CN111331098B - A kind of preparation method of high-performance magnesium matrix composite component - Google Patents
A kind of preparation method of high-performance magnesium matrix composite component Download PDFInfo
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- CN111331098B CN111331098B CN202010235754.0A CN202010235754A CN111331098B CN 111331098 B CN111331098 B CN 111331098B CN 202010235754 A CN202010235754 A CN 202010235754A CN 111331098 B CN111331098 B CN 111331098B
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- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
- B22D17/007—Semi-solid pressure die casting
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- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
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Abstract
本发明涉及一种高性能镁基复合材料构件的制备方法，其针对石墨烯作为增强体与镁基体润湿性差、易团聚，极易发生不良的界面反应，且制备过程复杂，不易控制等问题，采用羧基化石墨烯作为镁基复合材料的增强体，经镁合金板表面处理、表面处理后的镁合金板表面喷涂羧基化石墨烯、热压烧结、切碎成镁合金颗粒、半固态间接挤压铸造成型，制备出了高性能镁基复合材料构件。此制备方法工艺先进，数据精确翔实，制备出的镁基复合材料构件内部无缩孔、缩松缺陷，组织致密性好，晶粒细小、呈球状和近球状，羧基化石墨烯在基体中分散均匀，界面结合良好，构件抗拉强度达335Mpa，延伸率达5.6%，硬度达102HV，是先进的高性能镁基复合材料构件的制备方法。
The invention relates to a preparation method of a high-performance magnesium-based composite material component, which aims at the problems of poor wettability between graphene as a reinforcement and a magnesium matrix, easy agglomeration, easy occurrence of bad interface reaction, complicated preparation process and difficult control, etc. , using carboxylated graphene as the reinforcement of magnesium-based composite materials, after surface treatment of magnesium alloy plate, spraying carboxylated graphene on the surface of magnesium alloy plate after surface treatment, hot pressing sintering, chopped into magnesium alloy particles, semi-solid indirect Squeeze casting to prepare high-performance magnesium matrix composite components. This preparation method has advanced technology and accurate and detailed data. The prepared magnesium-based composite material has no shrinkage cavities and shrinkage defects inside, and has good organization density, fine grains, spherical and nearly spherical shapes, and carboxylated graphene is dispersed in the matrix. Uniform, good interface bonding, tensile strength of components up to 335Mpa, elongation up to 5.6%, hardness up to 102HV, it is an advanced preparation method for high-performance magnesium matrix composite components.
Description
Technical Field
The invention relates to a preparation method of a high-performance magnesium-based composite material member, belonging to the technical field of preparation of non-ferrous metal composite material members.
Background
The magnesium-based composite material has the advantages of high specific strength, high specific modulus, small density and good thermal stability, simultaneously has good damping performance and electromagnetic shielding performance, and becomes one of the hot spots of the research in the field of material science at present. The magnesium-based composite material consists of a magnesium matrix, a reinforcement and an interface region. Currently, ceramic particles are often used as reinforcement in the design and manufacture of magnesium-based composites. However, most of the ceramic particles are micron-sized, and the dispersion strengthening effect is limited; meanwhile, the interface of the ceramic particles and the magnesium matrix is generally simple and mechanical combination, and the performance of the interface combination part is poor; and the ceramic particles are brittle, and although the strength of the composite material can be improved, the plasticity and the toughness of the composite material are reduced.
The graphene is represented by sp2The two-dimensional material with the thickness of the monoatomic layer formed by hybridized carbon atoms has excellent mechanical, thermal and electrical properties and is considered as an ideal reinforcement of the magnesium-based composite material. According to the law of mixing, a magnesium-based composite material prepared by using graphene as a reinforcement has extremely excellent performance. However, current research results indicate that the properties of the composite material do not achieve the expected effect, mainly because: the graphene and the magnesium matrix have poor wettability and are easy to agglomerate; secondly, poor interface reaction is easily caused between the graphene and the magnesium substrate; and thirdly, the preparation process is complex and difficult to control. Therefore, the graphene reinforced magnesium-based composite material is not practically applied to the technical field of high-performance member preparation.
Disclosure of Invention
Object of the Invention
The invention aims to prepare a high-performance magnesium-based composite material component by using carboxylated graphene as a reinforcement of a magnesium-based composite material, performing surface treatment on a magnesium alloy plate, spraying the carboxylated graphene on the surface of the magnesium alloy plate after the surface treatment, performing hot-pressing sintering, cutting into magnesium alloy particles, and performing semisolid indirect extrusion casting molding.
Technical scheme
The chemical substance materials used in the invention are as follows: the magnesium alloy plate comprises a magnesium alloy plate, carboxylated graphene, polyvinyl alcohol, deionized water, absolute ethyl alcohol, argon, a magnesium oxide release agent and graphite lubricating oil, wherein the combined preparation dosage is as follows: in the form of block, g, ml, cm3As a unit of measure
Magnesium alloy sheet: AZ91D SOLID BLOCK 5 BLOCKS 350mm long 250mm wide 5mm high
20g +/-0.1 g of solid powder with oxygen content of carboxylated graphene of 24.5 at%
Polyvinyl alcohol: [ C ]2H4O]n1800g +/-10 g of solid powder
Deionized water: h2O liquid 140000mL +/-500 mL
Anhydrous ethanol: c2H55000mL +/-50 mL of OH liquid
Argon gas: ar gas 2000000cm3±100cm3
120mL +/-5 mL of liquid magnesium oxide release agent
Graphite lubricating oil liquid 50mL +/-5 mL
The preparation method comprises the following steps:
1) surface treatment of magnesium alloy plate
Adding 60000mL of deionized water into a polyvinyl alcohol liquid storage tank, heating to 80 ℃, then adding 1800g of polyvinyl alcohol, keeping the temperature for 1h, stirring, and cooling to room temperature after the polyvinyl alcohol is completely dissolved to prepare a polyvinyl alcohol solution;
secondly, polishing the surfaces of the five magnesium alloy plates by using 2000-mesh abrasive paper to clean the surfaces, and then cleaning the surfaces of the five magnesium alloy plates by using absolute ethyl alcohol to clean the surfaces;
opening the surface treatment chamber, sequentially placing the five magnesium alloy plates into a clamp in the surface treatment chamber, numbering the five magnesium alloy plates from top to bottom into a first magnesium alloy plate, a second magnesium alloy plate, a third magnesium alloy plate, a fourth magnesium alloy plate and a fifth magnesium alloy plate, and then sealing the surface treatment chamber;
opening a polyvinyl alcohol liquid inlet valve on the polyvinyl alcohol liquid storage tank, injecting the polyvinyl alcohol solution in the polyvinyl alcohol liquid storage tank into the surface treatment chamber through a liquid inlet pipe, completely soaking the five magnesium alloy plates in the polyvinyl alcohol solution, and then closing the polyvinyl alcohol liquid inlet valve;
fifthly, opening and adjusting a first temperature controller in the surface treatment chamber to keep the temperature of the polyvinyl alcohol solution in the surface treatment chamber at 55 +/-2 ℃, keeping the temperature for 15min, then opening an ultrasonic vibration table in the surface treatment chamber, vibrating and stirring at constant temperature for 45min, and then closing the ultrasonic vibration table;
sixthly, opening a polyvinyl alcohol drain valve on the polyvinyl alcohol liquid storage tank, pumping all the polyvinyl alcohol solution in the surface treatment chamber back to the polyvinyl alcohol liquid storage tank through a drain pipe, and then closing the polyvinyl alcohol drain valve;
seventhly, adding 60000mL of deionized water into the deionized water storage tank, opening a deionized water inlet valve on the deionized water storage tank, injecting the deionized water in the deionized water storage tank into the surface treatment chamber through a liquid inlet pipe, completely soaking the five magnesium alloy plates in the deionized water, and then closing the deionized water inlet valve;
eighthly, adjusting a first temperature controller to keep the temperature of the deionized water in the surface treatment chamber at 45 +/-2 ℃, starting an ultrasonic vibration table, carrying out vibration cleaning for 10min, and then closing the ultrasonic vibration table and the first temperature controller;
ninthly, opening a deionized water drain valve on the deionized water storage tank, completely pumping the deionized water in the surface treatment chamber back to the deionized water storage tank through a drain pipe, and then closing the deionized water drain valve;
opening a dryer on the surface treatment chamber at the front part, keeping the temperature in the surface treatment chamber at 80 +/-5 ℃, and preserving the heat for 40min to dry the surfaces of the five magnesium alloy plates after surface treatment for later use;
2) spraying carboxylated graphene on the surface of the magnesium alloy plate after surface treatment
Adding 20g of carboxylated graphene and 20000mL of deionized water into a container, stirring for 1h by ultrasonic vibration to prepare a carboxylated graphene dispersion liquid, and then respectively adding the carboxylated graphene dispersion liquid into an upper spraying machine and a lower spraying machine in a surface spraying chamber;
opening the surface treatment chamber and the surface spraying chamber, conveying the first magnesium alloy plate subjected to surface treatment from the surface treatment chamber to the surface spraying chamber by using a monorail crane, and then sealing the surface spraying chamber;
starting a second temperature controller in the surface spraying chamber to keep the temperature in the surface spraying chamber at 85 +/-1 ℃, starting an upper spraying machine and a lower spraying machine after heat preservation is carried out for 15min, spraying the carboxylated graphene dispersion liquid onto the upper surface and the lower surface of the first magnesium alloy plate after surface treatment through a nozzle of the upper spraying machine and a nozzle of the lower spraying machine, wherein the spraying pressure is 0.35MPa, the spraying is suspended for 30s every 15s, the spraying is carried out for 4 times in total, and then the upper spraying machine and the lower spraying machine are closed;
adjusting a second temperature controller to keep the temperature in the surface spraying chamber at 65 +/-1 ℃, preserving the temperature for 15min, and then closing the second temperature controller;
opening the surface spraying chamber, taking the first magnesium alloy plate after surface spraying out of the surface spraying chamber by using a monorail crane, placing the plate on a clean steel plate, and cooling the plate to room temperature for later use;
spraying carboxylated graphene on the surfaces of the second magnesium alloy plate, the third magnesium alloy plate, the fourth magnesium alloy plate and the fifth magnesium alloy plate after surface treatment in sequence;
3) hot pressed sintering
Opening a hot-pressing sintering furnace, sequentially placing five magnesium alloy plates with the surfaces sprayed into a mold of the hot-pressing sintering furnace, pushing a pressing plate of the hot-pressing sintering furnace by a pressure head of the hot-pressing sintering furnace to apply pressure to the five magnesium alloy plates with the surfaces sprayed, wherein the pressure is 30 MPa;
secondly, sealing the hot-pressing sintering furnace, extracting air in the furnace to reduce the air pressure in the furnace to 2Pa, and then starting a heater of the hot-pressing sintering furnace to raise the temperature in the furnace; when the temperature in the furnace rises to 150 ℃, introducing argon into the furnace, and keeping the pressure in the furnace at 1 atmosphere; when the temperature in the furnace rises to 550 +/-1 ℃, preserving heat, sintering for 5 hours at constant temperature and constant pressure, then closing a heater of the hot-pressing sintering furnace to reduce the temperature in the furnace to the normal temperature, opening the hot-pressing sintering furnace, and taking out the magnesium alloy block after hot-pressing sintering from a mold of the hot-pressing sintering furnace for later use;
4) cutting into magnesium alloy particles
Cutting the magnesium alloy block after hot-pressing sintering into rod-shaped magnesium alloy particles with the length of 6mm +/-1.5 mm and the equivalent diameter of the cross section phi of 0.8mm +/-0.15 mm by adopting a magnesium alloy particle cutting machine for later use;
5) semi-solid indirect extrusion casting molding
Preheating indirect extrusion casting die
Starting a third temperature controller on the indirect extrusion casting mold, and preheating a material cylinder of the indirect extrusion casting mold by the third temperature controller, wherein the preheating temperature is 295 +/-1 ℃; preheating a fixed mold core and a movable mold core of an indirect extrusion casting mold by adopting a resistance wire heating mode, wherein the preheating temperature is 280 +/-1 ℃; uniformly spraying 120mL of magnesium oxide release agent on the surface of a die cavity of an indirect extrusion casting die, wherein the spraying thickness is 0.05 mm; injecting 50mL of graphite lubricating oil into a gap between a material cylinder of the indirect extrusion casting die and a punch of the indirect extrusion casting die for lubrication;
② argon injection indirect extrusion casting die
Closing the indirect extrusion casting die, then opening a shielding gas inlet pipe on the indirect extrusion casting die, injecting argon gas into a material cylinder of the indirect extrusion casting die and a die cavity of the indirect extrusion casting die through the shielding gas inlet pipe, wherein the injection speed is 150cm3(ii)/s, injection time 25 s;
preparing semi-solid magnesium alloy slurry by screw conveyer
Starting a screw conveyor, adding rod-shaped magnesium alloy particles into a feed hopper of the screw conveyor, conveying the rod-shaped magnesium alloy particles into a feed pipe of the screw conveyor by the feed hopper of the screw conveyor, shearing and stirring the rod-shaped magnesium alloy particles by a screw shaft of the screw conveyor at a shearing and stirring speed of 150r/min, heating the rod-shaped magnesium alloy particles by a preheating section heater, a heating section heater and a heat preservation section heater on the feed pipe of the screw conveyor, wherein the set temperature of the preheating section heater is 350 +/-5 ℃, the set temperature of the heating section heater is 625 +/-1 ℃, and the set temperature of the heat preservation section heater is 605 +/-1 ℃; preparing semi-solid magnesium alloy slurry at the tail end of a feeding pipe of a screw conveyor under the actions of shearing, stirring and heating;
fourthly, injecting the semi-solid magnesium alloy slurry into an indirect extrusion casting die
Under the action of a driving device of the screw conveyer, a conical head of the screw conveyer pushes the semi-solid magnesium alloy slurry, so that the semi-solid magnesium alloy slurry is injected into a material cylinder of the indirect extrusion casting mould through a feed inlet of the indirect extrusion casting mould, and the pushing speed is 200 mm/s;
indirect squeeze casting
A push rod of the indirect extrusion casting die and a punch of the indirect extrusion casting die push the semi-solid magnesium alloy slurry into a die cavity of the indirect extrusion casting die together and maintain pressure, wherein the pushing speed is 350mm/s, the pressure maintaining pressure is 120MPa, and the pressure maintaining time is 15s, so that the magnesium-based composite material component is prepared;
demoulding magnesium base composite material member
Opening the indirect extrusion casting die, ejecting the magnesium-based composite material component by a push rod of the indirect extrusion casting die and a punch of the indirect extrusion casting die together, then taking down the magnesium-based composite material component, placing the magnesium-based composite material component on a wooden flat plate, and cooling the magnesium-based composite material component to 25 ℃ in air;
6) cleaning and rinsing
Cleaning each part and the periphery of the magnesium-based composite material member by using a steel wire brush, cleaning the magnesium-based composite material member by using absolute ethyl alcohol, and drying the magnesium-based composite material member after cleaning;
7) detection, analysis, characterization
Detecting, analyzing and representing the appearance, the tissue structure and the mechanical property of the magnesium-based composite material member;
carrying out metallographic structure analysis by using a metallographic microscope;
analyzing the tensile strength and the elongation by using an electronic universal tester;
performing hardness analysis by using a Vickers hardness tester;
and (4) conclusion: the magnesium-based composite material member has no shrinkage cavity and shrinkage porosity defects, good tissue compactness, fine and spherical crystal grains, uniform dispersion of the carboxylated graphene in a matrix, good interface bonding, tensile strength of the member up to 335Mpa, elongation of the member up to 5.6 percent and hardness of the member up to 102 HV.
Advantageous effects
Compared with the prior art, the method has obvious advancement, aims at the problems that graphene is used as a reinforcement, the graphene is poor in wettability and easy to agglomerate with a magnesium matrix, poor interface reaction is easy to occur, the preparation process is complex and not easy to control, and the like, adopts carboxylated graphene as a reinforcement of the magnesium-based composite material, sprays the carboxylated graphene on the surface of a magnesium alloy plate after surface treatment and surface treatment of the magnesium alloy plate, carries out hot-pressing sintering, cuts the magnesium alloy plate into magnesium alloy particles, and carries out semisolid indirect extrusion casting molding, thereby preparing the high-performance magnesium-based composite material component. The preparation method has the advantages of advanced process and precise and detailed data, the prepared magnesium-based composite material member has no shrinkage cavity and shrinkage porosity defects, good tissue compactness, fine, spherical and near-spherical crystal grains, uniform dispersion of the carboxylated graphene in the matrix, good interface bonding, tensile strength of the member up to 335Mpa, elongation of 5.6 percent and hardness of 102HV, and is an advanced preparation method of a high-performance magnesium-based composite material member.
Drawings
Fig. 1 is a state diagram of magnesium alloy plate surface treatment and the magnesium alloy plate surface spraying carboxylated graphene after the surface treatment.
FIG. 2 is a diagram showing a state of hot press sintering.
FIG. 3 is a diagram showing the state of preparing semi-solid magnesium alloy slurry by injecting argon into an indirect extrusion casting die and a screw conveyor.
FIG. 4 is a state diagram of semi-solid magnesium alloy slurry injected into an indirect squeeze casting die.
Fig. 5 is a view showing an indirect squeeze casting state.
Fig. 6 is a view showing a state where the magnesium-based composite material member is released from the mold.
As shown in the figures, the list of reference numbers is as follows:
1-a master control cabinet, 2-a surface treatment chamber, 3-a surface spraying chamber, 4-a first cable, 5-a second cable, 6-a liquid inlet pipe, 7-a liquid outlet pipe, 8-a first temperature controller, 9-a dryer, 10-a polyvinyl alcohol solution, 11-a first magnesium alloy plate, 12-a second magnesium alloy plate, 13-a third magnesium alloy plate, 14-a fourth magnesium alloy plate, 15-a fifth magnesium alloy plate, 16-an ultrasonic vibration table, 17-a clamp, 18-a monorail crane, 19-an upper spraying machine, 20-a nozzle of the upper spraying machine, 21-a lower spraying machine, 22-a nozzle of the lower spraying machine, 23-a surface treated magnesium alloy plate, 24-a second temperature controller, 25-a polyvinyl alcohol liquid storage tank and 26-a deionized water liquid storage tank, 27-polyvinyl alcohol liquid inlet valve, 28-polyvinyl alcohol liquid outlet valve, 29-deionized water liquid inlet valve, 30-deionized water liquid outlet valve, 31-magnesium alloy plate after surface spraying, 32-mould of hot-pressing sintering furnace, 33-press plate of hot-pressing sintering furnace, 34-press head of hot-pressing sintering furnace, 35-heater of hot-pressing sintering furnace, 36-rod-shaped magnesium alloy particles, 37-feed hopper of screw conveyer, 38-screw shaft of screw conveyer, 39-drive device of screw conveyer, 40-feed pipe of screw conveyer, 41-conical head of screw conveyer, 42-preheating section heater, 43-heating section heater, 44-heat preservation section heater, 45-semi-solid magnesium alloy slurry, 46-material cylinder of indirect extrusion casting mould, 47-a third temperature controller, 48-a protective gas inlet pipe, 49-a thermometer, 50-a punch of an indirect extrusion casting die, 51-a push rod of the indirect extrusion casting die, 52-argon, 53-a fixed die back plate of the indirect extrusion casting die, 54-a fixed die core of the indirect extrusion casting die, 55-a movable die back plate of the indirect extrusion casting die, 56-a movable die frame of the indirect extrusion casting die, 57-a movable die core of the indirect extrusion casting die, 58-a fixed die heating hole of the indirect extrusion casting die, 59-a movable die heating hole of the indirect extrusion casting die, 60-a die cavity of the indirect extrusion casting die, and 61-a magnesium-based composite material component.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
FIG. 1 is a state diagram of magnesium alloy plate surface treatment and carboxylated graphene spraying on the surface of the magnesium alloy plate after the surface treatment; the whole set of equipment comprises a master control cabinet 1, a surface treatment chamber 2 and a surface spraying chamber 3;
the master control cabinet 1 controls the working state of the surface treatment chamber 2 through a first cable 4 and a second cable 5 on one hand, and controls the working state of the surface spraying chamber 3 through the first cable 4 and the second cable 5 on the other hand;
a polyvinyl alcohol liquid storage tank 25 and a deionized water liquid storage tank 26 are respectively arranged below the main control cabinet 1; the side wall of the polyvinyl alcohol liquid storage tank 25 is respectively provided with a polyvinyl alcohol liquid inlet valve 27 and a polyvinyl alcohol liquid outlet valve 28; the side wall of the deionized water storage tank 26 is respectively provided with a deionized water inlet valve 29 and a deionized water outlet valve 30; the polyvinyl alcohol liquid storage tank 25 is communicated with the surface treatment chamber 2 sequentially through a polyvinyl alcohol liquid inlet valve 27 and a liquid inlet pipe 6 on one hand, and is communicated with the surface treatment chamber 2 sequentially through a polyvinyl alcohol liquid outlet valve 28 and a liquid outlet pipe 7 on the other hand; the deionized water storage tank 26 is communicated with the surface treatment chamber 2 sequentially through a deionized water inlet valve 29 and a liquid inlet pipe 6 on one hand, and is communicated with the surface treatment chamber 2 sequentially through a deionized water outlet valve 30 and a liquid outlet pipe 7 on the other hand; in the surface treatment process of the magnesium alloy plate, a polyvinyl alcohol liquid inlet valve 27 on a polyvinyl alcohol liquid storage tank 25 is opened, and the polyvinyl alcohol solution 10 in the polyvinyl alcohol liquid storage tank 25 is injected into the surface treatment chamber 2 through a liquid inlet pipe 6; opening a polyvinyl alcohol liquid discharge valve 28 on the polyvinyl alcohol liquid storage tank 25, and completely pumping the polyvinyl alcohol solution 10 in the surface treatment chamber 2 back to the polyvinyl alcohol liquid storage tank 25 through a liquid discharge pipe 7; opening a deionized water inlet valve 29 on the deionized water storage tank 26, and injecting the deionized water in the deionized water storage tank 26 into the surface treatment chamber 2 through a liquid inlet pipe 6; opening a deionized water drain valve 30 on the deionized water storage tank 26, and completely pumping the deionized water in the surface treatment chamber 2 back to the deionized water storage tank 26 through a drain pipe 7;
the inner side wall of the surface treatment chamber 2 is provided with a first temperature controller 8, the inner bottom wall is provided with an ultrasonic vibration table 16, the upper part of the right side wall is provided with a dryer 9, and the table top of the ultrasonic vibration table 16 is provided with a clamp 17; in the surface treatment process of the magnesium alloy plate, five magnesium alloy plates are sequentially placed in a clamp 17 in a surface treatment chamber 2 and numbered as a first magnesium alloy plate 11, a second magnesium alloy plate 12, a third magnesium alloy plate 13, a fourth magnesium alloy plate 14 and a fifth magnesium alloy plate 15 from top to bottom;
the inner top wall of the surface spraying chamber 3 is provided with an upper spraying machine 19, the inner bottom wall is provided with a lower spraying machine 21, and the inner side wall is provided with a second temperature controller 24; the monorail trolley 18 is mounted above the surface treatment chamber 2 and the surface painting chamber 3; in the process of spraying the carboxylated graphene on the surface of the magnesium alloy plate after surface treatment, a monorail crane 18 is used for conveying the magnesium alloy plate 23 after surface treatment from the surface treatment chamber 2 to the surface spraying chamber 3; the upper coater 19 and the lower coater 21 were turned on, and the carboxylated graphene dispersion was sprayed onto the upper surface and the lower surface of the magnesium alloy sheet 23 after the surface treatment through the nozzle 20 of the upper coater and the nozzle 22 of the lower coater.
FIG. 2 is a view showing a state of hot press sintering; in the hot-pressing sintering process, the five magnesium alloy plates 31 with the surfaces sprayed are sequentially placed into a mold 32 of a hot-pressing sintering furnace, and a pressure head 34 of the hot-pressing sintering furnace pushes a pressure plate 33 of the hot-pressing sintering furnace to apply pressure to the five magnesium alloy plates 31 with the surfaces sprayed; starting a heater 35 of the hot-pressing sintering furnace to raise the temperature in the furnace; the heater 35 of the hot-pressing sintering furnace is turned off to lower the temperature in the furnace.
FIG. 3 is a diagram showing a state in which semi-solid magnesium alloy slurry is prepared by injecting argon gas into an indirect extrusion casting mold and a screw conveyor; the screw conveyor is fixedly arranged on the side of the indirect extrusion casting die, the tail end of a feeding pipe 40 of the screw conveyor is communicated with a feeding hole of the indirect extrusion casting die in a sealing way, and a preheating section heater 42, a heating section heater 43 and a heat preservation section heater 44 are respectively arranged on the outer side wall of the feeding pipe 40 of the screw conveyor; the indirect extrusion casting die comprises a material cylinder 46, a punch 50, a push rod 51, a fixed die back plate 53, a fixed die core 54, a movable die back plate 55, a movable die frame 56 and a movable die core 57; a fixed mold heating hole 58 is formed in the fixed mold core 54, a movable mold heating hole 59 is formed in the movable mold core 57, and the fixed mold core 54 and the movable mold core 57 jointly enclose a mold cavity 60; a third temperature controller 47 is arranged on the outer side wall of the material cylinder 46 of the indirect extrusion casting die, a shielding gas inlet pipe 48 is arranged on the side wall of the material cylinder 46 of the indirect extrusion casting die, and a thermometer 49 is arranged inside the material cylinder 46 of the indirect extrusion casting die; during the process of injecting argon into the indirect extrusion casting die, injecting argon 52 into a material cylinder 46 of the indirect extrusion casting die and a die cavity 60 of the indirect extrusion casting die through a protective gas inlet pipe 48; in the process of preparing the semi-solid magnesium alloy slurry by the screw conveyor, rod-shaped magnesium alloy particles 36 are added into a feed hopper 37 of the screw conveyor, the rod-shaped magnesium alloy particles 36 are conveyed into a feeding pipe 40 of the screw conveyor by the feed hopper 37 of the screw conveyor, a screw shaft 38 of the screw conveyor carries out shearing and stirring on the rod-shaped magnesium alloy particles 36, and a preheating section heater 42, a heating section heater 43 and a heat preservation section heater 44 on the feeding pipe 40 of the screw conveyor jointly heat the rod-shaped magnesium alloy particles 36; under the action of shearing, stirring and heating, semi-solid magnesium alloy slurry 45 is prepared at the tail end of the feeding pipe 40 of the screw conveyor.
FIG. 4 is a diagram showing a state in which semi-solid magnesium alloy slurry is injected into an indirect squeeze casting mold; in the process of injecting the semi-solid magnesium alloy slurry into the indirect extrusion casting die, under the action of the driving device 39 of the screw conveyer, the conical head 41 of the screw conveyer pushes the semi-solid magnesium alloy slurry 45, so that the semi-solid magnesium alloy slurry 45 is injected into the material cylinder 46 of the indirect extrusion casting die through the feed inlet of the indirect extrusion casting die.
FIG. 5 is a view showing an indirect squeeze casting state; in the indirect extrusion casting process, a push rod 51 of the indirect extrusion casting die and a punch 50 of the indirect extrusion casting die jointly push the semi-solid magnesium alloy slurry 45 to enter a die cavity 60 of the indirect extrusion casting die and perform pressure maintaining to prepare a magnesium-based composite material member 61;
FIG. 6 is a view showing a state where the Mg-based composite material member is released from the mold; during the process of demoulding the magnesium-based composite material member, the push rod 51 of the indirect extrusion casting die and the punch 50 of the indirect extrusion casting die jointly push out the magnesium-based composite material member 61, and then the magnesium-based composite material member 61 is removed.
While specific embodiments of the invention have been described above, it will be appreciated by those skilled in the art that these are by way of example only, and that the scope of the invention is defined by the appended claims. Various changes and modifications to these embodiments may be made by those skilled in the art without departing from the spirit and scope of the invention, and these changes and modifications are within the scope of the invention.
Claims (1)
1. A preparation method of a high-performance magnesium-based composite material member is characterized by comprising the following steps:
the chemical materials used were: the magnesium alloy plate comprises a magnesium alloy plate, carboxylated graphene, polyvinyl alcohol, deionized water, absolute ethyl alcohol, argon, a magnesium oxide release agent and graphite lubricating oil, wherein the combined preparation dosage is as follows: in the form of block, g, ml, cm3To countUnit of measurement
Magnesium alloy sheet: AZ91D SOLID BLOCK 5 BLOCKS 350mm long 250mm wide 5mm high
20g of solid powder with carboxylation graphene oxygen content of 24.5 at%
Polyvinyl alcohol: [ C ]2H4O]n1800g of solid powder
Deionized water: h2O liquid 140000mL
Anhydrous ethanol: c2H55000mL of OH liquid
Argon gas: ar gas 2000000cm3
120mL of magnesium oxide release agent liquid
Graphite lubricating oil liquid 50mL
The preparation method comprises the following steps:
1) surface treatment of magnesium alloy plate
Adding 60000mL of deionized water into a polyvinyl alcohol liquid storage tank, heating to 80 ℃, then adding 1800g of polyvinyl alcohol, keeping the temperature for 1h, stirring, and cooling to room temperature after the polyvinyl alcohol is completely dissolved to prepare a polyvinyl alcohol solution;
secondly, polishing the surfaces of the five magnesium alloy plates by using 2000-mesh abrasive paper to clean the surfaces, and then cleaning the surfaces of the five magnesium alloy plates by using absolute ethyl alcohol to clean the surfaces;
opening the surface treatment chamber, sequentially placing the five magnesium alloy plates into a clamp in the surface treatment chamber, numbering the five magnesium alloy plates from top to bottom into a first magnesium alloy plate, a second magnesium alloy plate, a third magnesium alloy plate, a fourth magnesium alloy plate and a fifth magnesium alloy plate, and then sealing the surface treatment chamber;
opening a polyvinyl alcohol liquid inlet valve on the polyvinyl alcohol liquid storage tank, injecting the polyvinyl alcohol solution in the polyvinyl alcohol liquid storage tank into the surface treatment chamber through a liquid inlet pipe, completely soaking the five magnesium alloy plates in the polyvinyl alcohol solution, and then closing the polyvinyl alcohol liquid inlet valve;
fifthly, opening and adjusting a first temperature controller in the surface treatment chamber to keep the temperature of the polyvinyl alcohol solution in the surface treatment chamber at 55 +/-2 ℃, keeping the temperature for 15min, then opening an ultrasonic vibration table in the surface treatment chamber, vibrating and stirring at constant temperature for 45min, and then closing the ultrasonic vibration table;
sixthly, opening a polyvinyl alcohol drain valve on the polyvinyl alcohol liquid storage tank, pumping all the polyvinyl alcohol solution in the surface treatment chamber back to the polyvinyl alcohol liquid storage tank through a drain pipe, and then closing the polyvinyl alcohol drain valve;
seventhly, adding 60000mL of deionized water into the deionized water storage tank, opening a deionized water inlet valve on the deionized water storage tank, injecting the deionized water in the deionized water storage tank into the surface treatment chamber through a liquid inlet pipe, completely soaking the five magnesium alloy plates in the deionized water, and then closing the deionized water inlet valve;
eighthly, adjusting a first temperature controller to keep the temperature of the deionized water in the surface treatment chamber at 45 +/-2 ℃, starting an ultrasonic vibration table, carrying out vibration cleaning for 10min, and then closing the ultrasonic vibration table and the first temperature controller;
ninthly, opening a deionized water drain valve on the deionized water storage tank, completely pumping the deionized water in the surface treatment chamber back to the deionized water storage tank through a drain pipe, and then closing the deionized water drain valve;
opening a dryer on the surface treatment chamber at the front part, keeping the temperature in the surface treatment chamber at 80 +/-5 ℃, and preserving the heat for 40min to dry the surfaces of the five magnesium alloy plates after surface treatment for later use;
2) spraying carboxylated graphene on the surface of the magnesium alloy plate after surface treatment
Adding 20g of carboxylated graphene and 20000mL of deionized water into a container, stirring for 1h by ultrasonic vibration to prepare a carboxylated graphene dispersion liquid, and then respectively adding the carboxylated graphene dispersion liquid into an upper spraying machine and a lower spraying machine in a surface spraying chamber;
opening the surface treatment chamber and the surface spraying chamber, conveying the first magnesium alloy plate subjected to surface treatment from the surface treatment chamber to the surface spraying chamber by using a monorail crane, and then sealing the surface spraying chamber;
starting a second temperature controller in the surface spraying chamber to keep the temperature in the surface spraying chamber at 85 +/-1 ℃, starting an upper spraying machine and a lower spraying machine after heat preservation is carried out for 15min, spraying the carboxylated graphene dispersion liquid onto the upper surface and the lower surface of the first magnesium alloy plate after surface treatment through a nozzle of the upper spraying machine and a nozzle of the lower spraying machine, wherein the spraying pressure is 0.35MPa, the spraying is suspended for 30s every 15s, the spraying is carried out for 4 times in total, and then the upper spraying machine and the lower spraying machine are closed;
adjusting a second temperature controller to keep the temperature in the surface spraying chamber at 65 +/-1 ℃, preserving the temperature for 15min, and then closing the second temperature controller;
opening the surface spraying chamber, taking the first magnesium alloy plate after surface spraying out of the surface spraying chamber by using a monorail crane, placing the plate on a clean steel plate, and cooling the plate to room temperature for later use;
spraying carboxylated graphene on the surfaces of the second magnesium alloy plate, the third magnesium alloy plate, the fourth magnesium alloy plate and the fifth magnesium alloy plate after surface treatment in sequence;
3) hot pressed sintering
Opening a hot-pressing sintering furnace, sequentially placing five magnesium alloy plates with the surfaces sprayed into a mold of the hot-pressing sintering furnace, pushing a pressing plate of the hot-pressing sintering furnace by a pressure head of the hot-pressing sintering furnace to apply pressure to the five magnesium alloy plates with the surfaces sprayed, wherein the pressure is 30 MPa;
secondly, sealing the hot-pressing sintering furnace, extracting air in the furnace to reduce the air pressure in the furnace to 2Pa, and then starting a heater of the hot-pressing sintering furnace to raise the temperature in the furnace; when the temperature in the furnace rises to 150 ℃, introducing argon into the furnace, and keeping the pressure in the furnace at 1 atmosphere; when the temperature in the furnace rises to 550 +/-1 ℃, preserving heat, sintering for 5 hours at constant temperature and constant pressure, then closing a heater of the hot-pressing sintering furnace to reduce the temperature in the furnace to the normal temperature, opening the hot-pressing sintering furnace, and taking out the magnesium alloy block after hot-pressing sintering from a mold of the hot-pressing sintering furnace for later use;
4) cutting into magnesium alloy particles
Cutting the magnesium alloy block after hot-pressing sintering into rod-shaped magnesium alloy particles with the length of 6mm +/-1.5 mm and the equivalent diameter of the cross section phi of 0.8mm +/-0.15 mm by adopting a magnesium alloy particle cutting machine for later use;
5) semi-solid indirect extrusion casting molding
Preheating indirect extrusion casting die
Starting a third temperature controller on the indirect extrusion casting mold, and preheating a material cylinder of the indirect extrusion casting mold by the third temperature controller, wherein the preheating temperature is 295 +/-1 ℃; preheating a fixed mold core and a movable mold core of an indirect extrusion casting mold by adopting a resistance wire heating mode, wherein the preheating temperature is 280 +/-1 ℃; uniformly spraying 120mL of magnesium oxide release agent on the surface of a die cavity of an indirect extrusion casting die, wherein the spraying thickness is 0.05 mm; injecting 50mL of graphite lubricating oil into a gap between a material cylinder of the indirect extrusion casting die and a punch of the indirect extrusion casting die for lubrication;
② argon injection indirect extrusion casting die
Closing the indirect extrusion casting die, then opening a shielding gas inlet pipe on the indirect extrusion casting die, injecting argon gas into a material cylinder of the indirect extrusion casting die and a die cavity of the indirect extrusion casting die through the shielding gas inlet pipe, wherein the injection speed is 150cm3(ii)/s, injection time 25 s;
preparing semi-solid magnesium alloy slurry by screw conveyer
Starting a screw conveyor, adding rod-shaped magnesium alloy particles into a feed hopper of the screw conveyor, conveying the rod-shaped magnesium alloy particles into a feed pipe of the screw conveyor by the feed hopper of the screw conveyor, shearing and stirring the rod-shaped magnesium alloy particles by a screw shaft of the screw conveyor at a shearing and stirring speed of 150r/min, heating the rod-shaped magnesium alloy particles by a preheating section heater, a heating section heater and a heat preservation section heater on the feed pipe of the screw conveyor, wherein the set temperature of the preheating section heater is 350 +/-5 ℃, the set temperature of the heating section heater is 625 +/-1 ℃, and the set temperature of the heat preservation section heater is 605 +/-1 ℃; preparing semi-solid magnesium alloy slurry at the tail end of a feeding pipe of a screw conveyor under the actions of shearing, stirring and heating;
fourthly, injecting the semi-solid magnesium alloy slurry into an indirect extrusion casting die
Under the action of a driving device of the screw conveyer, a conical head of the screw conveyer pushes the semi-solid magnesium alloy slurry, so that the semi-solid magnesium alloy slurry is injected into a material cylinder of the indirect extrusion casting mould through a feed inlet of the indirect extrusion casting mould, and the pushing speed is 200 mm/s;
indirect squeeze casting
A push rod of the indirect extrusion casting die and a punch of the indirect extrusion casting die push the semi-solid magnesium alloy slurry into a die cavity of the indirect extrusion casting die together and maintain pressure, wherein the pushing speed is 350mm/s, the pressure maintaining pressure is 120MPa, and the pressure maintaining time is 15s, so that the magnesium-based composite material component is prepared;
demoulding magnesium base composite material member
Opening the indirect extrusion casting die, ejecting the magnesium-based composite material component by a push rod of the indirect extrusion casting die and a punch of the indirect extrusion casting die together, then taking down the magnesium-based composite material component, placing the magnesium-based composite material component on a wooden flat plate, and cooling the magnesium-based composite material component to 25 ℃ in air;
6) cleaning and rinsing
Cleaning each part and the periphery of the magnesium-based composite material member by using a steel wire brush, cleaning the magnesium-based composite material member by using absolute ethyl alcohol, and drying the magnesium-based composite material member after cleaning;
7) detection, analysis, characterization
Detecting, analyzing and representing the appearance, the tissue structure and the mechanical property of the magnesium-based composite material member;
carrying out metallographic structure analysis by using a metallographic microscope;
analyzing the tensile strength and the elongation by using an electronic universal tester;
performing hardness analysis by using a Vickers hardness tester;
and (4) conclusion: the magnesium-based composite material member has no shrinkage cavity and shrinkage porosity defects, good tissue compactness, fine and spherical crystal grains, uniform dispersion of the carboxylated graphene in a matrix, good interface bonding, tensile strength of the member up to 335Mpa, elongation of the member up to 5.6 percent and hardness of the member up to 102 HV.
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