloy, and the cermet phase exists in the form of a three-dimensional porous framework within the MAX reinforced magnesium matrix composite.
The manufacturing method of the MAX reinforced magnesium-based composite material comprises the following steps:
step one, providing base powder, wherein the base powder is Ti2AlC powder or Ti3AlC2Powder;
secondly, manufacturing a three-dimensional porous framework by using the base powder;
and step three, infiltrating the melted Mg or Mg alloy into the three-dimensional porous framework to form the MAX reinforced magnesium-based composite material.
In the MAX reinforced magnesium-based composite material disclosed by the invention, the metal ceramic phase exists in a three-dimensional porous framework form, and the structure shows that the ceramic phase and the metal phase are respectively continuous in each direction and are mutually interlocked in three dimensions, so that the problem of performance failure can be avoided, and the stable performance can be ensured to reach the standard.
Meanwhile, the MAX reinforced magnesium-based composite material manufacturing method provided by the invention prepares a three-dimensional porous framework with uniformly distributed pores in advance, and then infiltrates with Ti2AlC or Ti3AlC2The Mg or Mg alloy with better powder wettability is three-dimensionally penetrated by the framework, so the Mg or Mg alloy is melted to fill the gap and is also three-dimensionally penetrated, the Mg or Mg alloy and the Mg alloy both present a continuous structural state and are three-dimensionally interlocked, the problem of performance failure can be avoided, and the composite material prepared by the method provided by the invention has a compact structure and uniform components and has no obvious defects.
The technical solution of the present invention is further described below with reference to the following embodiments and the accompanying drawings.
Example one
This example provides a MAX reinforced Mg-based composite material composed of Ti2AlC or Ti3AlC2Gold (II) ofThe metal ceramic phase exists in the MAX reinforced magnesium-based composite material in a form of a three-dimensional porous framework. Is particularly expressed as Ti2AlC or Ti3AlC2The metal ceramic phase is penetrated in three dimensions, the metal phase and the ceramic phase are respectively continuous, the interface wetting is good, the problem of performance failure can be avoided, and the performance is ensured to be stable and reach the standard.
Wherein the porosity of the three-dimensional porous skeleton is 10-70%, the diameter of the unit ring of the three-dimensional porous skeleton is 10nm-100 μm, and the diameter of the metal phase of Mg or Mg alloy is 10nm-100 μm. The Ti2AlC or Ti3AlC2The volume fraction of the cermet phase of (a) is not less than 30%. In order to obtain better material properties, the Ti of the examples of the invention2AlC or Ti3AlC2The volume fraction of the cermet phase is generally greater than 30%, and is controlled to be between 30% and 90% in the production process, or between 50% and 90% according to actual requirements, or between 35% and 55%.
The material disclosed by the invention has high content of cermet, hardness of over 200HV and strength of over 700MPa, and can be further applied to the field with high requirements.
Example two
The embodiment provides a method for manufacturing a MAX reinforced magnesium-based composite material, which comprises the following steps:
step one, providing base powder, wherein the base powder is Ti2AlC powder or Ti3AlC2Powder;
secondly, manufacturing a three-dimensional porous framework by using the base powder;
and step three, infiltrating the melted Mg or Mg alloy into the three-dimensional porous framework to form the MAX reinforced magnesium-based composite material.
Wherein the second step comprises:
and step S21, forming a three-dimensional porous framework blank by using a compression molding process.
That is, the base powder is placed in a molding die;
applying pressure to 3-10 MPa;
keeping the constant pressure for 0.1h-2h to form the three-dimensional porous framework blank.
In this example, Ti in the material2AlC or Ti3AlC2The volume fraction of (A) is increased and decreased with an increase in pressure at the time of press molding, thereby enabling the Ti to be molded2AlC or Ti3AlC2Adjustment of the volume fraction of (a).
And step S22, sintering the green body to form the three-dimensional porous framework.
Namely, drying the three-dimensional porous framework blank to constant weight;
heating to 750-1200 ℃ in a protective atmosphere;
keeping the constant temperature for 0.5h-2h to form the three-dimensional porous framework.
The third step comprises:
placing solid Mg or a solid Mg alloy on the three-dimensional porous skeleton;
heating to a temperature higher than the melting point of solid Mg or a solid Mg alloy in a protective atmosphere or a vacuum environment to melt the solid Mg or the solid Mg alloy;
keeping the constant temperature for not less than 5min, so that the melted Mg or Mg alloy permeates into the three-dimensional porous framework;
and cooling and solidifying to form the MAX reinforced magnesium-based composite material.
The MAX reinforced magnesium-based composite material prepared by the method disclosed in the embodiment is Ti2AlC or Ti3AlC2The metal ceramic phase exists in a three-dimensional porous framework form, the structure shows that the ceramic phase and the metal phase are respectively continuous in all directions, and three dimensions are interlocked with each other, so that the problem of performance failure can be avoided, and the stable performance can be ensured to reach the standard. Furthermore, a three-dimensional porous framework with uniformly distributed pores is prepared in advance, and then the three-dimensional porous framework is infiltrated with Ti2AlC or Ti3AlC2The powder has better wettability of Mg or Mg alloy, so that the composite material prepared by the method has compact structure, uniform components and no obvious defects.
In addition, the present embodiment can anticipate Ti by adjusting the pressure of the process2AlC or Ti3AlC2And can adjust Ti in the material in a wide range2AlC or Ti3AlC2So that the performance thereof can be adjusted within a wide range to meet the performance requirements under different environments.
It should be noted that, in the examples of the present invention, the Ti is mentioned2AlC or Ti3AlC2The volume fraction of the metal-ceramic phase of (A) is tunable, so that in example one there is no Ti2AlC or Ti3AlC2The volume fraction of the metal-ceramic phase of (a) is more specifically limited. Meanwhile, the corresponding volume fraction is selected according to different performance requirements, which is also an important characteristic in the scheme of the invention.
EXAMPLE III
The embodiment provides a method for manufacturing a MAX reinforced magnesium-based composite material, which comprises the following steps:
step one, providing 20g of base powder, wherein the base powder is Ti2AlC powder.
And step two, manufacturing a three-dimensional porous framework by using the base powder. The method comprises the following steps:
and step S21, forming a three-dimensional porous framework blank by using a compression molding process.
Namely, uniformly putting the base powder into a mould;
adjusting the stroke of the hydraulic press to a complete die opening state, placing the die filled with the base powder at the center of the hydraulic press, pressurizing to 4MPa, keeping constant pressure for 0.2h, removing pressure, and opening the die again to obtain the three-dimensional porous skeleton blank.
And step S22, sintering the green body to form the three-dimensional porous framework.
Namely, the three-dimensional porous framework green body is naturally dried at room temperature, and is placed into a crucible after the green body reaches a constant weight, then the crucible filled with the three-dimensional porous framework green body is placed into a heating furnace, the heating is carried out under a protective atmosphere, the heating rate is 5 ℃/min, the temperature is raised to 900 ℃, the temperature is kept for 1h, and the three-dimensional porous framework green body is cooledTaking out the Ti after the temperature is reduced to room temperature to obtain Ti with certain strength2Three-dimensional porous skeleton of AlC.
And step three, infiltrating the melted Mg or Mg alloy into the three-dimensional porous framework to form the MAX reinforced magnesium-based composite material.
Weighing 30g of solid Mg, mechanically polishing, cleaning with acetone and alcohol, and drying to remove surface oxide layer and impurities.
And ultrasonically cleaning the graphite crucible in an absolute ethyl alcohol solution for 5 minutes, and then drying.
The three-dimensional porous framework and the solid Mg are sequentially arranged in a graphite crucible, and then the crucible is placed in a furnace cavity of heating equipment.
After the pressure in the furnace is stabilized, the temperature is raised to 850 ℃ at the speed of 10 ℃/min, and the temperature is maintained for 20 minutes, so that the melted Mg can fully permeate into the three-dimensional porous framework.
And cooling and solidifying to form the MAX reinforced magnesium-based composite material.
By testing the sample prepared by the method, the microstructure of the three-dimensional porous skeleton is shown in figure 1, and the microstructure of the obtained composite material is shown in figure 2 (wherein the light color is Ti2AlC, dark color Mg), the bending stress-strain curve is shown in fig. 3. It was further determined that the porosity of the three-dimensional porous skeleton was 56.75% on average, the density of the composite material was 1.86g/cm3 on average, the diameters of skeleton unit rings were 10 μm on average, the diameters of Mg phases were 50 μm on average, the flexural strength was 826MPa on average, and the hardness was 200HV on average.
Example four
This example provides a method for producing a MAX reinforced mg-based composite material, which is different from the third example in that the base powder used is Ti3AlC2Powder, wherein the metal is Mg alloy (the model is AZ91D), the compression molding pressure in the step S21 is 8Mpa, the sintering temperature in the step S22 is 1100 ℃, the Mg alloy required in the step three is 25g, the heating temperature is 900 ℃, and the heat preservation time is 30 min. Other steps and parameters are consistent.
By subjecting the sample obtained by the method toThe test shows that the microstructure of the three-dimensional porous skeleton is shown in FIG. 4, and the microstructure of the obtained composite material is shown in FIG. 5 (wherein, the light color is Ti3AlC2Dark AZ91D), the bending stress-strain curve is shown in fig. 6. Further, it was found that the porosity of the three-dimensional porous skeleton was 48.25% on average, the density of the composite material was 1.99g/cm3 on average, the diameter of the skeleton unit ring was 16 μm on average, the diameter of the Mg alloy phase was 9 μm on average, the flexural strength was 933MPa on average, and the hardness was 280HV on average.
As can be seen from the third comparative example, when the compression molding pressure was 4MPa, the corresponding volume fraction of cermet phase was 43.25%; when the compression molding pressure is 8MPa, the volume fraction of the corresponding metal ceramic phase is 51.75 percent, namely, the metal ceramic phase with different volume fractions can be obtained by controlling the compression molding pressure.
EXAMPLE five
The embodiment provides a method for manufacturing a MAX reinforced magnesium-based composite material, which comprises the following steps:
step one, providing base powder, wherein the base powder is Ti2AlC powder or Ti3AlC2Powder;
secondly, manufacturing a three-dimensional porous framework by using the base powder;
and step three, infiltrating the melted Mg or Mg alloy into the three-dimensional porous framework to form the MAX reinforced magnesium-based composite material.
Wherein the second step comprises:
and step S21, manufacturing and forming a three-dimensional porous framework blank by using a powder grouting process.
Mixing the base powder with deionized water to form slurry, wherein the base powder accounts for 40-70% of the mass of the slurry;
injecting the slip into a gypsum mold;
standing and curing to form the three-dimensional porous framework green body.
In this example, Ti in the material2AlC or Ti3AlC2The volume fraction of (A) increases with the mass fraction of the base powder in the slipLarge, small and small, thereby enabling to realize the pair of Ti2AlC or Ti3AlC2Adjustment of the volume fraction of (a).
And step S22, sintering the green body to form the three-dimensional porous framework.
Namely, drying the three-dimensional porous framework blank to constant weight;
heating to 750-1200 ℃ in a protective atmosphere;
keeping the constant temperature for 0.5h-2h to form the three-dimensional porous framework.
The third step comprises:
placing solid Mg or a solid Mg alloy on the three-dimensional porous skeleton;
heating to a temperature higher than the melting point of solid Mg or a solid Mg alloy in a protective atmosphere or a vacuum environment to melt the solid Mg or the solid Mg alloy;
keeping the constant temperature for not less than 5min, so that the melted Mg or Mg alloy permeates into the three-dimensional porous framework;
and cooling and solidifying to form the MAX reinforced magnesium-based composite material.
In the MAX reinforced Mg-based composite material prepared by the method disclosed in the embodiment, Ti2AlC or Ti3AlC2The cermet phase exists in a three-dimensional porous framework form, and structurally, the ceramic phase and the ceramic phase are respectively continuous in all directions and are three-dimensionally interlocked with each other, so that the problem of performance failure can be avoided, and the performance is ensured to be stable and reach the standard. Furthermore, a three-dimensional porous framework with uniformly distributed pores is prepared in advance, and then the three-dimensional porous framework is infiltrated with Ti2AlC or Ti3AlC2The powder has better wettability of Mg or Mg alloy, so that the composite material prepared by the method has compact structure, uniform components and no obvious defects.
In addition, the present embodiment can anticipate Ti by adjusting the pressure of the process2AlC or Ti3AlC2And can adjust Ti in the material in a wide range2AlC or Ti3AlC2So that its properties can be adjusted over a wide range to meet the differencePerformance requirements under the environment.
EXAMPLE six
The embodiment provides a method for manufacturing a MAX reinforced magnesium-based composite material, which comprises the following steps:
step one, providing 20g of base powder, wherein the base powder is Ti2AlC powder.
And step two, manufacturing a three-dimensional porous framework by using the base powder. The method comprises the following steps:
and step S21, manufacturing and forming a three-dimensional porous framework blank by using a powder grouting process.
Namely, 20g of base powder is added into 50g of deionized water, and the mixture is mechanically stirred uniformly to prepare a stable suspension state (namely powder slurry);
pouring the powder slurry into a gypsum mould and casting into a certain shape;
standing and curing, and curing the remaining powder after the liquid in the powder slurry is absorbed to obtain the three-dimensional porous framework blank.
And step S22, sintering the green body to form the three-dimensional porous framework.
Namely, drying the three-dimensional porous framework blank until the weight is constant, and then putting the blank into a crucible;
and (3) putting the crucible with the three-dimensional porous framework blank into a heating furnace, heating in a protective atmosphere at the heating rate of 5 ℃/min, heating to 900 ℃, preserving heat for 1h, and taking out after the furnace is cooled to room temperature to obtain the three-dimensional porous framework.
And step three, infiltrating the melted Mg or Mg alloy into the three-dimensional porous framework to form the MAX reinforced magnesium-based composite material.
Namely, 30g of solid Mg is weighed, and is mechanically polished, cleaned by acetone and alcohol, dried and the like to remove a surface oxide layer and impurities.
And ultrasonically cleaning the graphite crucible in an absolute ethyl alcohol solution for 5 minutes, and then drying.
The three-dimensional porous framework and the solid Mg are sequentially arranged in a graphite crucible (the solid Mg is arranged on the three-dimensional porous framework), and then the crucible is arranged in a furnace chamber of heating equipment.
After the pressure in the furnace is stabilized, the temperature is raised to 850 ℃ at the speed of 10 ℃/min, and the temperature is maintained for 20 minutes, so that the melted Mg can fully permeate into the three-dimensional porous framework.
And cooling and solidifying to form the MAX reinforced magnesium-based composite material.
By testing the sample prepared by the method, the microstructure of the three-dimensional porous skeleton is shown in FIG. 7, and the microstructure of the obtained composite material is shown in FIG. 8 (wherein the light color is Ti2AlC, dark color Mg). Further, it was found that the porosity of the three-dimensional porous skeleton was 64.77% on average, the density of the composite material was 1.81g/cm3 on average, the diameter of the skeleton unit ring was 30 μm on average, the diameter of the Mg phase was 70 μm on average, the flexural strength was 750MPa on average, and the hardness was 180HV on average.
EXAMPLE seven
This example provides a method for producing a MAX reinforced mg-based composite material, which is different from the sixth example in that the base powder used is Ti3AlC2And (3) taking 30g of deionized water in powder slurry casting in the step S21, wherein the sintering temperature in the step S22 is 1100 ℃, the required Mg alloy in the step three is 25g, the heating temperature is 900 ℃, and the heat preservation time is 30 min. Other steps and parameters are consistent.
By testing the sample prepared by the method, the microstructure of the three-dimensional porous skeleton is shown in FIG. 9, and the microstructure of the obtained composite material is shown in FIG. 10 (wherein the light color is Ti3AlC2And dark color AZ 91D). The average porosity of the three-dimensional porous skeleton is 49.54 percent, the average density of the composite material is 2.01g/cm3, the average diameter of skeleton unit rings is 15 mu m, the average diameter of Mg alloy phase is 7 mu m, the average bending strength is 960MPa, and the average hardness is 300 HV.
Example eight
The embodiment provides a method for manufacturing a MAX reinforced magnesium-based composite material, which comprises the following steps:
step one, providing base powder, wherein the base powder is Ti2AlC powder or Ti3AlC2Powder;
secondly, manufacturing a three-dimensional porous framework by using the base powder;
and step three, infiltrating the melted Mg or Mg alloy into the three-dimensional porous framework to form the MAX reinforced magnesium-based composite material.
Wherein the second step comprises:
placing the base powder in a hot-pressing mold;
heating to 750-1200 ℃ in protective atmosphere or vacuum environment, and pressurizing to 2-20 MPa;
keeping constant temperature and constant pressure for 0.5-3 h to form the three-dimensional porous skeleton.
The third step comprises:
placing solid Mg or a solid Mg alloy on the three-dimensional porous skeleton;
heating to a temperature higher than the melting point of solid Mg or a solid Mg alloy in a protective atmosphere or a vacuum environment to melt the solid Mg or the solid Mg alloy;
keeping the constant temperature for not less than 5min, so that the melted Mg or Mg alloy permeates into the three-dimensional porous framework;
and cooling and solidifying to form the MAX reinforced magnesium-based composite material.
The MAX reinforced magnesium-based composite material prepared by the method disclosed in the embodiment is Ti2AlC or Ti3AlC2The cermet phase exists in a three-dimensional porous framework form, and structurally, the ceramic phase and the ceramic phase are respectively continuous in all directions and are three-dimensionally interlocked with each other, so that the problem of performance failure can be avoided, and the stable performance is ensured to reach the standard. Furthermore, a three-dimensional porous framework with uniformly distributed pores is prepared in advance, and then the three-dimensional porous framework is infiltrated with Ti2AlC or Ti3AlC2The powder has better wettability of Mg or Mg alloy, so that the composite material prepared by the method has compact structure, uniform components and no obvious defects.
In addition, the present embodiment can also anticipate Ti by adjusting the pressure in step two2AlC or Ti3AlC2And can be adjusted over a wide rangeIn the material Ti2AlC or Ti3AlC2So that the performance thereof can be adjusted within a wide range to meet the performance requirements under different environments.
Example nine
The embodiment provides a method for manufacturing a MAX reinforced magnesium-based composite material, which comprises the following steps:
step one, providing 20g of base powder, wherein the base powder is Ti2AlC powder.
Secondly, manufacturing a three-dimensional porous framework by using the base powder;
that is, the base powder is placed in a hot-pressing mold, in this embodiment, the hot-pressing mold is preferably a graphite mold;
placing the hot-pressing die and the basic powder in a furnace chamber of heating equipment, vacuumizing, filling protective gas argon and the like, heating and pressurizing after the pressure in the furnace is stable, wherein the heating rate is 5 ℃/min, heating to 900 ℃, then preserving heat for 1h, keeping the pressure at 4MPa, cooling the furnace to room temperature, and then taking out to obtain Ti with certain strength2Three-dimensional porous skeleton of AlC.
And step three, infiltrating the melted Mg or Mg alloy into the three-dimensional porous framework to form the MAX reinforced magnesium-based composite material.
Namely, 30g of solid Mg is weighed, and is mechanically polished, cleaned by acetone and alcohol, dried and the like to remove a surface oxide layer and impurities.
And ultrasonically cleaning the graphite crucible in an absolute ethyl alcohol solution for 5 minutes, and then drying.
The three-dimensional porous framework and the solid Mg are sequentially arranged in a graphite crucible (the solid Mg is arranged on the three-dimensional porous framework), and then the crucible is arranged in a furnace chamber of heating equipment.
After the pressure in the furnace is stabilized, the temperature is raised to 850 ℃ at the speed of 10 ℃/min, and the temperature is maintained for 20 minutes, so that the melted Mg can fully permeate into the three-dimensional porous framework.
And cooling and solidifying to form the MAX reinforced magnesium-based composite material.
By testing the sample prepared by the method, the microstructure of the three-dimensional porous skeleton is shown in FIG. 11, and the microstructure of the obtained composite material is shown in FIG. 12 (wherein the light color is Ti2AlC, dark color Mg). The average porosity of the three-dimensional porous skeleton is 59.66%, the average density of the composite material is 1.82g/cm3, the average diameter of skeleton unit rings is 20 μm, the average diameter of Mg phases is 40 μm, the average bending strength is 780MPa, and the average hardness is 230 HV.
Example ten
This example provides a method for producing a MAX reinforced mg-based composite material, which is different from the ninth example in that the base powder used is Ti3AlC2And (3) powder, wherein the metal is Mg alloy (the model is AZ91D), the sintering temperature in the second step is 1100 ℃, and the pressure is 10 MPa. The Mg alloy needed in the third step is 25g, the heating temperature is 900 ℃, and the heat preservation time is 30 min. Other steps and parameters are consistent.
By testing the sample prepared by the method, the microstructure of the three-dimensional porous skeleton is shown in FIG. 13, and the microstructure of the obtained composite material is shown in FIG. 14 (wherein the light color is Ti3AlC2And dark color AZ 91D). The average porosity of the three-dimensional porous skeleton is 45.67%, the average density of the composite material is 2.11g/cm3, the average diameter of skeleton unit rings is 16 mu m, the average diameter of Mg alloy phase is 12 mu m, the average bending strength is 950MPa, and the average hardness is 302 HV.
By combining the MAX reinforced mg-based composite material and the manufacturing method thereof disclosed in the above embodiments, and the results of the performance test, it can be obtained that:
the MAX reinforced magnesium-based composite material provided by the invention contains Ti2AlC or Ti3AlC2The metal ceramic phase exists in a three-dimensional porous framework form, the structure shows that the ceramic phase and the metal phase are respectively continuous in all directions, and three dimensions are interlocked with each other, so that the problem of performance failure can be avoided, and the stable performance can be ensured to reach the standard. And, by preparing a three-dimensional porous skeleton with uniformly distributed pores in advance, infiltrating and Ti2AlC or Ti3AlC2Mg or Mg alloy with better powder wettabilityThe composite material prepared by the method has compact structure, uniform components, no obvious defects, high strength, high damping, high wear resistance, light weight and the like.
In addition, the present embodiment can also anticipate Ti by adjusting the pressure or raw material mix ratio of the process2AlC or Ti3AlC2And can adjust Ti in the material in a wide range2AlC or Ti3AlC2So that its properties can be adjusted over a wide range, with Ti2AlC or Ti3AlC2The alloy replaces partial Mg, can improve the strength on the premise of not sacrificing light weight, is suitable for batch production, and can meet the performance requirements under different environments.
It should be noted that the crucible, mold, etc. mentioned in the embodiments of the present invention should be protected from being damaged at the required test temperature and not react with the test material, and include but not limited to graphite, gypsum, etc.
The sequence of the above embodiments is only for convenience of description and does not represent the advantages and disadvantages of the embodiments.
Finally, it should be noted that: the above examples are only used to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (11)

1. A MAX reinforced Mg-base composite material is prepared from Ti2AlC or Ti3AlC2The cermet phase and the metal phase of Mg or Mg alloy, characterized in that the cermet phase is present in the form of a three-dimensional porous skeleton within the MAX reinforced magnesium matrix composite.
2. A MAX reinforced magnesium based composite material according to claim 1, wherein the volume fraction of cermet phase is 30% -90%.
3. A MAX reinforced magnesium based composite material according to claim 2, wherein the volume fraction of cermet phase is 50% -90%. .
4. The MAX reinforced magnesium-based composite material according to claim 1, wherein the three-dimensional porous skeleton unit rings have a diameter size of 10nm-100 μ ι η and the metal phase has a diameter size of 10nm-100 μ ι η.
5. A method for manufacturing MAX reinforced magnesium-based composite material is characterized by comprising the following steps:
step one, providing base powder, wherein the base powder is Ti2AlC powder or Ti3AlC2Powder;
secondly, manufacturing a three-dimensional porous framework by using the base powder;
and step three, infiltrating the melted Mg or Mg alloy into the three-dimensional porous framework to form the MAX reinforced magnesium-based composite material.
6. The method of claim 5, wherein the second step comprises:
s21, manufacturing a three-dimensional porous framework blank by using a compression molding process or a powder grouting process;
and step S22, sintering the green body to form the three-dimensional porous framework.
7. The method of claim 6, wherein the step of forming the three-dimensional porous skeleton blank by a compression molding process comprises:
placing the base powder in a molding die;
applying pressure to 3-10 MPa;
keeping the constant pressure for 0.1h-2h to form the three-dimensional porous framework blank.
8. The method of claim 6, wherein the step of forming the three-dimensional porous skeleton blank by powder grouting comprises:
mixing the base powder with deionized water to form a powder slurry, wherein the base powder accounts for 40-70% of the mass of the powder slurry;
injecting the slip into a gypsum mold;
standing and curing to form the three-dimensional porous framework green body.
9. The method according to claim 6, wherein the step S22 includes:
drying the three-dimensional porous framework blank to constant weight;
heating to 750-1200 ℃ in a protective atmosphere;
keeping the constant temperature for 0.5h-2h to form the three-dimensional porous framework.
10. The method of claim 5, wherein the second step comprises:
placing the base powder in a hot-pressing mold;
heating to 750-1200 ℃ in protective atmosphere or vacuum environment, and pressurizing to 2-20 MPa;
keeping constant temperature and constant pressure for 0.5-3 h to form the three-dimensional porous skeleton.
11. The method of claim 5, wherein the third step comprises:
placing solid Mg or a solid Mg alloy on the three-dimensional porous skeleton;
heating to a temperature higher than the melting point of solid Mg or a solid Mg alloy in a protective atmosphere or a vacuum environment to melt the solid Mg or the solid Mg alloy;
keeping the constant temperature for not less than 5min, so that the melted Mg or Mg alloy permeates into the three-dimensional porous framework;
and cooling and solidifying to form the MAX reinforced magnesium-based composite material.
CN202110575078.6A 2021-05-26 2021-05-26 MAX reinforced magnesium-based composite material and manufacturing method thereof Withdrawn CN113308637A (en)

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