CN109182821B - Die casting method for graphene-reinforced ADC12 aluminum alloy - Google Patents
Die casting method for graphene-reinforced ADC12 aluminum alloy Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 56
- 238000004512 die casting Methods 0.000 title claims abstract description 32
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 77
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 69
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000956 alloy Substances 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 32
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 30
- 238000001816 cooling Methods 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 24
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 17
- 238000002347 injection Methods 0.000 claims description 17
- 239000007924 injection Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 16
- 238000009210 therapy by ultrasound Methods 0.000 claims description 16
- 238000004321 preservation Methods 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 14
- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 5
- 238000007872 degassing Methods 0.000 claims description 5
- 230000002431 foraging effect Effects 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 6
- 238000003825 pressing Methods 0.000 abstract description 4
- 125000000524 functional group Chemical group 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 8
- 238000011160 research Methods 0.000 description 6
- 238000007747 plating Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000003014 reinforcing effect Effects 0.000 description 4
- 238000010335 hydrothermal treatment Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
- C22B9/026—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves by acoustic waves, e.g. supersonic waves
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/101—Pretreatment of the non-metallic additives by coating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
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- Acoustics & Sound (AREA)
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- Carbon And Carbon Compounds (AREA)
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Abstract
A die-casting method of graphene-reinforced ADC12 aluminum alloy is characterized in that in an anhydrous environment, alcohol heat high pressure is utilized, Ti ions are adsorbed under the action of a self-carried functional group of carboxylated graphene GO, and TiO2 (anatase type) coated carboxylated graphene GO is obtained in later-stage roasting. And mixing the obtained powder with pure aluminum powder according to a certain proportion, and cold-pressing to obtain the intermediate alloy. Adding the intermediate alloy into the aluminum alloy melt as required, and dispersing the titanium oxide coated graphene GO particles under the action of a high-energy ultrasonic instrument. Pouring the obtained slurry into a sprue of a die casting machine for die casting to obtain a die-casting blank, and then carrying out T6 heat treatment on the blank to obtain the high-performance composite material under the action of correct process parameters. The product prepared by the invention has excellent mechanical properties, and meanwhile, the invention has the advantages of simplicity, safety, easy operation, controllability and the like.
Description
Technical Field
The invention belongs to the technical field of material preparation.
Background
Graphene nanoplatelets are two-dimensional materials of monoatomic layer thickness consisting of sp2 hybridized carbon atoms, which exhibit a range of unusual physical properties. The graphene nanosheets have special two-dimensional structures, so that great interest of researchers in the physical, chemical and material science communities is brought, and basic research and engineering application research related to graphene become research hotspots in recent years. Due to the fact that graphene has high strength and tensile strength of 130GPa, the graphene has a huge application space in material application research.
In fact, research on enhancing the strength and other mechanical properties of aluminum materials using carbon materials such as carbon nanotubes or graphene has been ongoing and has made some progress. However, due to their extremely outstanding physical properties such as strength, their excellent properties in terms of material wear and hardness have been rather ignored.
With the development of national economy, people have more severe requirements on the high speed and heavy load of the carrying tool. If the surface layer of the brake disc of the vehicle is required to bear higher temperature in braking, the corresponding aluminum material is required to have more excellent wear resistance, better heat resistance and the like. A large number of researches show that the correct selection of the reinforcing phase can directly improve the wear resistance and hardness of the composite material. Due to the basic properties of the carbon material, the carboxylated graphene naturally inherits the characteristics of self lubrication, good heat dissipation and the like which are different from other reinforced materials. Proper use can effectively reduce material loss.
However, the defects of the carboxylated graphene are also obvious. The structures of carboxylated graphene similar to CNTs show very poor wettability, which directly results in poor interfacial bonding with the metal matrix, and is not favorable for the preparation of composite materials. Therefore, improving the wettability with the substrate and selecting the right process method become the key to using graphene to reinforce the metal-based material.
The existing method for improving the wettability of the carboxylated graphene comprises surface coating and the like, such as chemical nickel plating, the method is mainly characterized in that the carboxylated graphene is sensitized and activated and then put into chemical plating solution for plating, and a granular coating can be obtained on the surface of the carboxylated graphene along with the reaction, but the price is high, toxic reagents are commonly used, the method is not environment-friendly and high in production cost, and the method is not suitable for large-scale production.
In published patent No. 106702193a, the name is: the preparation method of the graphene/aluminum composite material is disclosed. And pretreating the graphene by chemical plating to obtain the nickel-plated graphene. Then mixing the powder and carrying out conventional hot-pressing sintering. In fact, the method has great harm to human bodies due to the limitation of chemical plating, and the graphene needs to be carboxylated independently, so that the production period is long, the waste degree of the powder is high, and the method has certain limitation.
Therefore, an economical and effective preparation and forming technology of the carboxylated graphene reinforced aluminum matrix composite material is still lacked at present.
Disclosure of Invention
The invention aims to provide a die casting method for graphene reinforced ADC12 aluminum alloy. The method comprises the steps of coating a layer of titanium oxide on the surface of carboxylated graphene by an alcohol heating method, and uniformly dispersing a nano enhanced phase in a matrix by using cavitation and acoustic flow effects of high-energy ultrasound when the enhanced phase is added to the matrix. The method has low cost and can be used for mass production. At the same time, formedAluminiumThe/graphene interface is stably combined through the titanium oxide layer, the combination performance is good, and the obtained composite material is fine in grain and excellent in mechanical performance.
The content of titanium oxide coated carboxylated graphene, the control of the environment and the determination of process parameters are very important in the process of die casting, and the three links are linked and buckled with each other, so that the quality of the product is directly influenced.
The specific principle of the invention is as follows: and (3) uniformly diffusing the titanium oxide coated carboxylated graphene particles into the matrix through the cavitation of high-energy ultrasound and the acoustic flow effect. In order to reduce the agglomeration of titanium oxide coated graphene particles, the surface of carboxylated graphene is treated by an alcohol heating method, so that the surface of the carboxylated graphene is coated with titanium oxide as a stable particle protective layer. Meanwhile, in the process of preparing the composite material slurry, high-energy ultrasonic vibration is introduced, so that the reinforcing phase and the intermediate phase can be effectively dispersed, and the mechanical property of the composite material is improved. In the process of die-casting solidification, the bonding strength of an aluminum/graphene interface can be effectively enhanced, and the carboxylated graphene is more stably fixed in a matrix, so that a product with excellent mechanical properties is obtained.
The invention is realized by the following technical scheme.
The die casting method of the graphene reinforced ADC12 aluminum alloy comprises the following steps.
(1) Performing ultrasonic pre-dispersion on carboxylated graphene in analytically pure ethanol for 1-3 hours at room temperature, and controlling the whole process to be free of water vapor. The volume ratio is controlled to be 0.2-0.4: 50.
(2) pouring the carboxylated graphene dispersion liquid pretreated in the step (1) into a precursor liquid composed of glycerol and tetraisopropyl titanate, sealing, and carrying out ultrasonic treatment again for 1-1.5 hours. Wherein the volume ratio of the glycerol to the tetraisopropyl titanate is 10: 0.4-1.2.
(3) And (3) introducing the precursor suspension obtained in the step (2) into a hydrothermal reaction kettle, wherein the volume of the suspension accounts for 35-70% of the volume of the reaction kettle. Heating the mixture in a reaction furnace, heating the mixture to 70-110 ℃ at a speed of 1-5 ℃/min, preserving heat for 1-2 hours, heating the mixture to 175-180 ℃ at a speed of 1-3 ℃/min, and preserving heat for 10-15 hours; taking out, sealing the reaction kettle and air cooling.
(4) And (4) taking out the solution obtained in the step (3), centrifuging, pouring analytically pure ethanol, and centrifuging for multiple times until the solution is colorless, wherein the rotating speed is controlled at 9000-16000 rpm. The whole process is sealed to ensure no water vapor.
(5) And (4) drying the mixed powder obtained in the step (4) in vacuum, and then roasting at 450-500 ℃ under the protection of argon. The time is controlled to be 1-3 h. The carboxylated graphene with the needle-shaped anatase titanium oxide coating on the surface can be obtained.
(6) Mixing the carboxylated graphene particles with the needle-shaped anatase titanium oxide coating on the surface obtained in the step (5) with pure aluminum powder at a mixing ratio of 1:4, maintaining the pressure of the mixed powder at 400MPa for 10min by cold pressure to prepare titanium oxide coated carboxylated graphene/aluminum precast blocks, and then cutting the precast blocks into pieces.
(7) The ADC12 aluminum alloy was placed in a graphite crucible and then heated to 750 ℃ in a well-type resistance furnace and held until molten. And after the aluminum alloy block ADC12 is completely melted, refining, degassing and deslagging the alloy melt. And (4) adding the titanium oxide coated carboxylated graphene/aluminum precast block obtained in the step (6) into the alloy melt, and controlling the content of titanium oxide coated graphene particles in the product to be 0.5-2.5 wt% according to the addition amount of the precast block.
(8) And then inserting an ultrasonic amplitude transformer into the melt to perform high-energy ultrasonic treatment on the alloy melt, introducing argon for protection in the process, wherein the flow of the argon is 20L/min, the pressure of the argon is 0.45MPa, and the process parameters comprise 1.5-2.5 Kw of ultrasonic power, 15000-25000 Hz of ultrasonic frequency and 10-20 min of ultrasonic time.
(9) And (3) preserving the temperature of the composite material slurry in the step (8) for 15min, skimming the obtained mixed melt after heat preservation, sampling and analyzing the mixed melt after skimming, and reducing the temperature of the melt with qualified components to 680-710 ℃ for heat preservation for later use.
(10) Pouring the slurry with qualified components obtained in the step (9) into a pouring gate of a die casting machine, and die-casting the slurry into a columnar aluminum alloy material; the die casting process is set as follows: controlling the casting temperature to be 680-710 ℃, controlling the thickness of the material handle to be 25mm, and controlling the temperature of the die to be 150-170 ℃; the injection pressure is controlled to be 330kN, and the diameter of the hammer head is controlled to be 60 mm; the injection pressure is controlled to be 116MPa, the injection time is controlled to be 3S, the cooling time is controlled to be 2S, and the mold remaining time is controlled to be 10S; the die handle action stroke position in the die-casting process is as follows: the slow shot start position was controlled to 80mm, the fast shot start position was controlled to 270mm, the pressurizing position was controlled to 280mm, and the tracking position was controlled to 350 mm.
(11) And (3) placing the blank obtained in the step (10) into a resistance furnace for primary solution treatment, wherein the temperature of the solution treatment is 440 +/-3 ℃, the heat preservation time is 2.5-3.5 hours, and then, quickly placing the blank into water with the temperature of 20 ℃ for cooling.
(12) And (3) placing the material obtained in the step (11) in a resistance furnace for secondary solution treatment, wherein the temperature of the solution treatment is 480 +/-3 ℃, the heat preservation time is 1.5-2.5 hours, and then quickly placing the material in water with the temperature of 20 ℃ for cooling.
(13) And (3) placing the material obtained in the step (12) at a temperature of 125 +/-3 ℃ for aging treatment, wherein the aging time is 5-6 hours, and then air cooling.
According to the invention, the titanium oxide-coated carboxylated graphene surface is treated by an alcohol-thermal method so as to improve the interface bonding strength between the carboxylated graphene and an ADC12 matrix, and titanium oxide-coated carboxylated graphene particles are uniformly dispersed by introducing high-energy ultrasound, wherein the content of the titanium oxide-coated carboxylated graphene in the product is 0.5-2.5 wt%.
The invention has the following uniqueness: (1) the cavitation and acoustic flow effect of the high-energy ultrasonic wave are utilized to uniformly disperse the reinforcing phase in the product. (2) The carboxylated graphene particles in the coating have the protection effect of titanium oxide, so that the interface is better, the wettability of the carboxylated graphene particles with metal is increased, and the agglomeration probability of the carboxylated graphene particles is further reduced. (3) Internal stress generated inside the material during die casting can be effectively reduced during the T6 heat treatment process, and a reinforcing phase and an intermediate phase can be effectively dispersed through recovery recrystallization, so that a product with excellent mechanical properties is obtained.
Detailed Description
The invention will be further illustrated by the following examples.
Example 1.
The carboxylated graphene is subjected to ultrasonic pre-dispersion for 1 hour in an analytically pure ethanol clock, the temperature is room temperature, and no water vapor is controlled in the whole process. Controlling the volume ratio at 0.2:50, and then pouring the obtained dispersion into a precursor solution consisting of glycerol and tetraisopropyl titanate for sealing and ultrasonic treatment for 1 h. Wherein the volume ratio of the glycerol to the tetraisopropyl titanate is 10: 0.9. Then, hydrothermal treatment is carried out, wherein the volume of the suspension accounts for 60% of the volume of the reaction kettle. Then putting the mixture into a reaction furnace for heating, raising the temperature to 100 ℃ at the speed of 5 ℃/min, preserving the heat for 2h, raising the temperature to 180 ℃ at the speed of 3 ℃/min, and preserving the heat for 10 h. Taking out the reaction kettle and then cooling in air. The resulting solution was taken out, centrifuged and centrifuged several times by pouring analytically pure ethanol until the solution was colorless. The whole process is sealed to ensure no water vapor. Then, the obtained powder is roasted at 450 ℃ under the protection of argon. The time is controlled to be 2 h. The carboxylated graphene with the needle-shaped anatase titanium oxide coating on the surface can be obtained.
The method comprises the steps of mixing the obtained carboxylated graphene particles with needle-shaped anatase titanium oxide coatings on the surfaces with pure aluminum powder, wherein the mixing ratio is 1:4, cold-pressing the mixed powder into a precast block, putting an ADC12 aluminum alloy into a graphite crucible, heating to 750 ℃ in a well-type resistance furnace, preserving heat until the mixture is molten, refining, degassing and deslagging the alloy melt after the ADC12 aluminum alloy block is completely molten, then adding the prefabricated titanium oxide coated carboxylated graphene/aluminum precast block into the alloy melt, controlling the content of the titanium oxide coated carboxylated graphene particles in the composite material to be 0.5wt% through the addition amount of the precast block, then inserting an ultrasonic amplitude transformer into the alloy melt to perform high-energy ultrasonic treatment on the alloy melt, wherein the technological parameters comprise that the ultrasonic power is 1.5Kw, the ultrasonic frequency is 15000Hz, the ultrasonic time is 10min, introducing argon for protection in the process, the flow rate is 20L/min, the argon pressure is 0.45MPa, carrying out ultrasonic treatment for 15min after the ultrasonic treatment is finished, and reducing the temperature of the qualified alloy melt to 680 ℃ to preserve heat for later.
Pouring the slurry with qualified components into a pouring gate of a die casting machine, and die-casting into a columnar aluminum alloy material; the die casting process is set as follows: controlling the casting temperature to be 680 ℃, controlling the thickness of the material handle to be 25mm, and controlling the temperature of the die to be 150 ℃; the injection pressure is controlled to be 330kN, and the diameter of the hammer head is controlled to be 60 mm; the injection pressure is controlled to be 116MPa, the injection time is controlled to be 3S, the cooling time is controlled to be 2S, and the mold remaining time is controlled to be 10S; the die handle action stroke position in the die-casting process is as follows: the slow shot start position was controlled to 80mm, the fast shot start position was controlled to 270mm, the pressurizing position was controlled to 280mm, and the tracking position was controlled to 350 mm. Carrying out T6 heat treatment on the obtained blank, placing the obtained blank in a resistance furnace for primary solution treatment, wherein the solution treatment temperature is 420 +/-3 ℃, the heat preservation time is 2.5 hours, and then rapidly putting the blank into water with the temperature of 20 ℃ for cooling. Then placing the mixture into a resistance furnace for secondary solution treatment, wherein the temperature of the solution treatment is 460 +/-3 ℃, the heat preservation time is 1.5 hours, and then quickly placing the mixture into water with the temperature of 20 ℃ for cooling. Finally, the obtained material is placed at the temperature of 125 +/-3 ℃ for aging treatment, the aging time is 5 hours, and then air cooling is carried out, so that the ultimate tensile strength of the obtained product is improved by 19.48 percent compared with that of the substrate.
Example 2.
The carboxylated graphene is subjected to ultrasonic pre-dispersion for 1 hour in an analytically pure ethanol clock, the temperature is room temperature, and no water vapor is controlled in the whole process. The volume ratio is strictly controlled at 0.2:50, and then the obtained dispersion liquid is poured into a precursor liquid consisting of glycerol and tetraisopropyl titanate for sealing and ultrasonic treatment for 1 h. Wherein the volume ratio of the glycerol to the tetraisopropyl titanate is 10: 0.4. Then carrying out hydrothermal treatment, wherein the volume of the suspension accounts for 50% of the volume of the reaction kettle. Then putting the mixture into a reaction furnace for heating, raising the temperature to 90 ℃ at the speed of 5 ℃/min, preserving the heat for 2h, raising the temperature to 180 ℃ at the speed of 2 ℃/min, and preserving the heat for 10 h. Taking out the reaction kettle and then cooling in air. The resulting solution was taken out, centrifuged and centrifuged several times by pouring analytically pure ethanol until the solution was colorless. The whole process is sealed to ensure no water vapor. Then, the obtained powder is roasted at 480 ℃ under the protection of argon. The time is controlled to be 1.5 h. The carboxylated graphene with the needle-shaped anatase titanium oxide coating on the surface can be obtained.
The method comprises the steps of mixing the obtained carboxylated graphene particles with needle-shaped anatase titanium oxide coatings on the surfaces with pure aluminum powder, wherein the mixing ratio is 1:4, cold-pressing the mixed powder into a precast block, putting an ADC12 aluminum alloy into a graphite crucible, heating to 750 ℃ in a well-type resistance furnace, preserving heat until the graphite is molten, refining, degassing and deslagging the alloy melt after the ADC12 aluminum alloy block is completely molten, then adding the prefabricated titanium oxide coated carboxylated graphene/aluminum precast block into the alloy melt, controlling the content of the titanium oxide coated carboxylated graphene particles in the composite material to be 1.5wt% through the addition amount of the precast block, then inserting an ultrasonic amplitude transformer into the alloy melt to perform high-energy ultrasonic treatment on the alloy melt, wherein the technological parameters comprise that the ultrasonic power is 2.5Kw, the ultrasonic frequency is 25000Hz, the ultrasonic time is 15min, introducing argon for protection in the process, the flow rate is 20L/min, the argon pressure is 0.45MPa, carrying out ultrasonic treatment for 15min after the ultrasonic treatment is finished, and carrying out heat preservation treatment on the qualified alloy melt, and reducing the temperature to 710 ℃ for later.
Pouring the slurry with qualified components into a pouring gate of a die casting machine, and die-casting into a columnar aluminum alloy material; the die casting process is set as follows: controlling the casting temperature to be 710 ℃, controlling the thickness of the material handle to be 25mm, and controlling the temperature of the die to be 170 ℃; the injection pressure is controlled to be 330kN, and the diameter of the hammer head is controlled to be 60 mm; the injection pressure is controlled to be 116MPa, the injection time is controlled to be 3S, the cooling time is controlled to be 2S, and the mold remaining time is controlled to be 10S; the die handle action stroke position in the die-casting process is as follows: the slow shot start position was controlled to 80mm, the fast shot start position was controlled to 270mm, the pressurizing position was controlled to 280mm, and the tracking position was controlled to 350 mm. Carrying out T6 heat treatment on the obtained blank, placing the obtained blank in a resistance furnace for primary solution treatment, wherein the solution treatment temperature is 420 +/-3 ℃, the heat preservation time is 3.5 hours, and then rapidly putting the blank into water with the temperature of 20 ℃ for cooling. Then placing the mixture into a resistance furnace for secondary solution treatment, wherein the temperature of the solution treatment is 460 +/-3 ℃, the heat preservation time is 1.5 hours, and then quickly placing the mixture into water with the temperature of 20 ℃ for cooling. Finally, the obtained material is placed at the temperature of 125 +/-3 ℃ for aging treatment, the aging time is 5 hours, and then air cooling is carried out, so that the ultimate tensile strength of the obtained product is improved by 23.21 percent compared with that of the substrate.
Example 3.
The carboxylated graphene is subjected to ultrasonic pre-dispersion for 1 hour in an analytically pure ethanol clock, the temperature is room temperature, and no water vapor is controlled in the whole process. The volume ratio is strictly controlled at 0.2:50, and then the obtained dispersion liquid is poured into a precursor liquid consisting of glycerol and tetraisopropyl titanate for sealing and ultrasonic treatment for 1 h. Wherein the volume ratio of the glycerol to the tetraisopropyl titanate is 10: 0.4. Then carrying out hydrothermal treatment, wherein the volume of the suspension accounts for 50% of the volume of the reaction kettle. Then putting the mixture into a reaction furnace for heating, raising the temperature to 90 ℃ at the speed of 5 ℃/min, preserving the heat for 2h, raising the temperature to 180 ℃ at the speed of 2 ℃/min, and preserving the heat for 10 h. Taking out the reaction kettle and then cooling in air. The resulting solution was taken out, centrifuged and centrifuged several times by pouring analytically pure ethanol until the solution was colorless. The whole process is sealed to ensure no water vapor. Then, the obtained powder is roasted at 480 ℃ under the protection of argon. The time is controlled to be 1.5 h. The carboxylated graphene with the needle-shaped anatase titanium oxide coating on the surface can be obtained.
The method comprises the steps of mixing the obtained carboxylated graphene particles with needle-shaped anatase titanium oxide coatings on the surfaces with pure aluminum powder, wherein the mixing ratio is 1:4, cold-pressing the mixed powder into a precast block, putting an ADC12 aluminum alloy into a graphite crucible, heating to 750 ℃ in a well-type resistance furnace, preserving heat until the graphite is molten, refining, degassing and deslagging the alloy melt after the ADC12 aluminum alloy block is completely molten, then adding the prefabricated titanium oxide coated carboxylated graphene/aluminum precast block into the alloy melt, controlling the content of the titanium oxide coated carboxylated graphene particles in the composite material to be 1.5wt% through the addition amount of the precast block, then inserting an ultrasonic amplitude transformer into the alloy melt to perform high-energy ultrasonic treatment on the alloy melt, wherein the process parameters are that the ultrasonic power is 2.5Kw, the ultrasonic frequency is 25000Hz, the ultrasonic time is 15min, argon is introduced for protection in the process, the flow rate is 20L/min, the argon pressure is 0.45MPa, carrying out ultrasonic treatment for 15min after the ultrasonic treatment is finished, and preserving heat for standby after the qualified alloy melt is deslagged.
Pouring the slurry with qualified components into a pouring gate of a die casting machine, and die-casting into a columnar aluminum alloy material; the die casting process is set as follows: controlling the casting temperature to be 710 ℃, controlling the thickness of the material handle to be 25mm, and controlling the temperature of the die to be 170 ℃; the injection pressure is controlled to be 330kN, and the diameter of the hammer head is controlled to be 60 mm; the injection pressure is controlled to be 116MPa, the injection time is controlled to be 3S, the cooling time is controlled to be 2S, and the mold remaining time is controlled to be 10S; the die handle action stroke position in the die-casting process is as follows: the slow shot start position was controlled to 80mm, the fast shot start position was controlled to 270mm, the pressurizing position was controlled to 280mm, and the tracking position was controlled to 350 mm. Carrying out T6 heat treatment on the obtained blank, placing the obtained blank in a resistance furnace for primary solution treatment, wherein the solution treatment temperature is 420 +/-3 ℃, the heat preservation time is 3.5 hours, and then rapidly putting the blank into water with the temperature of 20 ℃ for cooling. Then placing the mixture into a resistance furnace for secondary solution treatment, wherein the temperature of the solution treatment is 460 +/-3 ℃, the heat preservation time is 2.5 hours, and then quickly placing the mixture into water with the temperature of 20 ℃ for cooling. Finally, the obtained material is placed at the temperature of 125 +/-3 ℃ for aging treatment, the aging time is 6 hours, and the ultimate tensile strength of the product obtained by air cooling is improved by 20.38 percent compared with that of a matrix.
Claims (1)
1. A die-casting method of graphene reinforced ADC12 aluminum alloy is characterized by comprising the following steps:
(1) performing ultrasonic pre-dispersion on carboxylated graphene in analytically pure ethanol for 1-3 hours at room temperature, and controlling the whole process to be free of water vapor; the volume ratio is controlled to be 0.2-0.4: 50;
(2) pouring the carboxylated graphene dispersion liquid pretreated in the step (1) into a precursor liquid composed of glycerol and tetraisopropyl titanate, sealing, and carrying out ultrasonic treatment again for 1-1.5 hours; wherein the volume ratio of the glycerol to the tetraisopropyl titanate is 10: 0.4-1.2;
(3) introducing the precursor suspension obtained in the step (2) into a hydrothermal reaction kettle, wherein the volume of the suspension accounts for 35-70% of the volume of the reaction kettle; heating the mixture in a reaction furnace, heating the mixture to 70-110 ℃ at a speed of 1-5 ℃/min, preserving heat for 1-2 hours, heating the mixture to 175-180 ℃ at a speed of 1-3 ℃/min, and preserving heat for 10-15 hours; taking out, sealing the reaction kettle and air cooling;
(4) taking out the solution obtained in the step (3), centrifuging, pouring analytically pure ethanol, centrifuging for multiple times until the solution is colorless, and controlling the rotating speed at 9000-16000 rpm; the whole process is sealed to ensure that no water vapor exists;
(5) drying the mixed powder obtained in the step (4) in vacuum, and then roasting at 450-500 ℃ under the protection of argon; the time is controlled to be 1-3 h; obtaining carboxylated graphene with a needle-shaped anatase titanium oxide coating on the surface;
(6) mixing the carboxylated graphene particles with the needle-shaped anatase titanium oxide coating on the surface obtained in the step (5) with pure aluminum powder at a mixing ratio of 1:4, maintaining the pressure of the mixed powder at 400MPa for 10min by cold pressure to prepare titanium oxide coated carboxylated graphene/aluminum precast blocks, and then cutting the precast blocks into pieces;
(7) placing ADC12 aluminum alloy into a graphite crucible, heating to 750 ℃ in a well-type resistance furnace, and preserving heat until the aluminum alloy is molten; after the ADC12 aluminum alloy block is completely melted, refining, degassing and deslagging the alloy melt; adding the titanium oxide coated carboxylated graphene/aluminum precast block obtained in the step (6) into an alloy melt, and controlling the content of titanium oxide coated graphene particles in the product to be 0.5-2.5 wt% according to the addition amount of the precast block;
(8) then inserting an ultrasonic amplitude transformer into the melt to perform high-energy ultrasonic treatment on the alloy melt, introducing argon for protection in the process, wherein the flow of the argon is 20L/min, and the pressure of the argon is 0.45MPa, and the process parameters comprise that the ultrasonic power is 1.5-2.5 kW, the ultrasonic frequency is 15000-25000 Hz, and the ultrasonic time is 10-20 min;
(9) preserving the temperature of the composite material slurry in the step (8) for 15min, skimming the obtained mixed melt after heat preservation is finished, sampling and analyzing the mixed melt after skimming, and reducing the temperature of the melt with qualified components to 680-710 ℃ for heat preservation for later use;
(10) pouring the slurry with qualified components obtained in the step (9) into a pouring gate of a die casting machine, and die-casting the slurry into a columnar aluminum alloy material; the die casting process is set as follows: controlling the casting temperature to be 680-710 ℃, controlling the thickness of the material handle to be 25mm, and controlling the temperature of the die to be 150-170 ℃; the injection pressure is controlled to be 330kN, and the diameter of the hammer head is controlled to be 60 mm; the injection pressure is controlled to be 116MPa, the injection time is controlled to be 3s, the cooling time is controlled to be 2s, and the mold remaining time is controlled to be 10 s; the die handle action stroke position in the die-casting process is as follows: the slow injection starting position is controlled to be 80mm, the fast injection starting position is controlled to be 270mm, the pressurizing position is controlled to be 280mm, and the tracking position is controlled to be 350 mm;
(11) placing the blank obtained in the step (10) in a resistance furnace for primary solution treatment, wherein the temperature of the solution treatment is 440 +/-3 ℃, the heat preservation time is 2.5-3.5 hours, and then quickly placing the blank in water at the temperature of 20 ℃ for cooling;
(12) putting the material obtained in the step (11) into a resistance furnace for secondary solution treatment, wherein the temperature of the solution treatment is 480 +/-3 ℃, the heat preservation time is 1.5-2.5 hours, and then quickly putting the material into water with the temperature of 20 ℃ for cooling;
(13) and (3) placing the material obtained in the step (12) at a temperature of 125 +/-3 ℃ for aging treatment, wherein the aging time is 5-6 hours, and then air cooling.
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