CN113149653A - MAX-phase ceramic-magnesium or magnesium alloy composite material and preparation method thereof - Google Patents

MAX-phase ceramic-magnesium or magnesium alloy composite material and preparation method thereof Download PDF

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CN113149653A
CN113149653A CN202110375866.0A CN202110375866A CN113149653A CN 113149653 A CN113149653 A CN 113149653A CN 202110375866 A CN202110375866 A CN 202110375866A CN 113149653 A CN113149653 A CN 113149653A
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phase ceramic
magnesium
max
max phase
magnesium alloy
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刘增乾
谷瑞成
刘艳艳
张哲峰
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Institute of Metal Research of CAS
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Abstract

The invention relates to a MAX phase ceramic-magnesium or magnesium alloy composite material and a preparation method thereof. The main technical scheme adopted is as follows: a preparation method of MAX phase ceramic-magnesium or magnesium alloy composite material comprises the following steps: putting MAX phase ceramic powder or MAX phase ceramic blank made of MAX phase ceramic powder into a heating zone in a heating furnace, and putting a magnesium block or a magnesium alloy block into a feeder of the heating furnace; heating MAX phase ceramic powder or MAX phase ceramic blank placed in a heating zone under a protective atmosphere or vacuum condition to a sintering temperature, and preserving heat for a first set time to obtain a sintered block; and regulating the temperature of the sintered block to the infiltration temperature, controlling the feeder to turn over, feeding the magnesium block or the magnesium alloy block onto the sintered block, keeping the temperature for a second set time to perform high-temperature infiltration, and cooling to obtain the MAX-phase ceramic-magnesium or magnesium alloy composite material. The invention is mainly used for preparing the MAX phase ceramic-magnesium or magnesium alloy composite material with light weight, high strength and wear resistance by a simple process.

Description

MAX-phase ceramic-magnesium or magnesium alloy composite material and preparation method thereof
Technical Field
The invention relates to the technical field of light high-strength structural materials, in particular to an MAX phase ceramic-magnesium or magnesium alloy composite material and a preparation method thereof.
Background
The light high-strength structural material has light weight and excellent mechanical property, has important significance for the engineering application fields such as aerospace and automobile industries, and has the advantages of load reduction, weight reduction, energy conservation, emission reduction and the like.
The magnesium alloy is used as a light metal structure 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, and poor wear resistance and corrosion resistance, and greatly limits the industrial application thereof. The defects can be effectively made up by a composite strengthening method, the strength, the creep resistance and the wear resistance of the magnesium alloy can be further improved by compounding the strengthening phase while the light weight advantage of the magnesium alloy is kept, and thus the application field of the magnesium alloy is widened.
From MAX phase ceramics (e.g. Ti)2AlC、Ti3AlC2Etc.) and magnesium metal can obtain comprehensive performance which can not be achieved by a single composition phase through complementation and correlation of the performances of all components on the premise of keeping the advantages of the performances of the two composition phases. However, most of the composite materials composed of MAX phase ceramics and magnesium metal are prepared by methods such as powder metallurgy and adding a second phase into a liquid melt, secondary furnace opening and multiple heating are needed in the operation process, and the prepared materials still need further machining or deformation treatment, so that the methods mostly have long production period and effectLow rate, multiple preparation steps, complex process, high energy waste and the like. And the volume fraction of the ceramic phase in the prepared MAX-phase ceramic-Mg and Mg alloy composite material is not high, so that the mechanical properties such as the strength, the wear resistance and the like of the material are difficult to improve.
Currently, the related art for making composite materials from MAX phase ceramics and magnesium metal is as follows:
the first related art is: the magnesium alloy (AZ91D) is heated in a crucible to be molten, and then is cooled to 450-550 ℃ to reach the semi-solid state of the magnesium alloy, and the stirring function is started. Mixing MAX ceramic phase (such as Ti)2AlC，Ti3SiC2Etc.) the powder is added into a high-speed stirred semi-solid Mg melt. And heating to 680-750 ℃ again, stirring for 10-30min, cooling to a semi-solid state, pouring the melt into a stainless steel mold, maintaining the pressure at 50-100MPa, and cooling to room temperature to obtain a blank. And (2) placing the blank into a medium-frequency induction coil for secondary heating, taking out the blank and placing the blank into a pressure chamber of a die casting machine and an extrusion casting machine or a die cavity of a forging press after the blank reaches a semi-solid state, and then carrying out pressure forming on the semi-solid blank to prepare the piston made of MAX-phase ceramic-Mg alloy.
The second related art is: ti with wear-resisting self-lubricating property preheated to 60 DEG C3SiC2Adding the ceramic powder into a high-speed stirred semi-solid AE44 magnesium alloy, heating the melt to 700 ℃, preserving the heat for 10min, and cooling to 500 ℃ again to obtain a semi-solid blank. And (2) placing the blank with the temperature of 500 ℃ into a press, carrying out hot back extrusion at the speed of 0.5mm/s to obtain a tubular cylinder sleeve blank, and carrying out rough turning, rough boring, turning process excircle, fine boring and fine turning excircle, rough honing, fine honing and platform honing on the tubular cylinder sleeve blank in sequence to obtain the magnesium-based cylinder sleeve finished product.
The preparation technology of the composite material consisting of the two MAX phase ceramics and the magnesium metal is mainly to add MAX phase ceramic powder into semi-solid magnesium or magnesium alloy and stir, to melt uniformly by heating, to cool to semi-solid state again, and then to extrude or pressurize the blank to obtain MAX reinforced magnesium-based composite material. The material properties are improved by the distribution of the MAX phase and the plastic deformation. However, the inventors of the present invention have found that the above-described technique has at least the following technical problems: (1) in the operation process, secondary furnace opening is needed (namely, after magnesium or magnesium alloy is heated to semi-solid state, the furnace opening is needed again for adding MAX phase ceramic powder), heating and temperature rising are carried out for many times, and the prepared material still needs further machining or deformation treatment, so that the preparation production period is long, the efficiency is low, the preparation steps are multiple, the process is complex, the energy waste degree is high, and the like. (2) According to the method, the ceramic powder is added into the semi-solid magnesium or magnesium alloy and stirred, but the ceramic powder cannot be added infinitely, and excessive addition can cause the powder to gather in the semi-solid magnesium or magnesium alloy, disperse unevenly and form defects, so that the composite material prepared by the prior art has a low MAX phase ceramic volume content of 5-30% basically and is not easy to adjust, and the hardness, the strength and the wear resistance can not meet most of actual application requirements. (3) When the composite material is prepared by the traditional mechanical stirring method, the ceramic phase and the metal phase can not be uniformly dispersed, the interface combination of the ceramic phase and the metal phase is weaker, the ceramic phase is blocked by the metal, the connectivity is poorer, and the mechanical property is influenced.
Disclosure of Invention
In view of the above, the present invention provides a MAX-phase ceramic-magnesium or magnesium alloy composite material and a preparation method thereof, and mainly aims to prepare a MAX-phase ceramic-magnesium or magnesium alloy composite material with excellent performance by a simple process.
In order to achieve the purpose, the invention mainly provides the following technical scheme:
in one aspect, an embodiment of the present invention provides a method for preparing a MAX-phase ceramic-magnesium or magnesium alloy composite material, including the following steps:
a material discharging step: putting MAX phase ceramic powder or MAX phase ceramic blank made of MAX phase ceramic powder into a heating zone in a heating furnace, and putting a magnesium block or a magnesium alloy block into a feeder of the heating furnace;
sintering: under the condition of protective atmosphere or vacuum, heating the MAX-phase ceramic powder or MAX-phase ceramic blank placed in the heating area to a sintering temperature, and preserving heat for a first set time to sinter the MAX-phase ceramic powder or MAX-phase ceramic blank into blocks to obtain sintered blocks;
and (3) high-temperature infiltration: and adjusting the temperature of the sintered block to the infiltration temperature, controlling the feeder to turn over, feeding a magnesium block or a magnesium alloy block onto the sintered block placed in the heating area, keeping the temperature for a second set time to carry out high-temperature infiltration, and cooling to obtain the MAX-phase ceramic-magnesium or magnesium alloy composite material.
Preferably, the MAX phase ceramic powder is Ti2AlC powder and Ti3AlC2One kind of powder.
Preferably, the method for preparing the MAX phase ceramic body from the MAX phase ceramic powder comprises the following steps: forming the MAX phase ceramic powder into a MAX phase ceramic blank by adopting cold press forming; preferably, the MAX phase ceramic powder is placed into a mold, the mold is placed on a hydraulic press, the pressure is increased to 3-10MPa, the pressure is maintained for 0.1-2h, and the mold is opened to obtain a MAX phase ceramic blank.
Preferably, the method for preparing the MAX phase ceramic body from the MAX phase ceramic powder comprises the following steps: adopting slip casting to mold the MAX phase ceramic powder into MAX phase ceramic blank; preferably, MAX phase ceramic powder and a dispersing agent are mixed and stirred to prepare MAX phase ceramic powder slurry; injecting the MAX-phase ceramic slurry into a gypsum mold, and obtaining a MAX-phase ceramic blank after liquid in the MAX-phase ceramic slurry is absorbed; further preferably, the dispersant is deionized water; preferably, in the MAX phase ceramic powder slurry, the mass fraction of MAX phase ceramic powder is 40-70%.
Preferably, in the discharging step: the MAX phase ceramic powder is placed in a graphite mold, and the graphite mold is placed in a heating zone of a heating furnace.
Preferably, in the sintering step: the porosity of the sintered block is 15-70%, and the pore size is 10nm-100 μm.
Preferably, the mass ratio of the MAX phase ceramic powder to the Mg block or the Mg alloy block is less than or equal to 1: 2.
preferably, in the sintering step: the sintering temperature is 750-1200 ℃, and the heat preservation is carried out for 0.5-2h at the sintering temperature.
Preferably, in the high temperature infiltration step: if the batch feeder is placed with the magnesium blocks, the infiltration temperature is higher than the melting point of magnesium; if the batch feeder is placed with the magnesium alloy block, the infiltration temperature is higher than the melting point of the magnesium alloy; preferably, the infiltration temperature is 750-900 ℃; preferably, the second set time of incubation is at least 5 min.
Preferably, the heating furnace includes:
a furnace chamber;
a base disposed at an inner bottom of the cavity; wherein, the base is used for placing a heating container; the heating container is used for containing MAX phase ceramic powder or MAX phase ceramic blank (preferably, the heating container is a graphite crucible or a graphite mold);
the heating body is internally provided with an annular heating device which is used for heating the heating container arranged on the base; wherein the heating container is positioned in a heating zone surrounded by the annular heating device;
the feeding device is provided with a material containing structure, and the material containing structure is positioned in the furnace cavity and is close to the inner top of the furnace cavity; the material containing structure is used for placing magnesium blocks or magnesium alloy blocks, and the magnesium blocks or the magnesium alloy blocks are thrown onto the sintered blocks by controlling the material throwing device to turn over.
Preferably, the feeder is provided with a feeding rod, and the feeding rod is provided with a first end and a second end which are oppositely arranged, wherein the first end of the feeding rod is positioned in the furnace cavity, and the material containing structure is positioned at the first end of the feeding rod; the second end of the feeding rod is positioned outside the furnace chamber; preferably, the feeding rod is rotatably connected with the furnace chamber, so that the feeder can be turned over for feeding; preferably, the feeding rod is slidably connected to the furnace chamber, so that the length of the feeding rod in the furnace chamber is adjustable (preferably, the second end of the feeding rod is controlled to perform drawing, pushing (adjusting the length in the furnace chamber) and overturning, and the second end of the feeding rod has a rotation scale and a drawing and withdrawing mark, and the overturning angle and the extending length can be adjusted according to the scale and the mark).
On the other hand, the embodiment of the invention provides a MAX-phase ceramic-magnesium or magnesium alloy composite material, wherein the MAX-phase ceramic-magnesium or magnesium alloy composite material is a three-dimensional penetrating structure with a MAX-phase ceramic as a framework and Mg or Mg alloy infiltrated into the framework;
preferably, in the MAX phase ceramic-magnesium or magnesium alloy composite, the volume fraction of the MAX phase ceramic is higher than 30%, preferably 50-85%;
preferably, the MAX phase ceramic is Ti2AlC ceramic or Ti3AlC2A ceramic; further preferably, the MAX phase ceramic-magnesium or magnesium alloy composite material has a hardness of 200-300HV and a density of 1.8-2.1g/cm3The bending strength is 750MPa to 1 Gpa;
preferably, the MAX-phase ceramic-magnesium or magnesium alloy composite material is prepared by any one of the above methods for preparing a MAX-phase ceramic-magnesium or magnesium alloy composite material.
Compared with the prior art, the MAX-phase ceramic-magnesium or magnesium alloy composite material and the preparation method thereof have the following beneficial effects:
on one hand, the preparation method of the MAX-phase ceramic-magnesium or magnesium alloy composite material provided by the embodiment of the invention comprises the steps of firstly placing a MAX-phase ceramic blank into a heating zone in a heating furnace, placing a magnesium block or a magnesium alloy block on a controllable feeder on the heating furnace, then vacuumizing the heating furnace or introducing protective gas for treatment, heating the MAX-phase ceramic blank to a sintering temperature, keeping the temperature for a first set time to obtain a sintered block, then adjusting the temperature of the MAX-phase ceramic blank to the infiltration temperature, stopping applying pressure, controlling the feeder to turn over MAX, adding a Mg block or a Mg alloy block onto the sintered block, keeping the temperature for a second set time, and cooling to obtain the MAX-phase ceramic-magnesium or magnesium alloy composite material. Therefore, the preparation method of the MAX-phase ceramic-magnesium or magnesium alloy composite material provided by the invention is simple and convenient, can be continuously operated, does not need secondary blow-in and repeated heating, and does not need subsequent deformation processing, thereby having the advantages of high production efficiency, short period, low cost, energy conservation and the like. Selecting Ti2AlC or Ti3AlC2The powder acts as a ceramic phase due to Ti2AlC or Ti3AlC2The composite material has good wettability with Mg or Mg alloy interface, complete infiltration and is not easy to form defects such as holes and the like, so that the mechanical property of the composite material is further improved.
Further, in the preparation method of the embodiment of the invention, the porosity of the sintered block can be adjusted by adjusting the cold pressing pressure in cold press molding or the ratio of powder to slurry in slip casting or the quantity of ceramic powder in direct sintering in the process of preparing the MAX phase ceramic blank, and adjusting the heat preservation temperature and the heat preservation time in the pre-sintering step, so that the component content of the MAX phase ceramic blank is adjusted, and the hardness, the strength and the wear resistance of the MAX phase ceramic-magnesium or magnesium alloy composite material are improved.
It is further noted that: in the prior art, ceramic powder is mostly added into semi-solid magnesium or magnesium alloy and stirred, but the addition is not infinite, and excessive addition causes the powder to be clustered in the semi-solid magnesium or magnesium alloy, so that the powder is unevenly dispersed and forms defects, therefore, the composite MAX phase ceramic prepared by the prior art has low volume fraction. The scheme of the embodiment of the invention is that the ceramic powder is sintered firstly, and the porosity of the sintered framework can be controlled by controlling the process in the process, namely the relative content of the ceramic is controlled by controlling the content of magnesium or magnesium alloy, so that the volume fraction of MAX phase ceramic can be controlled.
On the other hand, the MAX phase ceramic-magnesium or magnesium alloy composite material provided by the invention is prepared by the preparation method of the MAX phase ceramic-magnesium or magnesium alloy composite material, wherein the MAX phase ceramic-magnesium or magnesium alloy composite material is a three-dimensional penetrating structure with MAX phase ceramic as a framework and Mg or Mg alloy penetrating into the framework, and the ceramic volume fraction in the MAX phase ceramic-Mg or Mg alloy composite material is higher than 30% (the MAX phase ceramic is Ti)2AlC or Ti3AlC2Ceramic) has the characteristics of high strength, high damping, high wear resistance, light weight and the like.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
Fig. 1 is a process diagram of a method for preparing a MAX-phase ceramic-Mg or Mg alloy composite material according to an embodiment of the present invention.
FIG. 2 shows Ti provided in example 1 of the present invention2The program control temperature-time curve of the preparation method of the AlC-Mg composite material.
FIG. 3 shows Ti prepared in example 1 of the present invention2Microscopic morphology of AlC-Mg composite material.
FIG. 4 shows Ti provided in example 2 of the present invention3AlC2-program controlled temperature-time curve of the preparation method of AZ91D magnesium alloy composite material.
FIG. 5 shows Ti prepared in example 2 of the present invention3AlC2-microscopic topography of AZ91D magnesium alloy composite.
Detailed Description
To further explain the technical means and effects of the present invention adopted to achieve the predetermined object, the following detailed description of the embodiments, structures, features and effects according to the present invention will be made with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
On one hand, the invention provides a preparation method of the MAX-phase ceramic-Mg or Mg alloy composite material, wherein the MAX-phase ceramic-Mg or Mg alloy composite material prepared by the preparation method is mainly used as a light high-strength structural material.
It should be noted that, the MAX phase ceramic-Mg or Mg alloy composite material provided by the present invention mainly uses two raw materials: first is Ti2AlC or Ti3AlC2Powder; second, Mg or Mg alloy blocks in which the metal phase (Mg or Mg alloy) is in excess to ensure completenessInfiltration (the dosage of MAX phase ceramic powder and metal phase has no specific proportional relation, and the Mg/Mg alloy is in excess filling in principle, so as to achieve the purpose of Mg/Mg alloy complete infiltration). Here, taking the heating furnace and the process principle shown in fig. 1 as an example, the specific preparation method is as follows:
ti is prepared by cold press molding and slip casting2AlC or Ti3AlC2The powder is formed into a green body and then a MAX phase ceramic green body 21 (i.e., Ti)2AlC or Ti3AlC2Green body) is added into a graphite crucible 14, the graphite crucible 14 and a base 11 surrounded by a heating body 12 (thermocouple) in a furnace chamber 1 of a heating furnace are placed in a protective atmosphere or vacuum, heated to a sintering temperature and kept warm for a first set time, the sintering is carried out to form blocks, the heat preservation is stopped, the temperature is reduced to an infiltration temperature, a metal block 22(Mg block or Mg alloy block) which is prepared and placed in a controllable telescopic and reversible feeder 13 is added onto the sintered blocks, the heat preservation is carried out for a second set time, and the MAX-phase ceramic-Mg or Mg alloy composite material is obtained after cooling.
The MAX phase ceramic body can be prepared by cold press molding and slip casting molding according to actual needs. Specifically, in the step of cold press molding: the pressure for compression molding is 3-10MPa, and the pressure maintaining time is 0.1-2 h. Specifically, in the slip casting step: deionized water as dispersant, drying Ti2AlC or Ti3AlC2The powder accounts for 40-70% of the total mass of the powder slurry.
Specifically, the set temperature during sintering is 750-. The set temperature for high-temperature infiltration is 750-.
For the above scheme, Ti can be directly added2AlC or Ti3AlC2Putting the powder into a graphite mould (or a graphite crucible), then putting the graphite mould on a base of a furnace chamber of a heating furnace, directly sintering the graphite mould into a sintered block, and then carrying out a high-temperature infiltration step.
In another aspect, embodiments of the present disclosure provide a MAX-phase ceramic-magnesium or magnesium alloy composite material. Prepared MAX phase ceramicsthe-Mg or Mg alloy composite material is a three-dimensional penetrating structure with MAX phase ceramics as a framework and Mg or Mg alloy infiltrated into the framework, wherein in the MAX phase ceramics-Mg or Mg alloy composite material, the volume fraction of the MAX phase ceramics is higher than 30%, and the MAX phase ceramics has the characteristics of high strength, good thermal conductivity, light weight, uniform and fine structure, excellent wear resistance and the like. Preferably, the MAX phase ceramic is Ti2AlC or Ti3AlC2A ceramic. Preferably, the MAX phase ceramic-Mg or Mg alloy composite material is prepared by the preparation method of the MAX phase ceramic-Mg or Mg alloy composite material.
The invention is further illustrated by the following specific experimental examples:
in the following examples, the sintering and high-temperature infiltration steps were carried out using the same heating furnace and a graphite crucible having a diameter of 26 mm.
Example 1
This example provides a Ti2The preparation method of AlC-Mg composite material adopts raw materials comprising Ti2AlC powder and Mg blocks. In which Ti was prepared in this example2The technological principle of the AlC-Mg composite material is shown in figure 1, and in the preparation process, a program control temperature-time curve arranged on a heating furnace is shown in figure 2, and the specific preparation steps are as follows:
preparation of Ti2An AlC blank body step: 20g of Ti2The AlC powder is uniformly placed in a mold. Then adjusting the stroke of the hydraulic press to a complete die opening state, and filling Ti2Placing the mold of AlC powder at the center of the hydraulic press, pressurizing to 4MPa, releasing pressure, adjusting the upper mold base to completely open the hydraulic press, taking out the mold and Ti2And (4) an AlC green body.
A material discharging step: ultrasonically cleaning a graphite crucible in an absolute ethyl alcohol solution for 5 minutes, drying the graphite crucible, and drying the prepared Ti2And uniformly placing the AlC blank into a graphite crucible, and placing the graphite crucible on a base surrounded by a thermocouple in a furnace cavity of a heating furnace. Weighing 30g of magnesium block, mechanically polishing to remove a surface oxide layer, sequentially cleaning in acetone and alcohol, blowing to dry by using a blower, and then placing on a controllable telescopic turnover feeder on a heating furnace.
Sintering: vacuumizing the heating furnace or introducing protective gas, heating the furnace chamber after the air pressure in the furnace is stable, wherein the heating rate is 5 ℃/min, heating to 1000 ℃, then preserving heat for 1h, and obtaining the sintered block after the heat preservation time is reached.
And (3) high-temperature infiltration: stopping heating, reducing the temperature to 800 ℃, turning over a feeder, feeding Mg blocks onto the sintered blocks in the graphite crucible, keeping the temperature for 20min, cooling the furnace to room temperature, and taking out to obtain Ti2AlC-Mg composite material.
Ti prepared in this example2The microscopic morphology of the AlC-Mg composite material is shown in FIG. 3 (light color is Ti)2AlC, dark color Mg). The analysis of FIG. 3 by Image-pro plus software revealed that: ti2Ti in AlC-Mg composite material2The volume fraction of AlC is 70.3 percent, and the average density of the composite material is 1.86g/cm3The flexural strength was 853MPa, and the hardness was 190 HV.
Example 2
This example provides a Ti3AlC2A method for preparing an — Mg alloy composite material, wherein the method for preparing the present example differs from example 1 as follows:
(1) the raw material used in this example included Ti3AlC2Powder and Mg alloy block with the model of AZ 91D;
(2) in the presence of Ti3AlC2Preparing Ti from the powder3AlC2When a blank is prepared: pressurizing to 8MPa, and then releasing the pressure;
(3) for Ti3AlC2When the green body is sintered, heating to 1200 ℃ and preserving heat;
(4) the mass of the Mg alloy block required by high-temperature infiltration is 25 g; and when the high-temperature infiltration is carried out, the temperature is reduced to 900 ℃, and the heat preservation time is 30 min.
Other steps and parameters are consistent.
This example prepares Ti3AlC2The programmed temperature-time curve of the AZ91D composite material is shown in FIG. 4, and the Ti finally obtained3AlC2The microstructure of the-AZ 91D composite material is shown in FIG. 5 (light color is Ti)3AlC2Deep color ofAZ 91D). The analysis of FIG. 5 by Image-pro plus software revealed that: ti3AlC2Ti in AZ91D composite3AlC2Is 81.7%, and the density of the composite material is 2.01g/cm on average3The flexural strength was 936MPa, and the hardness was 240 HV.
Example 3
This example prepares a Ti2AlC-Mg composite material, the adopted raw material comprises Ti2AlC powder and Mg blocks; the preparation method comprises the following specific steps:
preparation of Ti2An AlC blank body step: 20g of Ti2Adding AlC powder into 50g of deionized water, and mechanically stirring uniformly to prepare a stable suspension state to obtain Ti2AlC powder slurry; mixing Ti2Pouring the AlC slurry into gypsum mould and pouring to a certain shape until Ti is formed2Absorbing the liquid in the AlC powder slurry, and solidifying the rest powder to obtain Ti2And (4) an AlC green body.
A material discharging step: ultrasonically cleaning a graphite crucible in an absolute ethyl alcohol solution for 5 minutes, drying the graphite crucible, and drying the prepared Ti2And uniformly placing the AlC blank into a graphite crucible, and placing the graphite crucible on a base surrounded by a thermocouple in a furnace cavity of a heating furnace. Weighing 30g of Mg blocks, mechanically polishing to remove a surface oxide layer, sequentially cleaning in acetone and alcohol, blowing to dry by using a blower with cold air, and then placing on a feeding device capable of controlling stretching and overturning.
Sintering: vacuumizing the heating furnace or introducing protective gas, heating the furnace chamber at a heating rate of 5 ℃/min after the gas pressure in the furnace is stabilized, heating to 1000 ℃, and keeping the temperature for 1 h. And obtaining the sintered block after reaching the heat preservation time.
Infiltration: stopping heating, cooling to 800 deg.C, turning over the feeder to feed Mg blocks onto the sintered blocks in the graphite crucible, maintaining the temperature for 20min, cooling to room temperature, and taking out to obtain Ti2AlC-Mg composite material, the density of the composite material is measured to be 1.89g/cm on average3The flexural strength was 869MPa, and the hardness was 200 HV.
From the above example it follows that:
on one hand, the preparation method of the MAX-phase ceramic-magnesium or magnesium alloy composite material has the advantages of continuous operation, high production efficiency, short period, low cost, energy conservation and the like through the process steps of the embodiment. By comparison of example 1 with example 2, it can be seen that: if the temperature is properly raised in the sintering process, the compactness of the blank body is larger, the smaller the gap is, and the higher the content of the MAX-phase ceramic in the finally obtained MAX-phase ceramic-Mg or Mg alloy composite material is.
On the other hand, the MAX-phase ceramic-magnesium or magnesium alloy composite material prepared by the embodiment of the invention is a three-dimensional penetrating structure with MAX-phase ceramic as a framework and Mg or Mg alloy penetrating into the framework, wherein the volume fraction of MAX-phase ceramic is higher than 30%, and the MAX-phase ceramic-magnesium or magnesium alloy composite material has the characteristics of high strength, high wear resistance, light weight and the like. Therefore, the preparation method of the MAX-phase ceramic-Mg or Mg alloy composite material provided by the embodiment of the invention has considerable application prospect in the technical field of preparation of light high-strength structural materials.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.

Claims (10)

1. A preparation method of MAX phase ceramic-magnesium or magnesium alloy composite material is characterized by comprising the following steps:
a material discharging step: putting MAX phase ceramic powder or MAX phase ceramic blank made of MAX phase ceramic powder into a heating zone in a heating furnace, and putting a magnesium block or a magnesium alloy block into a feeder of the heating furnace;
sintering: under the condition of protective atmosphere or vacuum, heating the MAX-phase ceramic powder or MAX-phase ceramic blank placed in the heating area to a sintering temperature, and preserving heat for a first set time to sinter the MAX-phase ceramic powder or MAX-phase ceramic blank into blocks to obtain sintered blocks;
and (3) high-temperature infiltration: and adjusting the temperature of the sintered blocks to an infiltration temperature, controlling the feeder to turn over, feeding magnesium blocks or magnesium alloy blocks onto the sintered blocks placed in the heating area, keeping the temperature for a second set time to carry out high-temperature infiltration, and cooling to obtain the MAX-phase ceramic-magnesium or magnesium alloy composite material.
2. The method of claim 1, wherein the MAX phase ceramic powder is Ti2AlC powder and Ti3AlC2One kind of powder.
3. The method of preparing a MAX phase ceramic-magnesium or magnesium alloy composite material of claim 1 or 2, wherein the method of making a MAX phase ceramic body from the MAX phase ceramic powder is as follows:
forming the MAX phase ceramic powder into a MAX phase ceramic blank by adopting cold press forming;
preferably, the MAX phase ceramic powder is placed into a mold, the mold is placed on a hydraulic press, the pressure is increased to 3-10MPa, the pressure is maintained for 0.1-2h, and the mold is opened to obtain a MAX phase ceramic blank.
4. The method of preparing a MAX phase ceramic-magnesium or magnesium alloy composite material of claim 1 or 2, wherein the method of making a MAX phase ceramic body from the MAX phase ceramic powder is as follows:
adopting slip casting to mold the MAX phase ceramic powder into MAX phase ceramic blank;
preferably, MAX phase ceramic powder and a dispersing agent are mixed and stirred to prepare MAX phase ceramic powder slurry; injecting the MAX-phase ceramic slurry into a gypsum mold, and obtaining a MAX-phase ceramic blank after liquid in the MAX-phase ceramic slurry is absorbed; further preferably, the dispersant is deionized water; preferably, in the MAX phase ceramic powder slurry, the mass fraction of MAX phase ceramic powder is 40-70%.
5. The method of preparing a MAX phase ceramic-magnesium or magnesium alloy composite material of claim 1 or 2, wherein in the step of discharging: putting MAX phase ceramic powder into a graphite mold, and putting the graphite mold filled with MAX phase ceramic powder into a heating zone of a heating furnace; and/or
In the sintering step: the porosity of the sintered block is 15-70%, and the pore size is 10nm-100 μm.
6. The method of preparing a MAX phase ceramic-magnesium or magnesium alloy composite material of claim 1 or 2, wherein the mass ratio of the MAX phase ceramic powder to the Mg mass or Mg alloy mass is less than or equal to 1: 2.
7. a method of preparing a MAX phase ceramic-magnesium or magnesium alloy composite material as claimed in claim 1 or 2,
in the sintering step: the sintering temperature is 750-1200 ℃, and the heat preservation is carried out for 0.5-2h at the sintering temperature; and/or
In the high-temperature infiltration step: if the batch feeder is placed with the magnesium blocks, the infiltration temperature is higher than the melting point of magnesium; if the batch feeder is placed with the magnesium alloy block, the infiltration temperature is higher than the melting point of the magnesium alloy; preferably, the infiltration temperature is 750-900 ℃; preferably, the second set time is at least 5 min.
8. A method of producing a MAX phase ceramic-magnesium or magnesium alloy composite material as claimed in any of claims 1 to 7, wherein the furnace comprises:
a furnace chamber;
a base disposed at an inner bottom of the cavity; wherein, the base is used for placing a heating container; the heating container is used for accommodating MAX phase ceramic powder or MAX phase ceramic green body;
the heating body is internally provided with an annular heating device which is used for heating the heating container arranged on the base; wherein the heating container is positioned in a heating zone surrounded by the annular heating device;
the feeding device is provided with a material containing structure, and the material containing structure is positioned in the furnace cavity and is close to the inner top of the furnace cavity; the material containing structure is used for placing magnesium blocks or magnesium alloy blocks, and the magnesium blocks or the magnesium alloy blocks are thrown onto the sintered blocks by controlling the material throwing device to turn over.
9. The method of preparing a MAX phase ceramic-magnesium or magnesium alloy composite material of claim 8,
the feeding device is provided with a feeding rod, the feeding rod is provided with a first end and a second end which are oppositely arranged, the first end of the feeding rod is positioned in the furnace cavity, and the material containing structure is positioned at the first end of the feeding rod; the second end of the feeding rod is positioned outside the furnace chamber; preferably, the feeding rod is rotatably connected with the furnace chamber, so that the feeder can be turned over for feeding; preferably, the feeding rod is connected with the furnace chamber in a sliding manner, so that the length of the feeding rod in the furnace chamber is adjustable; and/or
A temperature control system is arranged on the heating furnace; wherein, the temperature control system is connected with the heating body.
10. The MAX-phase ceramic-magnesium or magnesium alloy composite material is characterized in that the MAX-phase ceramic-magnesium or magnesium alloy composite material is a three-dimensional penetrating structure with MAX-phase ceramic as a framework and Mg or Mg alloy penetrating into the framework; in the MAX phase ceramic-magnesium or magnesium alloy composite, the volume fraction of the MAX phase ceramic is higher than 30%, preferably 50-85%;
preferably, the MAX phase ceramic is Ti2AlC ceramic or Ti3AlC2A ceramic; further preferably, the MAX phase ceramic-magnesium or magnesium alloy composite material has a hardness of 200-300HV and a density of 1.8-2.1g/cm3The bending strength is 750MPa to 1 Gpa;
preferably, the MAX phase ceramic-magnesium or magnesium alloy composite is prepared by the method of preparation of a MAX phase ceramic-magnesium or magnesium alloy composite according to any of claims 1 to 9.
CN202110375866.0A 2021-04-08 2021-04-08 MAX-phase ceramic-magnesium or magnesium alloy composite material and preparation method thereof Pending CN113149653A (en)

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Application publication date: 20210723