CN111485152A - Semi-solid casting forming method for graphene oxide composite magnesium-based material - Google Patents
Semi-solid casting forming method for graphene oxide composite magnesium-based material Download PDFInfo
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- CN111485152A CN111485152A CN202010501959.9A CN202010501959A CN111485152A CN 111485152 A CN111485152 A CN 111485152A CN 202010501959 A CN202010501959 A CN 202010501959A CN 111485152 A CN111485152 A CN 111485152A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/09—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using pressure
- B22D27/11—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using pressure making use of mechanical pressing devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D29/00—Removing castings from moulds, not restricted to casting processes covered by a single main group; Removing cores; Handling ingots
- B22D29/04—Handling or stripping castings or ingots
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D35/00—Equipment for conveying molten metal into beds or moulds
- B22D35/04—Equipment for conveying molten metal into beds or moulds into moulds, e.g. base plates, runners
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/148—Agglomerating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
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- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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Abstract
The invention relates to a semi-solid casting and forming method of a graphene oxide composite magnesium-based material, which aims at solving the problems that graphene oxide is easy to agglomerate and cannot produce parts with complex structures in the current forming and processing process of the graphene oxide composite magnesium-based material, and the like. The forming method is advanced in process and precise and detailed in data, the prepared graphene oxide composite magnesium-based material casting has good internal tissue compactness, no shrinkage cavity and shrinkage porosity defects, round and fine crystal grains, the graphene oxide is uniformly dispersed in the matrix and does not agglomerate, the interface bonding is good, the tensile strength of the casting reaches 295MPa, the elongation reaches 5.5%, and the hardness reaches 103HV, and the method is an advanced semi-solid casting forming method for the graphene oxide composite magnesium-based material.
Description
Technical Field
The invention relates to a semi-solid casting forming method of a graphene oxide composite magnesium-based material, belonging to the technical field of casting forming of non-ferrous metal composite materials.
Background
The surface of the graphene oxide has a plurality of oxygen-containing functional groups, so that the graphene oxide is more active than graphene in property, has good hydrophilicity, is suitable for being dispersed in a solution, and is easy to perform chemical reaction with other materials and combine with the other materials, thereby preparing a composite material with excellent performance. In addition, the graphene oxide is simple in preparation method, relatively low in price and high in mechanical property, and is an ideal reinforcement of the magnesium-based material.
At present, the graphene oxide and magnesium alloy particles are mixed by a wet method and then are subjected to hot-pressing sintering and rolling, so that the graphene oxide composite magnesium-based material is a main preparation means. In the wet mixing process, graphene oxide has hydrophilicity, and magnesium matrix is wrapped by a naturally formed oxide layer to be hydrophobic, so that the wettability of water is greatly different, which means that the graphene oxide and magnesium alloy particles have little chance of being effectively adsorbed in the mixing stage. The oxide layer on the surface of the magnesium substrate has hydroxyl groups with low density, and most of graphene oxide can not be adsorbed even if the graphene oxide accidentally contacts the surface of magnesium by stirring or electrostatic attraction. Therefore, the graphene oxide is easy to agglomerate in the subsequent molding process, and parts with complex structures cannot be produced by the process.
Therefore, the surface modification treatment of the magnesium alloy particles can be considered, a polyvinyl alcohol film is introduced, hydroxyl groups of the magnesium matrix oxide layer adsorb polyvinyl alcohol molecules through hydrogen bonds, and when the number is large enough, the polyvinyl alcohol molecules are subjected to a crosslinking reaction to form the polyvinyl alcohol film. The polyvinyl alcohol film introduces a large amount of hydroxyl groups onto the surface of the magnesium alloy particles, so that the wettability of the magnesium alloy particles is improved, and graphene oxide can be uniformly adsorbed on the surface of the magnesium alloy particles through the hydrogen bond action between the hydroxyl groups of the polyvinyl alcohol film and the carboxyl groups of the graphene oxide, so that a high-quality graphene oxide composite magnesium-based material casting is prepared.
Disclosure of Invention
Object of the Invention
The invention aims to overcome the defects of the background technology, and the method comprises the steps of preparing mixed particles through surface treatment of rod-shaped magnesium alloy particles, pressing at high temperature, preparing semi-solid mixed slurry, carrying out transmission molding through an electromagnetic pump, and forming the graphene oxide composite magnesium-based material casting.
Technical scheme
The chemical substance materials used in the invention are as follows: the magnesium alloy mold release agent comprises a magnesium alloy ingot, graphene oxide, polyvinyl alcohol, deionized water, absolute ethyl alcohol and a magnesium oxide mold release agent, wherein the combined preparation dosage is as follows: taking g and ml as measurement unit
Magnesium alloy ingot: ZM5 solid block 5000 g. + -. 1g
Graphene oxide solid powder 20g +/-0.1 g
Polyvinyl alcohol: [ C ]2H4O]n solid powder 600g +/-10 g
Deionized water: h2O liquid 58000m L +/-500 m L
Without waterEthanol: c2H5OH liquid 2500m L +/-100 m L
Magnesium oxide release agent liquid 80m L +/-5 m L
The preparation method comprises the following steps:
1) preparation of mixed particles by surface treatment of rod-shaped magnesium alloy particles
① cutting rod-shaped magnesium alloy particles
Cutting 2500g of magnesium alloy ingot into rod-shaped magnesium alloy particles with the length of 5mm +/-1.5 mm and the equivalent diameter of the cross section of phi 0.50mm +/-0.15 mm by using a metal particle cutting machine for later use;
② preparing polyvinyl alcohol solution
Adding 20000m L deionized water into a polyvinyl alcohol solution tank in a mixed particle preparation chamber, starting and adjusting a first temperature controller in the polyvinyl alcohol solution tank to keep the temperature of the deionized water at 85 ℃, then adding 600g of polyvinyl alcohol, keeping the temperature for 0.5h, then starting a first ultrasonic vibration table below the polyvinyl alcohol solution tank for vibration stirring, and after the polyvinyl alcohol is completely dissolved, closing the first ultrasonic vibration table and the first temperature controller to prepare the polyvinyl alcohol solution;
③ preparing graphene oxide dispersion liquid
Preparing graphene oxide with the transverse dimension of 10 microns +/-1 micron, the thickness of 3nm +/-0.5 nm and the oxygen content of 31.5at +/-1 at% by adopting a Hummers method;
adding 20000m L deionized water into a graphene oxide dispersion liquid tank in a mixed particle preparation chamber, starting and adjusting a third temperature controller in the graphene oxide dispersion liquid tank to keep the temperature of the deionized water at 50 ℃, then adding 20g of graphene oxide, starting a third ultrasonic vibration table below the graphene oxide dispersion liquid tank for vibration stirring for 40min, and then closing the third ultrasonic vibration table and the third temperature controller to prepare graphene oxide dispersion liquid;
④ surface treatment of rod-shaped magnesium alloy particles
Starting and adjusting a first temperature controller to keep the temperature of the polyvinyl alcohol solution at 75 +/-2 ℃;
putting the rod-shaped magnesium alloy particles into a treatment box, and then putting the treatment box into a polyvinyl alcohol solution box by using a monorail crane and a hanging tongs, so that the rod-shaped magnesium alloy particles are completely soaked in the polyvinyl alcohol solution;
after the temperature is kept for 20min, starting a first ultrasonic vibration table to carry out constant-temperature vibration stirring for 45min, then closing the first ultrasonic vibration table and a first temperature controller, and standing for 15 min;
⑤ cleaning rod-shaped magnesium alloy particles
Adding 18000m L deionized water into a deionized water tank in the mixed particle preparation chamber, starting and adjusting a second temperature controller in the deionized water tank to keep the temperature of the deionized water at 65 +/-2 ℃, taking the treatment tank out of the polyvinyl alcohol solution tank by using a monorail crane and a hanging clamp, and then putting the treatment tank into the deionized water tank to completely soak the rod-shaped magnesium alloy particles in the deionized water;
starting a second ultrasonic vibration table below the deionized water tank for vibration cleaning for 15min, and then closing the second ultrasonic vibration table and a second temperature controller;
taking the treatment box out of the deionized water tank by using a monorail crane and a hanging clamp, placing the treatment box beside a heating dryer, then starting the heating dryer to dry the rod-shaped magnesium alloy particles, wherein the drying temperature is 75 ℃, the drying time is 30min, and then closing the heating dryer;
⑥ preparation of Mixed granules
Starting and adjusting a third temperature controller to keep the temperature of the graphene oxide dispersion liquid at 45 +/-2 ℃, and then putting the treatment box into the graphene oxide dispersion liquid box by using a monorail crane and a hanging tong to completely soak the rod-shaped magnesium alloy particles in the graphene oxide dispersion liquid;
after the temperature is kept for 5min, starting a third ultrasonic vibration table to carry out constant-temperature vibration stirring, pausing stirring for 10min every time stirring is carried out for 10min, stirring for 4 times in total, then closing the third ultrasonic vibration table and a third temperature controller, and standing for 20 min;
taking the treatment box out of the graphene oxide dispersion liquid box by using a monorail crane and a hanging clamp, then putting the rod-shaped magnesium alloy particles adsorbed with the graphene oxide into a constant-temperature oven for drying at 60 ℃ for 30min, and taking out after drying to obtain mixed particles;
2) high temperature pressing
Starting and adjusting a first heater on a pressing die, wherein the first heater preheats a female die and a male die of the pressing die, and the preheating temperature is 350 ℃;
putting the mixed particles into a concave die of a pressing die, and closing the pressing die; keeping the pressure at constant temperature after the die assembly is finished, wherein the pressure keeping pressure is 180MPa, and the pressure keeping time is 15min, so as to prepare a mixed particle pressed block;
opening a pressing die, ejecting the mixed particle pressed block by an ejector rod of the pressing die, taking down the mixed particle pressed block, and placing the mixed particle pressed block on a steel flat plate to be cooled to room temperature;
the mixed particle pressed block is cut into a mixed particle block body with the size of less than or equal to 50mm × 50mm × 40mm for standby;
3) preparation of semi-solid mixed slurry
① placing mixed particle block and magnesium alloy block
Cutting 2500g of magnesium alloy ingot into magnesium alloy blocks with the size of less than or equal to 50mm × 50mm × 40mm, and then putting the mixed particle blocks and the magnesium alloy blocks into a preheating furnace for preheating, wherein the preheating temperature is 220 ℃, and the preheating time is 25 min;
starting and adjusting a second heater on the semi-solid melting crucible in the semi-solid melting furnace, preheating the semi-solid melting crucible by the second heater at the preheating temperature of 250 ℃ for 15min, and then closing the second heater;
placing the preheated mixed particle blocks and the magnesium alloy blocks in a preheated semi-solid smelting crucible in a mutually staggered manner, and then sealing the semi-solid smelting furnace;
starting a vacuum pump on the semi-solid smelting furnace, pumping air in the furnace by the vacuum pump to reduce the air pressure in the furnace to 2Pa, and then closing the vacuum pump;
the second heater is started to heat the semi-solid smelting crucible, and when the temperature of the semi-solid smelting crucible rises to 350 ℃, the protective gas cylinder is arranged towards the semi-solid smelting crucible through a gas inlet pipe on the semi-solid smelting furnaceIntroducing protective gas into the solid smelting furnace at the speed of 200cm3Min, simultaneously, regulating and controlling the air pressure in the furnace by using an exhaust pipe on the semi-solid smelting furnace to keep the air pressure in the furnace at 1 atmosphere;
② semi-solid smelting
Adjusting a second heater, heating and smelting the mixed particle block and the magnesium alloy block, wherein the heating rate is 10 ℃/min, and when the temperature of the semi-solid smelting crucible rises to 650 +/-1 ℃, preserving the heat for 20 min;
adjusting the second heater to reduce the temperature of the semi-solid melting crucible to 625 +/-1 ℃, then starting a fourth ultrasonic vibration table below the semi-solid melting crucible to perform constant-temperature vibration stirring, wherein the ultrasonic frequency is 120kHz, the stirring time is 15min, and then closing the fourth ultrasonic vibration table;
starting an electromagnetic stirrer in the semi-solid smelting furnace to stir by a rotating magnetic field, wherein the stirring frequency is 35Hz, clockwise stirring and anticlockwise stirring are alternately carried out, the clockwise single stirring time is 30s, the anticlockwise single stirring time is 30s, the stirring time is 15min in total, and then closing the electromagnetic stirrer;
adjusting the second heater to reduce the temperature of the semi-solid melting crucible to 615 +/-1 ℃, then starting a fourth ultrasonic vibration table to perform constant-temperature vibration stirring, wherein the ultrasonic frequency is 100kHz, the stirring time is 5min, then closing the fourth ultrasonic vibration table, and standing at constant temperature for 5min to prepare semi-solid mixed slurry;
4) electromagnetic pump transmission forming
① preheating forming die
Preheating a movable mold core and a fixed mold core of a forming mold by adopting a resistance wire heating mode, wherein the preheating temperature of the movable mold core is 330 +/-1 ℃, and the preheating temperature of the fixed mold core is 350 +/-1 ℃;
uniformly spraying a magnesium oxide release agent on the surface of a die cavity of a forming die, wherein the spraying thickness is 0.05 mm;
② semi-solid slurry is injected into the cavity of the mold
Starting an electromagnetic pump, conveying the semi-solid mixed slurry in the semi-solid melting crucible into a die cavity of a forming die through a material pipe by the electromagnetic pump, continuously pressurizing by the electromagnetic pump after the semi-solid mixed slurry is filled in the die cavity of the forming die to enable the static pressure head pressure to rise to 0.65MPa +/-0.05 MPa and the pressurizing time to be 25s, and then closing the electromagnetic pump to obtain a graphene oxide composite magnesium-based material casting;
③ demolding of graphene oxide composite magnesium-based material castings
Opening the forming die, ejecting the graphene oxide composite magnesium-based material casting by an ejection mechanism of the forming die, taking down the graphene oxide composite magnesium-based material casting, placing the graphene oxide composite magnesium-based material casting on a wooden flat plate, and cooling the graphene oxide composite magnesium-based material casting to room temperature in the air;
5) cleaning and rinsing
Cleaning each part and the periphery of the graphene oxide composite magnesium-based material casting by using a steel wire brush, cleaning the graphene oxide composite magnesium-based material casting by using absolute ethyl alcohol, and drying after cleaning;
6) detection, analysis, characterization
Detecting, analyzing and representing the appearance, the tissue structure and the mechanical property of the graphene oxide composite magnesium-based material casting;
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 graphene oxide composite magnesium-based material casting has the advantages of good compactness of internal tissues, no shrinkage cavity or shrinkage porosity defects, round and fine crystal grains, uniform dispersion of graphene oxide in a matrix, no agglomeration, good interface bonding, casting tensile strength of 295MPa, elongation of 5.5 percent and hardness of 103 HV.
Advantageous effects
Compared with the prior art, the method has obvious advancement, and aims at solving the problems that graphene oxide is easy to agglomerate and cannot produce parts with complex structures in the current graphene oxide composite magnesium-based material forming and processing process, mixed particles are prepared by surface treatment of rod-shaped magnesium alloy particles, high-temperature pressing is carried out, semi-solid mixed slurry is prepared, the mixture is transmitted and formed by an electromagnetic pump, and a graphene oxide composite magnesium-based material casting is formed. The forming method is advanced in process and precise and detailed in data, the prepared graphene oxide composite magnesium-based material casting has good internal tissue compactness, no shrinkage cavity and shrinkage porosity defects, round and fine crystal grains, the graphene oxide is uniformly dispersed in the matrix and does not agglomerate, the interface bonding is good, the tensile strength of the casting reaches 295MPa, the elongation reaches 5.5%, and the hardness reaches 103HV, and the method is an advanced semi-solid casting forming method for the graphene oxide composite magnesium-based material.
Drawings
FIG. 1 is a view showing a state of a mixed particle prepared by surface treatment of a rod-shaped magnesium alloy particle.
Fig. 2 is a high-temperature pressing state diagram.
FIG. 3 is a view showing a state where a mixed particle mass and a magnesium alloy mass are placed.
Fig. 4 is a diagram of a semi-solid melting state.
Fig. 5 is a state diagram of a mold cavity of the semi-solid mixed slurry injection molding mold.
Fig. 6 is a demolding state diagram of the graphene oxide composite magnesium-based material casting.
As shown in the figures, the list of reference numbers is as follows:
1-a first control cabinet, 2-a mixed particle preparation chamber, 3-a first cable, 4-a second cable, 5-a polyvinyl alcohol solution tank, 6-a deionized water tank, 7-a graphene oxide dispersion liquid tank, 8-a monorail crane, 9-a hanging clamp, 10-a treatment tank, 11-a polyvinyl alcohol solution, 12-deionized water, 13-a graphene oxide dispersion liquid, 14-a first temperature controller, 15-a first ultrasonic vibration table, 16-a second temperature controller, 17-a second ultrasonic vibration table, 18-a third temperature controller, 19-a third ultrasonic vibration table, 20-a heating dryer, 21-rod-shaped magnesium alloy particles, 22-a male mold of a pressing mold, 23-a female mold of the pressing mold, 24-a first heater, 25-a top rod of the pressing mold, 26-mixed particles, 27-a second control cabinet, 28-a semi-solid smelting furnace, 29-a semi-solid smelting crucible, 30-a third cable, 31-a fourth cable, 32-an electromagnetic stirrer, 33-a second heater, 34-a fourth ultrasonic vibration table, 35-an electromagnetic pump, 36-a material pipe, 37-a magnesium alloy block, 38-a mixed particle block, 39-a protective gas cylinder, 40-a gas inlet pipe, 41-a gas outlet pipe, 42-a vacuum pump, 43-semi-solid mixed slurry, 44-a movable mould back plate of a forming mould, 45-a movable mould frame of the forming mould, 46-a movable mould core of the forming mould, 47-a fixed mould back plate of the forming mould, 48-a fixed mould core of the forming mould and 49-a movable mould heating hole of the forming mould, 50-a fixed die heating hole of a forming die, 51-an ejection mechanism of the forming die, 52-a sprue bush of the forming die and 53-a graphene oxide composite magnesium-based material casting.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
FIG. 1 is a diagram showing a state of preparing a mixed particle by surface treatment of a rod-shaped magnesium alloy particle;
the whole set of equipment comprises a first control cabinet 1, a mixed particle preparation chamber 2, a first cable 3, a second cable 4, a polyvinyl alcohol solution tank 5, a deionized water tank 6, a graphene oxide dispersion liquid tank 7, a monorail crane 8, a hanging clamp 9, a treatment tank 10, a first temperature controller 14, a first ultrasonic vibration table 15, a second temperature controller 16, a second ultrasonic vibration table 17, a third temperature controller 18, a third ultrasonic vibration table 19 and a heating dryer 20;
the first control cabinet 1 respectively controls the working states of a monorail crane 8, a hanging tong 9, a first temperature controller 14, a first ultrasonic vibration table 15, a second temperature controller 16, a second ultrasonic vibration table 17, a third temperature controller 18, a third ultrasonic vibration table 19 and a heating dryer 20 through a first cable 3 and a second cable 4;
a monorail crane 8 is installed above the mixed particle preparation chamber 2; the hanging tongs 9 is arranged at the lower end of the hanging arm of the monorail hoist 8; the treatment box 10 is a mesh box body; the first ultrasonic vibration table 15, the second ultrasonic vibration table 17 and the third ultrasonic vibration table 19 are all arranged on the inner bottom wall of the mixed particle preparation chamber 2; the polyvinyl alcohol solution tank 5 is arranged on the table top of the first ultrasonic vibration table 15; the deionized water tank 6 is arranged on the table top of the second ultrasonic vibration table 17; the graphene oxide dispersion liquid tank 7 is arranged on the table top of the third ultrasonic vibration table 19; the first temperature controller 14 is arranged on the inner bottom wall of the polyvinyl alcohol solution tank 5; the second temperature controller 16 is arranged on the inner bottom wall of the deionized water tank 6; the third temperature controller 18 is arranged on the inner bottom wall of the graphene oxide dispersion liquid tank 7; the heating dryer 20 is arranged above the deionized water tank 6;
in the process of preparing mixed particles by surface treatment of the rod-shaped magnesium alloy particles, a polyvinyl alcohol solution 11 is contained in the polyvinyl alcohol solution tank 5 and is used for carrying out surface treatment on the rod-shaped magnesium alloy particles 21; deionized water 12 is contained in the deionized water tank 6 and used for cleaning rod-shaped magnesium alloy particles 21; the graphene oxide dispersion liquid tank 7 contains a graphene oxide dispersion liquid 13 for preparing mixed particles 26; rod-shaped magnesium alloy particles 21 are contained in the treatment box 10, the rod-shaped magnesium alloy particles 21 cannot leak out of the meshes of the treatment box 10, and external liquid enters the treatment box 10 through the meshes of the treatment box 10; the monorail crane 8 and the hanging tongs 9 are utilized to place the treatment box 10 into the polyvinyl alcohol solution box 5, the deionized water box 6 and the graphene oxide dispersion liquid box 7, the treatment box 10 can be taken out of the polyvinyl alcohol solution box 5, the deionized water box 6 and the graphene oxide dispersion liquid box 7, and the treatment box 10 can be placed beside the heating dryer 20.
FIG. 2 is a high temperature press state diagram;
the pressing mould comprises a male mould 22, a female mould 23 and a mandril 25; the outer side wall of the female die 23 of the pressing die is provided with a first heater 24;
in the high-temperature pressing process, a first heater 24 on a pressing mold is started and adjusted, and the female mold 23 and the male mold 22 of the pressing mold are preheated by the first heater 24; placing the mixed particles 26 into a concave die 23 of a pressing die, and then closing the pressing die; after the die assembly is finished, keeping the temperature and the pressure at constant temperature to prepare a mixed particle pressed block; opening the pressing die, and ejecting the mixed particle pressed block by an ejector rod 25 of the pressing die; the blended granulation is pressed into briquettes and cut into briquettes 38.
FIG. 3 is a view showing a state where a mixed particle block and a magnesium alloy block are placed;
the whole set of equipment comprises a second control cabinet 27, a semi-solid smelting furnace 28, a semi-solid smelting crucible 29, a third cable 30, a fourth cable 31, an electromagnetic stirrer 32, a second heater 33, a fourth ultrasonic vibration table 34, an electromagnetic pump 35, a material pipe 36, a protective gas cylinder 39, a gas inlet pipe 40, a gas outlet pipe 41 and a vacuum pump 42;
the second control cabinet 27 controls the working states of the semi-solid smelting furnace 28, the electromagnetic stirrer 32, the second heater 33, the fourth ultrasonic vibration table 34, the electromagnetic pump 35 and the vacuum pump 42 through a third cable 30 and a fourth cable 31 respectively;
the fourth ultrasonic vibration table 34 is arranged on the inner bottom wall of the semi-solid smelting furnace 28; the semi-solid smelting crucible 29 is arranged on the table top of the fourth ultrasonic vibration table 34; the second heater 33 is arranged on the outer side wall of the semi-solid smelting crucible 29; the electromagnetic stirrer 32 is provided outside the second heater 33; the gas inlet pipe 40 is arranged at the upper part of the left side wall of the semi-solid smelting furnace 28; the exhaust pipe 41 is arranged at the upper part of the right side wall of the semi-solid smelting furnace 28; the protective gas cylinder 39 is communicated with the semi-solid smelting furnace 28 through a gas inlet pipe 40; the vacuum pump 42 is arranged at the lower part of the right side wall of the semi-solid smelting furnace 28;
in the process of placing the mixed particle block and the magnesium alloy block, the second heater 33 on the semi-solid melting crucible 29 in the semi-solid melting furnace 28 is started and adjusted, the semi-solid melting crucible 29 is preheated by the second heater 33, and then the second heater 33 is closed; placing the preheated mixed particle blocks 38 and the magnesium alloy blocks 37 in the preheated semi-solid melting crucible 29 in a mutually staggered manner, and then sealing the semi-solid melting furnace 28; starting a vacuum pump 42 on the semi-solid smelting furnace 28, pumping air in the furnace by the vacuum pump 42, and then closing the vacuum pump 42; the protective gas bottle 39 is used for introducing protective gas into the semi-solid smelting furnace 28 through a gas inlet pipe 40 on the semi-solid smelting furnace 28, and meanwhile, the gas pressure in the semi-solid smelting furnace 28 is regulated and controlled through a gas outlet pipe 41 on the semi-solid smelting furnace 28.
FIG. 4 is a diagram showing a semi-solid smelting state;
in the semi-solid smelting process, the second heater 33 is adjusted to heat and smelt the mixed particle block 38 and the magnesium alloy block 37; adjusting the second heater 33, then starting a fourth ultrasonic vibration table 34 below the semi-solid melting crucible 29 for constant-temperature vibration stirring, and then closing the fourth ultrasonic vibration table 34; starting an electromagnetic stirrer 32 in the semi-solid smelting furnace 28 for stirring by a rotating magnetic field, and then closing the electromagnetic stirrer 32; and adjusting the second heater 33, then starting the fourth ultrasonic vibration table 34 to perform constant-temperature vibration stirring, and then closing the fourth ultrasonic vibration table 34 to prepare the semi-solid mixed slurry 43.
FIG. 5 is a schematic view showing a state in which the semi-solid mixed slurry is injected into a cavity of a molding die;
the forming die comprises a movable die back plate 44, a movable die frame 45, a movable die core 46, a fixed die back plate 47, a fixed die core 48, an ejection mechanism 51 and a sprue bush 52; a movable mold heating hole 49 is formed in the movable mold core 46, a fixed mold heating hole 50 is formed in the fixed mold core 48, and the movable mold core 46 and the fixed mold core 48 jointly enclose a mold cavity;
and in the process of injecting the semi-solid mixed slurry into the die cavity of the forming die, starting the electromagnetic pump 35, conveying the semi-solid mixed slurry 43 in the semi-solid melting crucible 29 into the die cavity of the forming die through the material pipe 36 by the electromagnetic pump 35, continuously pressurizing by the electromagnetic pump 35 after the semi-solid mixed slurry 43 is filled in the die cavity of the forming die, and then closing the electromagnetic pump 35 to obtain the graphene oxide composite magnesium-based material casting 53.
FIG. 6 is a diagram showing a demolding state of a graphene oxide composite magnesium-based material casting;
in the demolding process of the graphene oxide composite magnesium-based material casting, the mold is opened, the graphene oxide composite magnesium-based material casting 53 is ejected out by the ejection mechanism 51 of the mold, and then the graphene oxide composite magnesium-based material casting 53 is taken down.
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 semi-solid casting forming method of graphene oxide composite magnesium-based material is characterized by comprising the following steps:
the chemical materials used were: the magnesium alloy mold release agent comprises a magnesium alloy ingot, graphene oxide, polyvinyl alcohol, deionized water, absolute ethyl alcohol and a magnesium oxide mold release agent, wherein the combined preparation dosage is as follows: taking g and ml as measurement unit
Magnesium alloy ingot: ZM5 solid block 5000 g. + -. 1g
Graphene oxide solid powder 20g +/-0.1 g
Polyvinyl alcohol: [ C ]2H4O]n solid powder 600g +/-10 g
Deionized water: h2O liquid 58000m L +/-500 m L
Anhydrous ethanol: c2H5OH liquid 2500m L +/-100 m L
Magnesium oxide release agent liquid 80m L +/-5 m L
The preparation method comprises the following steps:
1) preparation of mixed particles by surface treatment of rod-shaped magnesium alloy particles
① cutting rod-shaped magnesium alloy particles
Cutting 2500g of magnesium alloy ingot into rod-shaped magnesium alloy particles with the length of 5mm +/-1.5 mm and the equivalent diameter of the cross section of phi 0.50mm +/-0.15 mm by using a metal particle cutting machine for later use;
② preparing polyvinyl alcohol solution
Adding 20000m L deionized water into a polyvinyl alcohol solution tank in a mixed particle preparation chamber, starting and adjusting a first temperature controller in the polyvinyl alcohol solution tank to keep the temperature of the deionized water at 85 ℃, then adding 600g of polyvinyl alcohol, keeping the temperature for 0.5h, then starting a first ultrasonic vibration table below the polyvinyl alcohol solution tank for vibration stirring, and after the polyvinyl alcohol is completely dissolved, closing the first ultrasonic vibration table and the first temperature controller to prepare the polyvinyl alcohol solution;
③ preparing graphene oxide dispersion liquid
Preparing graphene oxide with the transverse dimension of 10 microns +/-1 micron, the thickness of 3nm +/-0.5 nm and the oxygen content of 31.5at +/-1 at% by adopting a Hummers method;
adding 20000m L deionized water into a graphene oxide dispersion liquid tank in a mixed particle preparation chamber, starting and adjusting a third temperature controller in the graphene oxide dispersion liquid tank to keep the temperature of the deionized water at 50 ℃, then adding 20g of graphene oxide, starting a third ultrasonic vibration table below the graphene oxide dispersion liquid tank for vibration stirring for 40min, and then closing the third ultrasonic vibration table and the third temperature controller to prepare graphene oxide dispersion liquid;
④ surface treatment of rod-shaped magnesium alloy particles
Starting and adjusting a first temperature controller to keep the temperature of the polyvinyl alcohol solution at 75 +/-2 ℃;
putting the rod-shaped magnesium alloy particles into a treatment box, and then putting the treatment box into a polyvinyl alcohol solution box by using a monorail crane and a hanging tongs, so that the rod-shaped magnesium alloy particles are completely soaked in the polyvinyl alcohol solution;
after the temperature is kept for 20min, starting a first ultrasonic vibration table to carry out constant-temperature vibration stirring for 45min, then closing the first ultrasonic vibration table and a first temperature controller, and standing for 15 min;
⑤ cleaning rod-shaped magnesium alloy particles
Adding 18000m L deionized water into a deionized water tank in the mixed particle preparation chamber, starting and adjusting a second temperature controller in the deionized water tank to keep the temperature of the deionized water at 65 +/-2 ℃, taking the treatment tank out of the polyvinyl alcohol solution tank by using a monorail crane and a hanging clamp, and then putting the treatment tank into the deionized water tank to completely soak the rod-shaped magnesium alloy particles in the deionized water;
starting a second ultrasonic vibration table below the deionized water tank for vibration cleaning for 15min, and then closing the second ultrasonic vibration table and a second temperature controller;
taking the treatment box out of the deionized water tank by using a monorail crane and a hanging clamp, placing the treatment box beside a heating dryer, then starting the heating dryer to dry the rod-shaped magnesium alloy particles, wherein the drying temperature is 75 ℃, the drying time is 30min, and then closing the heating dryer;
⑥ preparation of Mixed granules
Starting and adjusting a third temperature controller to keep the temperature of the graphene oxide dispersion liquid at 45 +/-2 ℃, and then putting the treatment box into the graphene oxide dispersion liquid box by using a monorail crane and a hanging tong to completely soak the rod-shaped magnesium alloy particles in the graphene oxide dispersion liquid;
after the temperature is kept for 5min, starting a third ultrasonic vibration table to carry out constant-temperature vibration stirring, pausing stirring for 10min every time stirring is carried out for 10min, stirring for 4 times in total, then closing the third ultrasonic vibration table and a third temperature controller, and standing for 20 min;
taking the treatment box out of the graphene oxide dispersion liquid box by using a monorail crane and a hanging clamp, then putting the rod-shaped magnesium alloy particles adsorbed with the graphene oxide into a constant-temperature oven for drying at 60 ℃ for 30min, and taking out after drying to obtain mixed particles;
2) high temperature pressing
Starting and adjusting a first heater on a pressing die, wherein the first heater preheats a female die and a male die of the pressing die, and the preheating temperature is 350 ℃;
putting the mixed particles into a concave die of a pressing die, and closing the pressing die; keeping the pressure at constant temperature after the die assembly is finished, wherein the pressure keeping pressure is 180MPa, and the pressure keeping time is 15min, so as to prepare a mixed particle pressed block;
opening a pressing die, ejecting the mixed particle pressed block by an ejector rod of the pressing die, taking down the mixed particle pressed block, and placing the mixed particle pressed block on a steel flat plate to be cooled to room temperature;
the mixed particle pressed block is cut into a mixed particle block body with the size of less than or equal to 50mm × 50mm × 40mm for standby;
3) preparation of semi-solid mixed slurry
① placing mixed particle block and magnesium alloy block
Cutting 2500g of magnesium alloy ingot into magnesium alloy blocks with the size of less than or equal to 50mm × 50mm × 40mm, and then putting the mixed particle blocks and the magnesium alloy blocks into a preheating furnace for preheating, wherein the preheating temperature is 220 ℃, and the preheating time is 25 min;
starting and adjusting a second heater on the semi-solid melting crucible in the semi-solid melting furnace, preheating the semi-solid melting crucible by the second heater at the preheating temperature of 250 ℃ for 15min, and then closing the second heater;
placing the preheated mixed particle blocks and the magnesium alloy blocks in a preheated semi-solid smelting crucible in a mutually staggered manner, and then sealing the semi-solid smelting furnace;
starting a vacuum pump on the semi-solid smelting furnace, pumping air in the furnace by the vacuum pump to reduce the air pressure in the furnace to 2Pa, and then closing the vacuum pump;
starting a second heater, heating the semi-solid smelting crucible by the second heater, and introducing protective gas into the semi-solid smelting furnace through a gas inlet pipe on the semi-solid smelting furnace by the protective gas bottle when the temperature of the semi-solid smelting crucible rises to 350 ℃, wherein the introducing speed of the protective gas is 200cm3Min, simultaneously, regulating and controlling the air pressure in the furnace by using an exhaust pipe on the semi-solid smelting furnace to keep the air pressure in the furnace at 1 atmosphere;
② semi-solid smelting
Adjusting a second heater, heating and smelting the mixed particle block and the magnesium alloy block, wherein the heating rate is 10 ℃/min, and when the temperature of the semi-solid smelting crucible rises to 650 +/-1 ℃, preserving the heat for 20 min;
adjusting the second heater to reduce the temperature of the semi-solid melting crucible to 625 +/-1 ℃, then starting a fourth ultrasonic vibration table below the semi-solid melting crucible to perform constant-temperature vibration stirring, wherein the ultrasonic frequency is 120kHz, the stirring time is 15min, and then closing the fourth ultrasonic vibration table;
starting an electromagnetic stirrer in the semi-solid smelting furnace to stir by a rotating magnetic field, wherein the stirring frequency is 35Hz, clockwise stirring and anticlockwise stirring are alternately carried out, the clockwise single stirring time is 30s, the anticlockwise single stirring time is 30s, the stirring time is 15min in total, and then closing the electromagnetic stirrer;
adjusting the second heater to reduce the temperature of the semi-solid melting crucible to 615 +/-1 ℃, then starting a fourth ultrasonic vibration table to perform constant-temperature vibration stirring, wherein the ultrasonic frequency is 100kHz, the stirring time is 5min, then closing the fourth ultrasonic vibration table, and standing at constant temperature for 5min to prepare semi-solid mixed slurry;
4) electromagnetic pump transmission forming
① preheating forming die
Preheating a movable mold core and a fixed mold core of a forming mold by adopting a resistance wire heating mode, wherein the preheating temperature of the movable mold core is 330 +/-1 ℃, and the preheating temperature of the fixed mold core is 350 +/-1 ℃;
uniformly spraying a magnesium oxide release agent on the surface of a die cavity of a forming die, wherein the spraying thickness is 0.05 mm;
② semi-solid slurry is injected into the cavity of the mold
Starting an electromagnetic pump, conveying the semi-solid mixed slurry in the semi-solid melting crucible into a die cavity of a forming die through a material pipe by the electromagnetic pump, continuously pressurizing by the electromagnetic pump after the semi-solid mixed slurry is filled in the die cavity of the forming die to enable the static pressure head pressure to rise to 0.65MPa +/-0.05 MPa and the pressurizing time to be 25s, and then closing the electromagnetic pump to obtain a graphene oxide composite magnesium-based material casting;
③ demolding of graphene oxide composite magnesium-based material castings
Opening the forming die, ejecting the graphene oxide composite magnesium-based material casting by an ejection mechanism of the forming die, taking down the graphene oxide composite magnesium-based material casting, placing the graphene oxide composite magnesium-based material casting on a wooden flat plate, and cooling the graphene oxide composite magnesium-based material casting to room temperature in the air;
5) cleaning and rinsing
Cleaning each part and the periphery of the graphene oxide composite magnesium-based material casting by using a steel wire brush, cleaning the graphene oxide composite magnesium-based material casting by using absolute ethyl alcohol, and drying after cleaning;
6) detection, analysis, characterization
Detecting, analyzing and representing the appearance, the tissue structure and the mechanical property of the graphene oxide composite magnesium-based material casting;
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 graphene oxide composite magnesium-based material casting has the advantages of good compactness of internal tissues, no shrinkage cavity or shrinkage porosity defects, round and fine crystal grains, uniform dispersion of graphene oxide in a matrix, no agglomeration, good interface bonding, casting tensile strength of 295MPa, elongation of 5.5 percent and hardness of 103 HV.
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