CN112281086B - Preparation method of high-heat-resistance three-dimensional woven fiber reinforced magnesium-based composite material - Google Patents

Preparation method of high-heat-resistance three-dimensional woven fiber reinforced magnesium-based composite material Download PDF

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CN112281086B
CN112281086B CN202011214577.4A CN202011214577A CN112281086B CN 112281086 B CN112281086 B CN 112281086B CN 202011214577 A CN202011214577 A CN 202011214577A CN 112281086 B CN112281086 B CN 112281086B
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liquid
composite material
carbon fiber
packaging mold
carbon dioxide
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CN112281086A (en
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王振军
蔡长春
徐志锋
余欢
杨伟
熊博文
汪志太
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Nanchang Hangkong University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02—Pretreatment of the fibres or filaments
    • C22C47/06—Pretreatment of the fibres or filaments by forming the fibres or filaments into a preformed structure, e.g. using a temporary binder to form a mat-like element
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02—Pretreatment of the fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02—Pretreatment of the fibres or filaments
    • C22C47/04—Pretreatment of the fibres or filaments by coating, e.g. with a protective or activated covering
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/08—Making alloys containing metallic or non-metallic fibres or filaments by contacting the fibres or filaments with molten metal, e.g. by infiltrating the fibres or filaments placed in a mould
    • C22C47/12—Infiltration or casting under mechanical pressure
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C22C49/04—Light metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments

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Abstract

The invention relates to the technical field of magnesium-based composite materials, in particular to a preparation method of a high-heat-resistance three-dimensional woven fiber reinforced magnesium-based composite material. The method comprises the following steps: placing the carbon fiber preform in a packaging mold; removing the photoresist: introducing liquid carbon dioxide into the packaging mold under the pressure and temperature which enable the carbon dioxide to be in a liquid state, enabling the liquid carbon dioxide to completely immerse the carbon fiber preform, and soaking for 20-24 hours; surface modification: placing the packaging mold in a sealed environment of 950 plus materials at 980 ℃, and carrying out heat preservation and activation for 90-120 min; infiltration: and (3) placing the packaging mold in a vacuum pressure impregnation device, pressing the molten liquid metal into the packaging mold through air pressure to impregnate the carbon fiber preform, and obtaining the composite material. The carbon dioxide is utilized to carry out gas phase oxidation on the surface of the carbon fiber, and the carbon dioxide and unsaturated carbon atoms on the surface of the carbon fiber are subjected to chemical reaction, so that active oxygen-containing functional groups are added on the surface of a carbon fiber preform, and the interface bonding strength of the carbon fiber composite material is improved by adding the gas surface roughness.

Description

Preparation method of high-heat-resistance three-dimensional woven fiber reinforced magnesium-based composite material
Technical Field
The invention relates to the technical field of magnesium-based composite materials, in particular to a preparation method of a high-heat-resistance three-dimensional woven fiber reinforced magnesium-based composite material.
Background
Composite materials, as the name implies, are a class of multiphase systems composed of multiple material phases. The composite material mainly comprises three parts: reinforcement material, matrix material, interface material. The reinforcement material has high strength and modulus, is distributed in the composite material in a solid form in the preparation process, is also called as a dispersion phase, can be composed of fibers, graphite, ceramics and metals, plays a bearing role in the structure, and plays roles of reinforcement, toughness resistance, wear resistance, heat resistance, corrosion resistance, thermal vibration resistance and the like in the composite material. The matrix material is uninterrupted in the composite material, also called as continuous phase, and mainly has the functions of bonding the reinforcement material into a solid whole, protecting the reinforcement material, transmitting load and preventing crack propagation. The interface material is a bridge connecting the reinforcement and the substrate. The metal-based composite material is a material compounded by taking fibers, whiskers or particles as a reinforcement and a matrix metal or alloy, and has the characteristics of high specific strength, high specific modulus, good toughness, high impact resistance, good wear resistance, remarkable damping performance, good electrical conductivity, excellent thermal conductivity, no aging and the like. With the rapid development of modern high and new technologies, especially the continuous progress in the technology-intensive fields such as aerospace, the design and manufacture process of aircrafts face challenges in terms of structural function, weight, strength and the like. The continuous carbon fiber reinforced magnesium-based composite material has the advantages of excellent mechanical property, good space stability, high damping resistance, low thermal expansion coefficient, light weight, high strength and the like, has a great application prospect, and is paid more attention to the high-tech fields of aerospace and the like.
However, the wettability of the carbon fiber and the magnesium matrix is poor, the wetting angle of the carbon fiber and the magnesium solution is less than 90 ℃ when the temperature is over 1000 ℃, and the temperature is extremely easy to oxidize and burn for magnesium alloy and is generally not feasible. Therefore, the improvement of the wettability of the carbon fiber and the magnesium matrix can be achieved only by means of carbon fiber modification, surface coating treatment, addition of alloy elements and the like.
For example, patent document No. CN104947008A discloses a method for preparing a carbon fiber reinforced magnesium-based composite material, which comprises using magnesium and carbon fibers as raw materials, and subjecting the carbon fibers to surface galvanization, ball milling, powder mixing, die filling, vacuum discharge plasma sintering, and rolling to obtain the carbon fiber reinforced magnesium-based composite material. The wettability of the carbon fiber and a magnesium matrix is improved through the zinc coating on the surface of the carbon fiber. For another example, patent document CN101250677A discloses a titanium dioxide coated carbon fiber reinforced magnesium matrix composite material in the technical field of such composite materials. The composite material is composed of magnesium alloy and carbon fiber with a titanium dioxide coating, wherein the weight percentage of the added reinforcing phase is as follows: 30-70% of carbon fiber, 6-8 μm of carbon fiber monofilament diameter and the balance of magnesium alloy. The invention improves the wettability between magnesium and carbon fiber by using the titanium dioxide coating on the surface of the carbon fiber. Coating treatment is mostly used at present, but the content of oxygen-containing polar groups on the surface of carbon fiber is low, so that the coating is difficult to adhere to the surface of the carbon fiber closely.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of a high-heat-resistance three-dimensional woven fiber reinforced magnesium matrix composite.
The technical scheme for solving the problems is to provide a preparation method of a high heat-resistant three-dimensional woven fiber reinforced magnesium matrix composite, which comprises the following steps:
(1) preparing a carbon fiber preform, and placing the carbon fiber preform in a packaging mold;
(2) removing the photoresist: introducing liquid carbon dioxide into the packaging mold under the pressure and temperature which enable the carbon dioxide to be in a liquid state, enabling the liquid carbon dioxide to completely immerse the carbon fiber preform, and soaking for 20-24 hours;
(3) surface modification: placing the packaging mold in a sealed environment of 950 plus materials at 980 ℃, and carrying out heat preservation and activation for 90-120 min;
(4) infiltration: and placing the packaging mold in a vacuum pressure infiltration device, pressing molten liquid metal into the packaging mold through air pressure to infiltrate the carbon fiber preform, and obtaining the composite material.
Preferably, the carbon fiber preform is a three-dimensional five-direction braided graphite fiber M40. The three-dimensional five-direction knitting is based on three-dimensional four-direction knitting and is obtained by adding axially immovable yarns in all directions to a three-dimensional four-direction knitting material.
Preferably, the molten liquid metal for infiltration is one or more of an AZ91D magnesium alloy, an AZ31D magnesium alloy and an AZ61D magnesium alloy. The alloys have higher strength, good melt fluidity and lower hot cracking tendency, and can effectively improve the combination degree of the matrix and the carbon fiber and the strength of the composite material when being used as the matrix of the magnesium-based composite material. In the present invention, preferably, the molten liquid metal for infiltration is AZ91D magnesium alloy.
The composite material is prepared by adopting a vacuum pressure infiltration method, and as the optimization of the invention, in the step (4), the technological parameters of the vacuum pressure infiltration are as follows: the preheating temperature is 550-.
In order to protect the fibers from electrostatic friction during the manufacturing process of the carbon fibers, a layer of organic glue is often coated on the surfaces of the fibers, so that the carbon fibers need to be subjected to glue removal treatment during the preparation of the composite material. In this application, adopt liquid carbon dioxide as solvent extraction to remove the glue, it can dissolve multiple organic matter, and low pollution, low residue. The bonding effect between the fibers subjected to the degumming treatment and the matrix material is better.
On this basis, this application has utilized carbon dioxide again to carry out the characteristic of vapor phase oxidation as mild oxidant, and it takes place chemical reaction with the unsaturated carbon atom on carbon fiber surface for carbon fiber perform increases active oxygen-containing functional group on the surface, increases the interface bonding strength of gas surface roughness in order to improve carbon-fibre composite simultaneously.
Meanwhile, the liquid carbon dioxide can be gasified in the heating process, so that the carbon fiber preform can expand, the impregnation of subsequent liquid metal is facilitated, and the residual stress can be reduced.
In the gas phase oxidation, the oxidation conditions are different, the mechanical properties of the composite material are also different, and a plurality of uneven grooves are formed on the surface of the carbon fiber by rapid oxidation, as the optimization of the invention, in the step (3), firstly, the temperature is increased to 550-600 ℃ at the speed of 3-5 ℃/min, then, the temperature is increased to 950-980 ℃ at the speed of 10-15 ℃/min, and then, the heat preservation and activation are carried out.
In order to further improve the bonding between the carbon fiber preform and the metal matrix, it is preferable that step (4) is performed under vibration conditions. The vibration can play a role in stirring, promotes the flow of liquid metal, improves the wettability between fibers and metal, enables the fibers to be uniformly distributed in the metal, and improves the bonding strength between the fibers and the metal. Preferably, the vibration is carried out under ultrasonic waves of 15 to 20 kHz.
In order to further improve the wettability, as a preferable aspect of the present invention, in the step (3), after the activation by heat preservation, a coating treatment is further included: introducing a sol solution into the packaging mold to enable the sol solution to completely immerse the carbon fiber preform, discharging the sol solution after soaking for 5-8h, and drying the packaging mold at the temperature of 450-490 ℃; the sol solution is one or more of SiO2, TiO2 and ZrO 2.
As a preference of the invention, the encapsulating mould is immersed under ultrasound at 15-20 kHz.
Preferably, the drying is carried out by firstly heating to 150-180 ℃ for drying for 30-45min and then heating to 450-490 ℃ for drying for 60-90 min.
Preferably, the temperature is raised to 150-180 ℃ at a rate of 1-2 ℃/min and to 450-490 ℃ at a rate of 5-7 ℃/min.
The invention has the beneficial effects that:
in this application, adopt liquid carbon dioxide as solvent extraction to remove the glue, it can dissolve multiple organic matter, and low pollution, low residue. The bonding effect between the fibers subjected to the degumming treatment and the matrix material is better. On this basis, this application has utilized carbon dioxide again to carry out the characteristic of vapor phase oxidation as mild oxidant, and it takes place chemical reaction with the unsaturated carbon atom on carbon fiber surface for carbon fiber perform increases active oxygen-containing functional group on the surface, increases the interface bonding strength of gas surface roughness in order to improve carbon-fibre composite simultaneously. Meanwhile, the liquid carbon dioxide can be gasified in the heating process, so that the carbon fiber preform can expand, the impregnation of subsequent liquid metal is facilitated, and the residual stress can be reduced.
After the gas phase oxidation, the surface activity of the carbon fiber is enhanced, and at the moment, the carbon fiber is subjected to coating treatment, so that the adhesion rate of the coating on the surface of the carbon fiber can be improved, and the wettability between the carbon fiber and metal is improved.
Detailed Description
The following are specific embodiments of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
Example 1
A preparation method of a high heat-resistant three-dimensional woven fiber reinforced magnesium matrix composite material comprises the following steps:
(1) preparing a carbon fiber preform, wherein the carbon fiber preform is woven into a preform plate with a three-dimensional five-direction microscopical structure by graphite fiber M40 of Jiangsu Xinliwea Kogyo through a four-step method. And then placing the carbon fiber preform in an encapsulation mold, wherein the encapsulation mold is formed by vertically fixing the carbon fiber preform with a high-temperature-resistant graphite gasket, manufacturing an outer package mold according to the size of the carbon fiber preform, and then putting the carbon fiber preform fixed by graphite into the mold. The packaging mold is provided with a liquid inlet for introducing liquid carbon dioxide and liquid metal subsequently.
(2) Removing the photoresist: at 20 ℃ and 5.6X 106And (3) introducing liquid carbon dioxide into the packaging mold under the condition of Pa, so that the carbon fiber preform is completely immersed by the liquid carbon dioxide, and soaking for 22 hours after the liquid inlet is closed.
(3) Surface modification: and (3) placing the packaging mold in a closed environment, opening the liquid inlet, heating to 580 ℃ at the speed of 4 ℃/min, heating to 960 ℃ at the speed of 12 ℃/min, and then carrying out heat preservation and activation for 100 min.
(4) Infiltration: the packaging mold and the AZ91D magnesium alloy are respectively placed in an upper chamber and a lower chamber of a vacuum pressure infiltration device, a liquid inlet of the packaging mold faces downwards and faces towards the magnesium alloy, and a liquid lifting pipe is arranged, and is not inserted into the magnesium alloy at the beginning.
Vacuumizing and filling argon, and simultaneously preheating the fiber preform and the magnesium alloy at the preheating temperature of 580 ℃ for 1h to melt the magnesium alloy. Then argon in the furnace is discharged and the furnace is vacuumized to 10Pa, a crucible is lifted to enable a liquid lifting pipe to be inserted into the magnesium alloy molten metal, then nitrogen of 8MPa is filled into the whole device, the magnesium alloy molten metal is filled into a packaging mold along the liquid lifting pipe through air pressure difference, and the pressure is maintained for 20min at 720 ℃ and 8 MPa. And finally, taking out the packaging mold, naturally cooling to room temperature, and removing the packaging mold and the graphite to obtain the composite material.
The composite material thus obtained was cut into standard test specimens (20X 6X 2 mm) by a wheel cutter, and then the interlaminar shear strength ILSS (average of ten specimens) was measured by a three-point short beam method (span-thickness ratio of five to one) in a universal material testing machine, and the test results are shown in Table 1 below.
Example 2
A preparation method of a high heat-resistant three-dimensional woven fiber reinforced magnesium matrix composite material comprises the following steps:
(1) preparing a carbon fiber preform, wherein the carbon fiber preform is woven into a preform plate with a three-dimensional five-direction microscopical structure by graphite fiber M40 of Jiangsu Xinliwea Kogyo through a four-step method. The carbon fiber preform was then placed in an encapsulating mold adapted to the size of the fiber preform in the same production method as in example 1. The packaging mold is provided with two liquid inlets, one liquid inlet is provided with a liquid lifting pipe for liquid inlet of subsequent liquid metal, and the other liquid inlet is provided with a liquid conveying pipe for liquid inlet of liquid carbon dioxide.
(2) Removing the photoresist: the packaging mold and the AZ91D magnesium alloy are respectively placed in an upper chamber and a lower chamber of a vacuum pressure infiltration device, a liquid lifting pipe of the packaging mold faces downwards and faces towards the magnesium alloy, and at the beginning, the liquid lifting pipe is not inserted into the magnesium alloy, and meanwhile, a liquid conveying pipe is communicated with the outside. The vacuum pressure infiltration device is fixed on a vibration platform, and the vibration frequency is adjusted to be 18 kHz.
Closing the infusion tube, vacuumizing the vacuum pressure impregnation device, introducing argon into the vacuum pressure impregnation device, and adjusting the pressure to be 5.6 multiplied by 106Pa, and simultaneously controlling the temperature in the device to be 20 ℃. Then closing the liquid lifting pipe, opening the liquid conveying pipe, introducing liquid carbon dioxide into the packaging mold, and then closing the liquid conveying pipe to enable the liquid carbon dioxide to completely immerse the carbon fiberThe body was prepared and immersed for 20 hours.
(3) Surface modification: and opening the liquid lifting pipe, simultaneously heating up and preheating the carbon fiber preform and the magnesium alloy, firstly heating up to 550 ℃ at the speed of 3 ℃/min, then heating up to 950 ℃ at the speed of 10 ℃/min, and then carrying out heat preservation and activation for 120 min. During the period, most of the gasified carbon dioxide escapes to the vacuum pressure infiltration device, so that the pressure in the device rises, and a small part of the gasified carbon dioxide reacts with the carbon fiber to be activated.
(4) Infiltration: after the heat preservation and activation are finished, closing the liquid lifting pipe, cooling to 700 ℃, adjusting the pressure in the whole device to 7MPa, and starting the crucible lifting to enable the liquid lifting pipe to be inserted into the magnesium alloy molten metal. And after the interior of the packaging mold is vacuumized through a liquid conveying pipe, closing the liquid conveying pipe, opening a liquid lifting pipe, filling the packaging mold with magnesium alloy metal liquid along the liquid lifting pipe through air pressure difference, maintaining the pressure for 25min, taking out the packaging mold, naturally cooling to room temperature, and removing the packaging mold and graphite to obtain the composite material.
The composite material thus obtained was cut into standard test specimens (20X 6X 2 mm) by a wheel cutter, and then the interlaminar shear strength ILSS (average of ten specimens) was measured by a three-point short beam method (span-thickness ratio of five to one) in a universal material testing machine, and the test results are shown in Table 1 below.
Example 3
A preparation method of a high heat-resistant three-dimensional woven fiber reinforced magnesium matrix composite material comprises the following steps:
(1) preparing a carbon fiber preform, wherein the carbon fiber preform is woven into a preform plate with a three-dimensional five-direction microscopical structure by graphite fiber M40 of Jiangsu Xinliwea Kogyo through a four-step method. The carbon fiber preform was then placed in an encapsulating mold adapted to the size of the fiber preform in the same production method as in example 1.
(2) Removing the photoresist: at 20 ℃ and 5.6X 106And (3) introducing liquid carbon dioxide into the packaging mold under the condition of Pa, so that the carbon fiber preform is completely immersed by the liquid carbon dioxide, and soaking for 24 hours after the liquid inlet is closed.
(3) Surface modification: and (3) placing the packaging mold in a closed environment, opening the liquid inlet, heating to 600 ℃ at the speed of 5 ℃/min, heating to 980 ℃ at the speed of 15 ℃/min, and then carrying out heat preservation and activation for 90 min.
And naturally cooling, introducing a sol solution into the packaging mold to enable the sol solution to completely immerse the carbon fiber preform, soaking for 8 hours under 18kHz ultrasonic waves, discharging the sol solution, placing the packaging mold at 180 ℃ for drying for 45min, and then heating to 490 ℃ for drying for 90 min. Wherein the sol solution is SiO2Sol solution.
(4) Infiltration: the packaging mold and the AZ31D magnesium alloy are respectively placed in an upper chamber and a lower chamber of a vacuum pressure infiltration device, a liquid inlet of the packaging mold faces downwards and faces towards the magnesium alloy, and a liquid lifting pipe is arranged, and is not inserted into the magnesium alloy at the beginning.
Vacuumizing and filling argon, and simultaneously preheating the fiber preform and the magnesium alloy at the preheating temperature of 600 ℃ for 1h to melt the magnesium alloy. Then argon in the furnace is discharged and the furnace is vacuumized to 10Pa, a crucible is lifted to enable a liquid lifting pipe to be inserted into the magnesium alloy molten metal, then 9MPa of nitrogen is filled into the whole device, the magnesium alloy molten metal is filled into a packaging mold along the liquid lifting pipe through air pressure difference, and the pressure is maintained for 15min at 750 ℃ and 9 MPa. And finally, taking out the packaging mold, naturally cooling to room temperature, and removing the packaging mold and the graphite to obtain the composite material.
The composite material thus obtained was cut into standard test specimens (20X 6X 2 mm) by a wheel cutter, and then the interlaminar shear strength ILSS (average of ten specimens) was measured by a three-point short beam method (span-thickness ratio of five to one) in a universal material testing machine, and the test results are shown in Table 1 below.
Example 4
A preparation method of a high heat-resistant three-dimensional woven fiber reinforced magnesium matrix composite material comprises the following steps:
(1) preparing a carbon fiber preform, wherein the carbon fiber preform is woven into a preform plate with a three-dimensional five-direction microscopical structure by graphite fiber M40 of Jiangsu Xinliwea Kogyo through a four-step method. The carbon fiber preform was then placed in an encapsulating mold adapted to the size of the fiber preform in the same production method as in example 1. The packaging mold is provided with two liquid inlets, one liquid inlet is provided with a liquid lifting pipe for liquid inlet of subsequent liquid metal, and the other liquid inlet is provided with a liquid conveying pipe for liquid inlet of liquid carbon dioxide.
(2) Removing the photoresist: the packaging mold and the AZ61D magnesium alloy are respectively placed in an upper chamber and a lower chamber of a vacuum pressure infiltration device, a liquid lifting pipe of the packaging mold faces downwards and faces towards the magnesium alloy, and at the beginning, the liquid lifting pipe is not inserted into the magnesium alloy, and meanwhile, a liquid conveying pipe is communicated with the outside. The vacuum pressure infiltration device is fixed on a vibration platform, and the vibration frequency is adjusted to 15 kHz.
Closing the infusion tube, vacuumizing the vacuum pressure impregnation device, introducing argon into the vacuum pressure impregnation device, and adjusting the pressure to be 5.6 multiplied by 106Pa, and simultaneously controlling the temperature in the device to be 20 ℃. And then closing the liquid lifting pipe, opening the liquid conveying pipe, introducing liquid carbon dioxide into the packaging mold, closing the liquid conveying pipe, and completely immersing the fiber preform in the liquid carbon dioxide for 21 hours.
(3) Surface modification: and opening a lift tube, simultaneously heating up and preheating the carbon fiber preform and the magnesium alloy, firstly heating up to 560 ℃ at the speed of 4 ℃/min, then heating up to 970 ℃ at the speed of 14 ℃/min, and then carrying out heat preservation and activation for 110 min. During this period, most of the vaporized carbon dioxide escapes into the vacuum pressure impregnation apparatus, so that the pressure in the apparatus rises and a small portion reacts with the carbon fibers.
And then closing the liquid lifting pipe, opening the liquid conveying pipe, introducing sol solution into the packaging mold through the liquid conveying pipe, so that the carbon fiber preform is completely immersed in the sol solution, and after dipping for 5 hours, sucking out the sol solution through the liquid conveying pipe. Heating to 150 deg.C by vacuum pressure infiltration device, drying for 30min, heating to 450 deg.C, and drying for 60 min. Wherein the sol solution is TiO2 sol solution.
(4) Infiltration: the lift tube was kept closed and the temperature was raised to 710 ℃. Then the pressure in the whole device is adjusted to 7.5MPa, and the crucible is started to enable the liquid lifting pipe to be inserted into the magnesium alloy molten metal. And after the interior of the packaging mold is vacuumized through the infusion tube, closing the infusion tube, opening the liquid lifting tube, filling the packaging mold with magnesium alloy metal liquid along the liquid lifting tube through air pressure difference, maintaining the pressure for 22min, taking out the packaging mold, naturally cooling to room temperature, and removing the packaging mold and graphite to obtain the composite material.
The composite material thus obtained was cut into standard test specimens (20X 6X 2 mm) by a wheel cutter, and then the interlaminar shear strength ILSS (average of ten specimens) was measured by a three-point short beam method (span-thickness ratio of five to one) in a universal material testing machine, and the test results are shown in Table 1 below.
Example 5
A preparation method of a high heat-resistant three-dimensional woven fiber reinforced magnesium matrix composite material comprises the following steps:
(1) preparing a carbon fiber preform, wherein the carbon fiber preform is woven into a preform plate with a three-dimensional five-direction microscopical structure by graphite fiber M40 of Jiangsu Xinliwea Kogyo through a four-step method. The carbon fiber preform was then placed in an encapsulating mold adapted to the size of the fiber preform in the same production method as in example 1.
(2) Removing the photoresist: at 20 ℃ and 5.6X 106And (3) introducing liquid carbon dioxide into the packaging mold under the condition of Pa, so that the carbon fiber preform is completely immersed by the liquid carbon dioxide, and soaking for 24 hours after the liquid inlet is closed.
(3) Surface modification: and (3) placing the packaging mold in a closed box body, opening a liquid inlet, heating to 570 ℃ at the speed of 3.5 ℃/min, heating to 955 ℃ at the speed of 11 ℃/min, and then carrying out heat preservation and activation for 95 min.
And then introducing a sol solution into the packaging mold to enable the sol solution to completely immerse the carbon fiber preform, soaking for 6 hours under 20kHz ultrasonic waves, discharging the sol solution, placing the packaging mold at 160 ℃, drying for 40min, and then heating to 460 ℃ and drying for 80 min. Wherein the sol solution is ZrO2 sol solution.
(4) Infiltration: the packaging mold and the AZ31D magnesium alloy are respectively placed in an upper chamber and a lower chamber of a vacuum pressure infiltration device, a liquid inlet of the packaging mold faces downwards and faces towards the magnesium alloy, and a liquid lifting pipe is arranged, and is not inserted into the magnesium alloy at the beginning. The vacuum pressure infiltration device is fixed on a vibration platform, and the vibration frequency is adjusted to be 20 kHz.
Vacuumizing and filling argon, and simultaneously preheating the fiber preform and the magnesium alloy at 570 ℃ for 1h to melt the magnesium alloy. Then argon in the furnace is discharged and the furnace is vacuumized to 10Pa, a crucible is raised to enable a liquid lifting pipe to be inserted into the magnesium alloy molten metal, then nitrogen with the pressure of 8.5MPa is filled into the whole device, the magnesium alloy molten metal is filled into a packaging mold along the liquid lifting pipe through the air pressure difference, and the pressure is maintained for 18min at the temperature of 740 ℃ and the pressure of 8.5 MPa. And finally, taking out the packaging mold, naturally cooling to room temperature, and removing the packaging mold and the graphite to obtain the composite material.
The composite material thus obtained was cut into standard test specimens (20X 6X 2 mm) by a wheel cutter, and then the interlaminar shear strength ILSS (average of ten specimens) was measured by a three-point short beam method (span-thickness ratio of five to one) in a universal material testing machine, and the test results are shown in Table 1 below.
Comparative example 1
The preparation method of the three-dimensional woven fiber reinforced magnesium-based composite material in the comparative example comprises the following steps:
(1) preparing a carbon fiber preform, wherein the carbon fiber preform is woven into a preform plate with a three-dimensional five-direction microscopical structure by graphite fiber M40 of Jiangsu Xinliwea Kogyo through a four-step method. The carbon fiber preform is then placed in an encapsulation mold.
(2) Infiltration: the packaging mold and the AZ91D magnesium alloy are respectively placed in an upper chamber and a lower chamber of a vacuum pressure infiltration device, a liquid inlet of the packaging mold faces downwards and faces towards the magnesium alloy, and a liquid lifting pipe is arranged, and is not inserted into the magnesium alloy at the beginning.
Vacuumizing and filling argon, and simultaneously preheating the fiber preform and the magnesium alloy at the preheating temperature of 580 ℃ for 1h to melt the magnesium alloy. Then argon in the furnace is discharged and the furnace is vacuumized to 10Pa, a crucible is lifted to enable a liquid lifting pipe to be inserted into the magnesium alloy molten metal, then nitrogen of 8MPa is filled into the whole device, the magnesium alloy molten metal is filled into a packaging mold along the liquid lifting pipe through air pressure difference, and the pressure is maintained for 20min at 720 ℃ and 8 MPa. And finally, taking out the packaging mold, naturally cooling to room temperature, and removing the packaging mold and the graphite to obtain the composite material.
The composite material thus obtained was cut into standard test specimens (20X 6X 2 mm) by a wheel cutter, and then the interlaminar shear strength ILSS (average of ten specimens) was measured by a three-point short beam method (span-thickness ratio of five to one) in a universal material testing machine, and the test results are shown in Table 1 below.
TABLE 1
Figure DEST_PATH_IMAGE002
As can be seen from Table 1, the treatment method of the present application can effectively improve the interlaminar shear strength of the composite material.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.

Claims (9)

1. A preparation method of a high heat-resistant three-dimensional woven fiber reinforced magnesium matrix composite is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a carbon fiber preform, and placing the carbon fiber preform in a packaging mold; the packaging mold is provided with two liquid inlets, one liquid inlet is provided with a liquid lifting pipe for feeding liquid into the subsequent liquid metal, and the other liquid inlet is provided with a liquid conveying pipe for feeding liquid into the liquid carbon dioxide;
(2) removing the photoresist: respectively placing the packaging mold and the metal in an upper chamber and a lower chamber of a vacuum pressure infiltration device, wherein a liquid lifting pipe of the packaging mold faces downwards and towards the metal, and is not inserted into the metal at the beginning, and meanwhile, a liquid conveying pipe is communicated with the outside; under the pressure and temperature that the carbon dioxide is in a liquid state, closing the liquid lifting pipe, opening the liquid conveying pipe, introducing the liquid carbon dioxide into the packaging mold, closing the liquid conveying pipe, completely immersing the carbon fiber preform in the liquid carbon dioxide, and soaking for 20-24 hours;
(3) surface modification: placing the packaging mold in a sealed environment of 950 plus materials at 980 ℃, and carrying out heat preservation and activation for 90-120 min; in the step (3), the lift tube is opened, the temperature is raised to 550-; during the period, most of gasified carbon dioxide escapes to the vacuum pressure infiltration device, so that the pressure in the device rises, and a small part of gasified carbon dioxide reacts with carbon fibers to be activated;
(4) infiltration: and pressing the molten liquid metal into a packaging mold through air pressure to infiltrate the carbon fiber preform to obtain the composite material.
2. The method for preparing the high heat-resistant three-dimensional braided fiber-reinforced magnesium-based composite material as claimed in claim 1, wherein the method comprises the following steps: and (4) carrying out the step under a vibration condition.
3. The method for preparing the high heat-resistant three-dimensional braided fiber reinforced magnesium matrix composite material as claimed in claim 2, wherein the method comprises the following steps: vibrating under 15-20kHz ultrasonic wave.
4. The method for preparing the high heat-resistant three-dimensional braided fiber-reinforced magnesium-based composite material as claimed in claim 1, wherein the method comprises the following steps: in the step (3), after heat preservation and activation, the method further comprises coating treatment: introducing a sol solution into the packaging mold to enable the sol solution to completely immerse the carbon fiber preform, discharging the sol solution after soaking for 5-8h, and drying the packaging mold at the temperature of 450-490 ℃; the sol solution is SiO2、TiO2、ZrO2One or more of them.
5. The method for preparing the high heat-resistant three-dimensional braided fiber reinforced magnesium matrix composite material as claimed in claim 4, wherein the method comprises the following steps: and (3) dipping the packaging mold under the ultrasonic wave of 15-20 kHz.
6. The method for preparing the high heat-resistant three-dimensional braided fiber reinforced magnesium matrix composite material as claimed in claim 4, wherein the method comprises the following steps: when drying, firstly heating to 150-180 ℃ for drying for 30-45min, and then heating to 450-490 ℃ for drying for 60-90 min.
7. The method for preparing the high heat-resistant three-dimensional braided fiber-reinforced magnesium-based composite material as claimed in claim 1, wherein the method comprises the following steps: the molten liquid metal for infiltration is one or more of AZ91D magnesium alloy, AZ31D magnesium alloy and AZ61D magnesium alloy.
8. The method for preparing the high heat-resistant three-dimensional braided fiber-reinforced magnesium-based composite material as claimed in claim 1, wherein the method comprises the following steps: the carbon fiber preform is made of three-dimensional five-direction braided graphite fibers M40.
9. The method for preparing the high heat-resistant three-dimensional braided fiber-reinforced magnesium-based composite material as claimed in claim 1, wherein the method comprises the following steps: in the step (4), the parameters of the vacuum pressure infiltration process are as follows: the preheating temperature is 550-.
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