CN112080711A - Aluminum-based composite material forging and preparation method thereof - Google Patents
Aluminum-based composite material forging and preparation method thereof Download PDFInfo
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Abstract
The invention provides an aluminum-based composite material forging, which comprises the following components in percentage by mass: 0.1-5% of adamantane and TiB21-5% of ceramic fiber modified graphene oxide, 1-5% of Si, 0.5-2% of Cu, 0.2-0.5% of Ni, 0.1-0.5% of V, 0.2-0.4% of Fe0.01-0.1% of La0.03-0.07% of Pr0.03-0.07% of Al, and the balance of Al. The aluminum alloy composite material forging has good performanceThe mechanical property, the wear resistance and the high-temperature forging property of the alloy have wide application prospect.
Description
Technical Field
The invention relates to the technical field of aluminum alloy, in particular to an aluminum-based composite material forging and a preparation method thereof.
Background
The aluminum-based composite material mainly takes pure aluminum or aluminum alloy as a matrix, and achieves the purposes of improving the matrix structure of the alloy and improving the material performance by adding substances such as particles, fibers or whiskers and the like. The aluminum matrix composite has high specific strength, specific modulus, good electrical and thermal conductivity and high temperature performance, has been applied in the fields of aerospace, automobiles, microelectronics and the like, and draws more and more attention. The particle reinforced aluminum matrix composite has the advantages of high specific strength, high specific modulus, small thermal expansion coefficient, good high temperature resistance, good wear resistance and the like, and is widely applied to the fields of aerospace, transportation and the like as a lightweight structural material. In recent years, with the rapid development of domestic aerospace industry and automobile and electronic industry, the demand of particle reinforced aluminum matrix composite materials is increasing year by year. The main preparation processes of the particle reinforced aluminum matrix composite material include powder metallurgy, spray deposition, extrusion casting, stirring casting and the like. The composite material prepared by the powder metallurgy method has excellent performance, but the process flow is long, the working procedure is complex, the cost of metal powder is high, and the explosion is easily generated when the reinforcing phase is mixed with the powder; at the same time, the size of the article is also limited. The disadvantage of the extrusion casting process is that the precast block is easy to deform under the action of pressure, the microstructure of the prepared composite material is not uniform, the grain size is large, and the harmful interface reaction is difficult to control. The jet deposition preparation method has high cost and complicated equipment, and is not beneficial to realizing industrialization. The stirring casting method has the advantages of low cost, short process flow and easy realization of batch production. The semi-solid stirring casting is a preparation process of a particle reinforced aluminum matrix composite material which is widely applied at present, but the semi-solid stirring casting has the problems of uneven particle distribution, gas entrapment and the like. To solve this problem, vacuum stirring has been used. However, the vacuum stirring equipment has high cost and is difficult to produce in batch.
Disclosure of Invention
The invention aims to provide an aluminum-based composite material forging and a preparation method thereof, which have good mechanical property, wear resistance and high-temperature forging property and wide application prospect.
The technical scheme of the invention is realized as follows:
the invention provides an aluminum-based compositeThe material forging comprises the following components in percentage by mass: 0.1-5% of adamantane and TiB21-5% of ceramic fiber modified graphene oxide, 1-5% of Si, 0.5-2% of Cu, 0.2-0.5% of Ni, 0.1-0.5% of V, 0.2-0.4% of Fe0.01-0.1% of La0.03-0.07% of Pr0.03-0.07% of Al in balance;
the TiB2The ceramic fiber modified graphene oxide is prepared by the following method:
s1, preparing graphene oxide: weighing graphite flakes, dropwise adding concentrated sulfuric acid and mechanically stirring for 10-20min under an ice bath condition, simultaneously adding potassium permanganate in batches to enable the reaction temperature to be not higher than 5 ℃, reacting for 1-3H at normal temperature after the materials are added, heating to 30-40 ℃, reacting for 1-3H at constant temperature, then adding deionized water, controlling the temperature to be 90-100 ℃, cooling after keeping for 10-40min, finally adding deionized water for dilution, and dropwise adding 20-40 wt% of H2O2When the liquid turns from brown to yellow, standing for 5-10h, centrifugally washing with 5-10 wt% hydrochloric acid and proper deionized water until no sulfate ions exist, and collecting a sample for later use;
S2.TiB2preparing ceramic fibers: TiOCl2Dissolving in water, adding into boric acid-ethanol-water solution while stirring, adding glucose-citric acid water solution, mixing, adjusting pH to 2-5, stirring and reacting for 2-4h to obtain precursor solution; at room temperature, the precursor solution and the surfactant are mixed uniformly to obtain TiB2Electrostatic spinning of ceramic fiber to obtain TiB2Precursor of ceramic fiber, cracking the precursor fiber in a static furnace under argon atmosphere to obtain TiB2Ceramic fibers;
S3.TiB2preparing ceramic fiber modified graphene oxide: weighing graphene oxide, ultrasonically dispersing in water, adding a silane coupling agent, mixing and stirring uniformly, adjusting the pH to 3-5, reacting in a constant-temperature water bath for 2-5h, and adding TiB2Adding ceramic fiber into the system, stirring for 10-30min, heating to 50-70 deg.C, reacting for 30-50min to obtain TiB2Ceramic fiber modified graphene oxide.
As a further improvement of the invention, the components and the mass percent thereof are as follows: 0.5-3.5% of adamantane and TiB2Ceramic fiber2-4% of dimension-modified graphene oxide, 2-4% of Si, 1-1.5% of Cu, 0.3-0.4% of Ni0.2-0.4% of V, 0.25-0.35% of Fe0.05-0.07% of La0.04-0.06% of Pr0.04-0.06% of the balance of Al.
As a further improvement of the invention, the components and the mass percent thereof are as follows: 2.5% of adamantane and TiB23% of ceramic fiber modified graphene oxide, 3% of Si, 1.2% of Cu1, 0.35% of Ni0, 0.3% of V, 0.3% of Fe0.06%, 0.05% of La0, and the balance of Al.
As a further improvement of the invention, the judgment method of the sulfate ion-free is to add a small amount of water washing liquid into 1-2mol/L barium chloride solution, and if no precipitate is generated, the judgment method indicates that no sulfate ion is generated.
As a further improvement of the invention, the graphite flake, concentrated sulfuric acid, potassium permanganate and 20-40 wt% of H2O2The mass ratio of (A) to (B) is 10: (1-5): (0.2-1): (10-20); the mass percent of the concentrated sulfuric acid is more than 98%.
As a further improvement of the invention, the TiOCl2And the solid-to-liquid ratio of the boric acid-ethanol-water solution is 1: (3-5) g/mL, wherein the boric acid content in the boric acid-ethanol-water solution is 15-30 wt%, the ethanol content is 5-25 wt%, and the balance is water; the volume ratio of the glucose-citric acid aqueous solution to the boric acid-ethanol-aqueous solution is (3-5): 1; the content of glucose in the glucose-citric acid aqueous solution is 35-55 wt%, and the content of citric acid is 12-25 wt%; the mass ratio of the TiOCl2 to the surfactant is 10: (1-2); the cracking temperature is 300-400 ℃.
As a further improvement of the invention, the surfactant is selected from one or a mixture of more of disodium lauryl sulfosuccinate, disodium cocomonoethanolamide sulfosuccinate, monolauryl phosphate, potassium lauryl alcohol ether phosphate, cocomonoethanolamide, cocodiethanolamide, cocamidopropyl betaine and lauramidopropyl betaine; the silane coupling agent is selected from one or a mixture of KH550, KH560, KH570, KH580, KH602 and KH 792.
As a further improvement of the invention, the graphene oxide and TiB2The mass ratio of the ceramic fiber to the silane coupling agent is 10: (3-5): (0.1-0.5).
The invention further provides a preparation method of the aluminum-based composite material forging, which comprises the following steps:
s1, weighing simple substances of Si, Cu, Ni, V, Fe, La, Pr and Al raw materials in proportion, adding the simple substances into an induction furnace for heating, melting, refining and degassing, circularly flowing molten metal into a device through a leakage nozzle by adopting a supersonic gas atomization method, spraying supersonic gas to alloy liquid flow, cooling and solidifying to form fine powder to obtain aluminum alloy powder;
s2, mixing TiB2Putting the ceramic fiber modified graphene oxide into a stirring type ball mill, introducing liquid nitrogen or liquid argon for low-temperature ball milling, drying powder slurry after ball milling, and then putting the powder slurry into an aluminum sheath;
s3, mixing adamantane and aluminum alloy powder, adding an organic solvent which does not react with the raw materials, stirring and mixing for 60-90min by adopting an ultrasonic dispersion method, and carrying out vacuum drying on the mixed liquid for 12-15h at the drying temperature of 50-70 ℃ to obtain mixed powder;
s4, screening the mixed powder prepared in the step S3, mixing, primarily loading, compacting, loading into the aluminum sheath obtained in the step S2, degassing in vacuum, welding the sheath, heating the sheath, preserving heat, and extruding on a hydraulic press to obtain the aluminum-based composite material forging blank.
As a further improvement of the invention, the technological parameters of the ball milling are as follows: the ball milling rotation speed is 100-500r/min, the ball milling time is 2-5h, the ball material mass ratio is 1:5-50, the grinding ball material is steel or ceramic, and the diameter is 3-15 mm; the supersonic gas is provided by a supersonic nozzle vortex tube, the flow is 50-300m3/h, the pressure is 1-1.5 atmospheric pressures, and the temperature is 120-; the particle size of the screen is 100 meshes, the heating temperature of the sheath is 400-500 ℃, the heat preservation time is 1-2h, the extrusion ratio is 15-20, the extrusion speed is 0.5-1cm/min, and the extrusion cone angle is 90 degrees.
As a further improvement of the present invention.
The invention has the following beneficial effects: the aluminum-based composite material forging contains Cu and Ni, wherein the Cu and Ni play roles in oxidation resistance and high temperature resistance, and have higher strength and oxidation resistance at the high temperature of 750-; v, Si is contained in the material, so that the capability of resisting various chemical corrosion and stress corrosion can be improved, the friction loss of the material is reduced, and the wear resistance of the material is improved; the rare earth elements La and Pr are added into the alloy material, so that the effects of refining, desulfurizing, neutralizing low-melting-point harmful impurities can be achieved, the processing performance of the alloy can be improved, the physical and chemical properties of the alloy can be improved to a great extent, and the room-temperature and high-temperature mechanical properties of the alloy can be improved;
graphene (Graphene) is a two-dimensional material with a hexagonal structure formed by carbon atoms, and belongs to allotropes of carbon with graphite, carbon nanotubes and the like, so that the Graphene has excellent physical and chemical properties and mechanical properties, plays an important role in improving alloy tissues and alloy properties, and is an ideal reinforcement of an aluminum-based composite material, namely TB2The graphene reinforced by the ceramic material can obviously improve the mechanical property, high-temperature oxidation resistance and thermal shock resistance of the aluminum alloy composite material, and the ceramic fiber prepared by electrostatic spinning has a series of excellent characteristics, such as high specific surface area, high heat resistance, high insulativity and high modulus, wherein TB2The ceramic material keeps a better fiber state in the preparation process, Ti4+Hydroxyl in glucose, carboxyl in citric acid and hydroxyl in boric acid may react to form a cross-linking or coupling structure, which is favorable for combination between C and C after high-temperature cracking and also favorable for uniform distribution of Ti and B, and mutually and timely participate in carbothermic reduction reaction, when the cracking temperature is raised to about 300-400 ℃, glucose is decomposed into carbon which is combined to keep the state of fiber; when Ti is oxidized to form-Ti-O-Ti-, the precursor can still keep fibrous; with the start of carbothermic reduction reaction, Ti and B form a gap phase covalent bond TiB2Finally obtaining the TiB after pyrolysis2Ceramic fibers; the good fiber structure is coupled with graphene oxide to obtain a lamellar and fiber composite reinforced composite, the lamellar and fiber composite reinforced composite is added into the aluminum alloy, and because the elastic modulus of the matrix is small, the stress can be effectively transmitted to the reinforced composite with higher elastic modulus from the matrix through the interface, and the load is transferredAnd meanwhile, the reinforced composite body also bears partial load and restrains the deformation of the matrix, so that the material is reinforced, the mechanical property of the aluminum alloy is obviously improved, and the wear resistance of the aluminum alloy is improved to a certain extent.
Adamantane is a white acicular crystal of all carbon with a special microstructure, is added into aluminum alloy, and under the Orowan strengthening action, hard strengthening crystal particles are dispersed in a matrix to block dislocation movement, the spacing between the hard strengthening crystal particles is large enough, the particles are hard enough to resist the cutting action of dislocation, the dislocation movement is blocked, dislocation lines only can protrude from the strengthening particles and finally are connected together to continue moving, dislocation rings are left around the strengthening particles, and the dislocation lines moving next through the dislocation rings are blocked, so that the function of strengthening the matrix is achieved, the matrix is forged at a higher temperature, the plasticity of the material is better, and the deformation rate of pass is favorably improved. Meanwhile, the forging is specified at a higher speed, so that the heat released by plastic deformation can be increased, the temperature drop during free forging is compensated, and the temperature uniformity of the forged piece is controlled.
The aluminum alloy composite material forging piece has good mechanical property, wear resistance and high-temperature forging property, and has wide application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 shows TiB in preparation example 3 of the present invention2SEM images of ceramic fibers;
FIG. 2 is an SEM image of an aluminum-based composite forging blank in example 3 of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Preparation example TiB2Ceramic fiber modified graphene oxide
Preparation example 1
TiB2The ceramic fiber modified graphene oxide is prepared by the following method:
s1, preparing graphene oxide: weighing 10g of graphite flake, dropwise adding 1g of concentrated sulfuric acid under an ice bath condition, mechanically stirring for 10min, simultaneously adding 0.2g of potassium permanganate in batches to enable the reaction temperature to be not higher than 5 ℃, reacting at normal temperature for 1H after the material is added, heating to 30 ℃, reacting at constant temperature for 1H, then adding deionized water, controlling the temperature to be 90 ℃, keeping the temperature for 10min, cooling, finally adding deionized water for dilution, and dropwise adding 10g of 20 wt% H2O2When the liquid turns from brown to yellow, standing for 5h, centrifugally washing with 5 wt% hydrochloric acid and proper deionized water until no sulfate ions exist, and collecting a sample for later use;
the judgment method of no sulfate ion is that a small amount of water washing liquor is added into 1mol/L barium chloride solution, if no precipitate is generated, no sulfate ion is generated; the mass percent of the concentrated sulfuric acid is more than 98 percent;
S2.TiB2preparing ceramic fibers: 10g of TiOCl are taken2Dissolving in water, adding into 30mL boric acid-ethanol-water solution while stirring, adding 10g glucose-citric acid water solution, mixing well, adjusting pH to 2, stirring and reacting for 2h to obtain precursor solution; at room temperature, the precursor solution is uniformly mixed with 1g of monolauryl phosphate to obtain TiB2Electrostatic spinning of ceramic fiber to obtain TiB2Precursor of ceramic fiber, cracking the precursor fiber in a static furnace under argon atmosphere to obtain TiB2The cracking temperature of the ceramic fiber is 300 ℃;
the boric acid-ethanol-water solution contains 15 wt% of boric acid, 5 wt% of ethanol and the balance of water; the glucose content of the glucose-citric acid aqueous solution was 35 wt%, and the citric acid content was 12 wt%;
S3.TiB2preparing ceramic fiber modified graphene oxide: weighing 10g of graphene oxide, ultrasonically dispersing in water, adding 0.1g of silane coupling agent KH580, mixing and stirring uniformly, adjusting the pH to 3, reacting in a constant-temperature water bath for 2 hours, and adding 3g of TiB2Adding ceramic fiber into the system, stirring for 10min, heating to 50 deg.C, reacting for 30min to obtain TiB2Ceramic fiber modified graphene oxide.
Preparation example 2
TiB2The ceramic fiber modified graphene oxide is prepared by the following method:
s1, preparing graphene oxide: weighing 10g of graphite flake, dropwise adding 5g of concentrated sulfuric acid under an ice bath condition, mechanically stirring for 20min, simultaneously adding 1g of potassium permanganate in batches to enable the reaction temperature to be not higher than 5 ℃, reacting at normal temperature for 3H after the material is added, heating to 40 ℃, reacting at constant temperature for 3H, then adding deionized water, controlling the temperature to be 100 ℃, keeping the temperature for 40min, cooling, finally adding deionized water for dilution, and dropwise adding 20g of 40 wt% H2O2When the liquid turns from brown to yellow, standing for 10h, centrifugally washing with 10 wt% hydrochloric acid and proper deionized water until no sulfate ions exist, and collecting a sample for later use;
the judgment method of no sulfate ion is that a small amount of water washing liquor is added into 2mol/L barium chloride solution, if no precipitate is generated, no sulfate ion is generated; the mass percent of the concentrated sulfuric acid is more than 98 percent;
S2.TiB2preparing ceramic fibers: 10g of TiOCl are taken2Dissolving in water, adding into 50mL boric acid-ethanol-water solution while stirring, adding 10g glucose-citric acid water solution, mixing well, adjusting pH to 5, stirring and reacting for 4h to obtain precursor solution; at room temperature, the precursor solution is evenly mixed with 2g of monolauryl phosphate to obtain TiB2Electrostatic spinning of ceramic fiber to obtain TiB2Precursor of ceramic fiber, cracking the precursor fiber in a static furnace under argon atmosphere to obtain TiB2Ceramic fiber, the cracking temperature is 400 ℃;
the boric acid-ethanol-water solution contains 30 wt% of boric acid, 25 wt% of ethanol and the balance of water; the glucose-citric acid aqueous solution had a glucose content of 55 wt% and a citric acid content of 25 wt%;
S3.TiB2preparing ceramic fiber modified graphene oxide: weighing 10g of graphene oxide, ultrasonically dispersing in water, adding 0.5g of silane coupling agent KH560, mixing and stirring uniformly, adjusting the pH to 5, reacting in a constant-temperature water bath for 5 hours, and mixing 5g of TiB2Adding ceramic fiber into the system, stirring for 30min, heating to 70 deg.C, and reacting for 50min to obtain TiB2Ceramic fiber modified graphene oxide.
Preparation example 3
TiB2The ceramic fiber modified graphene oxide is prepared by the following method:
s1, preparing graphene oxide: weighing 10g of graphite flake, dropwise adding 3g of concentrated sulfuric acid under an ice bath condition, mechanically stirring for 15min, simultaneously adding 0.6g of potassium permanganate in batches to enable the reaction temperature to be not higher than 5 ℃, reacting at normal temperature for 2H after the material is completely added, heating to 35 ℃ for constant temperature reaction for 2H, then adding deionized water, controlling the temperature to be 95 ℃, keeping the temperature for 25min, cooling, finally adding deionized water for dilution, and dropwise adding 15g of 30 wt% H2O2After the liquid turns from brown to yellow, standing for 7 hours, centrifugally washing with 7 wt% hydrochloric acid and proper deionized water until no sulfate ions exist, and collecting a sample for later use;
the judgment method of no sulfate ion is that a small amount of water washing liquor is added into 1.5mol/L barium chloride solution, if no precipitate is generated, no sulfate ion is generated; the mass percent of the concentrated sulfuric acid is more than 98 percent;
S2.TiB2preparing ceramic fibers: 10g of TiOCl are taken2Dissolving in water, adding into 40mL boric acid-ethanol-water solution while stirring, adding 10g glucose-citric acid water solution, mixing well, adjusting pH to 3, stirring and reacting for 3h to obtain precursor solution; at room temperature, the precursor solution is evenly mixed with 1.5g of disodium lauryl sulfosuccinate to obtain TiB2Electrostatic spinning of ceramic fiber to obtain TiB2Precursor of ceramic fiber, precursor fiberCracking in a static furnace under argon atmosphere to obtain TiB2Ceramic fiber, the cracking temperature is 350 ℃; the SEM image of the fiber is shown in FIG. 1.
The boric acid-ethanol-water solution contains 22 wt% of boric acid, 15 wt% of ethanol and the balance of water; the content of glucose in the glucose-citric acid aqueous solution was 45 wt%, and the content of citric acid was 17 wt%;
S3.TiB2preparing ceramic fiber modified graphene oxide: weighing 10g of graphene oxide, ultrasonically dispersing in water, adding 0.35g of silane coupling agent KH560, mixing and stirring uniformly, adjusting the pH to 4, reacting in a constant-temperature water bath for 4 hours, and mixing 4g of TiB2Adding ceramic fiber into the system, stirring for 20min, heating to 60 deg.C, reacting for 30-50min to obtain TiB2Ceramic fiber modified graphene oxide.
Example 1
The composition comprises the following components in percentage by mass: adamantane 0.1% TiB prepared in example 121% of ceramic fiber modified graphene oxide, 1% of Si, 0.5% of Cu0.2%, 0.1% of Ni0.2%, 0.2% of V, 0.01% of Fe0.03% of La0%, and the balance of Al.
The method comprises the following steps:
s1, weighing simple substances of Si, Cu, Ni, V, Fe, La, Pr and Al raw materials in proportion, adding the simple substances into an induction furnace for heating, melting, refining and degassing, circularly flowing molten metal into a device through a leakage nozzle by adopting a supersonic gas atomization method, spraying supersonic gas to alloy liquid flow, cooling and solidifying to form fine powder to obtain aluminum alloy powder;
the supersonic gas is provided by a supersonic nozzle vortex tube with a flow rate of 50m3H, the pressure is 1 atmosphere, and the temperature is 120 ℃;
s2, mixing TiB2Putting the ceramic fiber modified graphene oxide into a stirring type ball mill, introducing liquid nitrogen or liquid argon for low-temperature ball milling, drying powder slurry after ball milling, and then putting the powder slurry into an aluminum sheath;
the technological parameters of ball milling are as follows: the ball milling speed is 100r/min, the ball milling time is 2 hours, the ball material mass ratio is 1:5, the material of the grinding ball is steel or ceramic, and the diameter is 3 mm;
s3, mixing adamantane and aluminum alloy powder, adding 100mL acetone, stirring and mixing for 60min by adopting an ultrasonic dispersion method, and carrying out vacuum drying on the mixed liquid for 12h at the drying temperature of 50 ℃ to obtain mixed powder;
s4, the mixed powder prepared in the step S3 is screened by a screen of 100 meshes, mixed, initially loaded, compacted, loaded into the aluminum sheath in the step S2, subjected to vacuum degassing, welded, sheathed, heated, insulated and extruded on a hydraulic press to obtain the aluminum-based composite material forging blank.
The heating temperature of the sheath is 400 ℃, the heat preservation time is 1h, the extrusion ratio is 15, the extrusion speed is 0.5cm/min, and the extrusion cone angle is 90 degrees.
Example 2
The composition comprises the following components in percentage by mass: adamantane 5% TiB prepared in example 225% of ceramic fiber modified graphene oxide, 5% of Si, 2% of Cu, 0.5% of Ni0.5%, 0.5% of V, 0.4% of Fe0.1%, 0.07% of La0%, and the balance of Al.
The method comprises the following steps:
s1, weighing simple substances of Si, Cu, Ni, V, Fe, La, Pr and Al raw materials in proportion, adding the simple substances into an induction furnace for heating, melting, refining and degassing, circularly flowing molten metal into a device through a leakage nozzle by adopting a supersonic gas atomization method, spraying supersonic gas to alloy liquid flow, cooling and solidifying to form fine powder to obtain aluminum alloy powder;
the supersonic gas is provided by a supersonic nozzle vortex tube with a flow rate of 300m3H, the pressure is 1.5 atmospheric pressure, and the temperature is 150 ℃;
s2, mixing TiB2Putting the ceramic fiber modified graphene oxide into a stirring type ball mill, introducing liquid nitrogen or liquid argon for low-temperature ball milling, drying powder slurry after ball milling, and then putting the powder slurry into an aluminum sheath;
the technological parameters of ball milling are as follows: the ball milling speed is 500r/min, the ball milling time is 5h, the ball material mass ratio is 1:50, the material of the grinding ball is steel or ceramic, and the diameter is 15 mm;
s3, mixing adamantane and aluminum alloy powder, adding 100mL acetonitrile, stirring and mixing for 90min by adopting an ultrasonic dispersion method, and carrying out vacuum drying on the mixed liquid for 15h at the drying temperature of 70 ℃ to obtain mixed powder;
s4, the mixed powder prepared in the step S3 is screened by a screen of 100 meshes, mixed, initially loaded, compacted, loaded into the aluminum sheath in the step S2, subjected to vacuum degassing, welded, sheathed, heated, insulated and extruded on a hydraulic press to obtain the aluminum-based composite material forging blank.
The heating temperature of the sheath is 500 ℃, the heat preservation time is 2h, the extrusion ratio is 20, the extrusion speed is 1cm/min, and the extrusion cone angle is 90 degrees.
Example 3
The composition comprises the following components in percentage by mass: adamantane 0.5% and TiB prepared in example 322% of ceramic fiber modified graphene oxide, 2% of Si, 1% of Cu, 0.3% of Ni0.2% of V, 0.25% of Fe0.05% of La0.04% of Pr0.04% of Al, and the balance of Al.
The method comprises the following steps:
s1, weighing simple substances of Si, Cu, Ni, V, Fe, La, Pr and Al raw materials in proportion, adding the simple substances into an induction furnace for heating, melting, refining and degassing, circularly flowing molten metal into a device through a leakage nozzle by adopting a supersonic gas atomization method, spraying supersonic gas to alloy liquid flow, cooling and solidifying to form fine powder to obtain aluminum alloy powder;
the supersonic gas is provided by a supersonic nozzle vortex tube with a flow rate of 150m3H, the pressure is 1.2 atmospheric pressure, and the temperature is 135 ℃;
s2, mixing TiB2Putting the ceramic fiber modified graphene oxide into a stirring type ball mill, introducing liquid nitrogen or liquid argon for low-temperature ball milling, drying powder slurry after ball milling, and then putting the powder slurry into an aluminum sheath;
the technological parameters of ball milling are as follows: the ball milling speed is 300r/min, the ball milling time is 3h, the ball material mass ratio is 1:25, the grinding ball material is steel or ceramic, and the diameter is 10 mm;
s3, mixing adamantane and aluminum alloy powder, adding 100mL tetrahydrofuran, stirring and mixing for 75min by adopting an ultrasonic dispersion method, and carrying out vacuum drying on the mixed liquid for 13h at the drying temperature of 60 ℃ to obtain mixed powder;
s4, the mixed powder prepared in the step S3 is screened by a 100-mesh screen, mixed, initially loaded and vibrated, loaded into the aluminum sheath in the step S2, subjected to vacuum degassing, welded, heated, sheathed and insulated, and extruded on a hydraulic press to obtain an aluminum-based composite material forging blank, wherein an SEM picture is shown in figure 2, and the aluminum alloy matrix can be subjected to non-uniform deformation by the reinforcement, so that the stress around the reinforcement is large, and stress concentration is formed.
The heating temperature of the sheath is 450 ℃, the heat preservation time is 1.5h, the extrusion ratio is 17, the extrusion speed is 0.75cm/min, and the extrusion cone angle is 90 degrees.
Example 4
The composition comprises the following components in percentage by mass: adamantane 3.5% and TiB prepared in example 324% of ceramic fiber modified graphene oxide, 4% of Si, 1.5% of Cu1, 0.4% of Ni0, 0.4% of V, 0.35% of Fe0.07%, 0.06% of La0, and the balance of Al.
The same preparation conditions as in example 3 were used.
Example 5
The composition comprises the following components in percentage by mass: 2.5% adamantane, TiB prepared in example 323% of ceramic fiber modified graphene oxide, 3% of Si, 1.2% of Cu1, 0.35% of Ni0, 0.3% of V, 0.3% of Fe0.06%, 0.05% of La0, and the balance of Al.
The same preparation conditions as in example 3 were used.
Comparative example 1
Compared with example 5, Ni was not added, and other conditions were the same.
The composition comprises the following components in percentage by mass: 2.5% adamantane, TiB prepared in example 323% of ceramic fiber modified graphene oxide, 3% of Si, 1.55% of Cu1, 0.3% of V, 0.3% of Fe0.3%, 0.06% of La0.05% of Pr0.05% of Al in balance.
Comparative example 2
Compared with example 5, Cu was not added, and other conditions were the same.
The composition comprises the following components in percentage by mass: 2.5% adamantane, TiB prepared in example 323% of ceramic fiber modified graphene oxide, 3% of Si, 1.55% of Ni1, 0.3% of V, 0.3% of Fe0.3%, 0.06% of La0.05% of Pr0.05%,The balance being Al.
Comparative example 3
In comparison with example 5, V was not added, and other conditions were the same.
The composition comprises the following components in percentage by mass: 2.5% adamantane, TiB prepared in example 323% of ceramic fiber modified graphene oxide, 3.3% of Si, 1.2% of Cu, 0.35% of Ni, 0.3% of Fe0.06%, Pr0.05% and the balance of Al.
Comparative example 4
In comparison with example 5, Si was not added, and other conditions were the same.
The composition comprises the following components in percentage by mass: 2.5% adamantane, TiB prepared in example 323% of ceramic fiber modified graphene oxide, 1.2% of Cu1, 0.35% of Ni0, 3.3% of V, 0.3% of Fe0, 0.06% of La0, 0.05% of Pr0, and the balance of Al.
Comparative example 5
In comparison with example 5, La was not added, and other conditions were the same.
The composition comprises the following components in percentage by mass: 2.5% adamantane, TiB prepared in example 323% of ceramic fiber modified graphene oxide, 3% of Si, 1.2% of Cu1, 0.35% of Ni0, 0.3% of V, 0.3% of Fe0.11%, Pr0.11% and the balance of Al.
Comparative example 6
In comparison with example 5, no Pr was added, and other conditions were the same.
The composition comprises the following components in percentage by mass: 2.5% adamantane, TiB prepared in example 323% of ceramic fiber modified graphene oxide, 3% of Si, 1.2% of Cu1, 0.35% of Ni0, 0.3% of V, 0.3% of Fe0.11% of La0, and the balance of Al.
Comparative example 7
In comparison with example 5, adamantane was not added, and other conditions were the same.
The composition comprises the following components in percentage by mass: example 3 preparation of TiB25.5% of ceramic fiber modified graphene oxide, 3% of Si, 1.2% of Cu1.35% of Ni0.35%, 0.3% of V, 0.3% of Fe0.06%, 0.06% of La0.05% of Pr0.05% of Al in balance.
Comparative example 8
In comparison with example 5, no addition of fruitTiB prepared in example 32And modifying the graphene oxide by the ceramic fiber under the same other conditions.
The composition comprises the following components in percentage by mass: 5.5% of adamantane, 3% of Si, 1.2% of Cu1, 0.35% of Ni0.3% of V, 0.3% of Fe0.3%, 0.06% of La0.05% of Pr0.05% and the balance of Al.
Test example 1
The aluminum-based composite material forgings prepared in the embodiments 1 to 5 and the comparative examples 1 to 8 of the invention and the aluminum-based composite material forgings sold in the market are subjected to tensile property test, normal temperature and high temperature tensile tests are carried out on an Instron5569 universal tensile testing machine, and the tensile rate is 0.2 mm/min. The tensile sample size meets the national standard of GBT228-2002 tensile sample. The results are shown in Table 1.
TABLE 1
| Group of | Tensile strength at 25 ℃ (MPa) | 300 ℃ tensile Strength (MPa) |
| Example 1 | 1752 | 1701 |
| Example 2 | 1765 | 1712 |
| Example 3 | 1744 | 1698 |
| Example 4 | 1772 | 1734 |
| Example 5 | 1785 | 1755 |
| Comparative example 1 | 1652 | 1234 |
| Comparative example 2 | 1575 | 1023 |
| Comparative example 3 | 1672 | 1523 |
| Comparative example 4 | 1702 | 1511 |
| Comparative example 5 | 1245 | 762 |
| Comparative example 6 | 1125 | 824 |
| Comparative example 7 | 925 | 623 |
| Comparative example 8 | 872 | 572 |
| Commercial aluminum matrix composite forging | 579 | 502 |
As can be seen from the table, the aluminum matrix composite material forged piece prepared by the embodiment of the invention has better normal-temperature and high-temperature mechanical properties.
Test example 2
The aluminum-based composite material forged pieces prepared in the embodiments 1-5 and the comparative examples 1-8 of the invention and the aluminum-based composite material forged pieces sold in the market are subjected to a friction resistance test, and a high-temperature friction test is carried out on an MMU-5G material end surface high-temperature friction abrasion tester. The test method of pin-disc type sliding friction and abrasion is adopted in the test. Alloy sample size d4mm X15 mm pin specimen, 43mm diameter GCr15 steel for the grinding disc. The friction test is carried out under the condition of dry friction, the sample alloy is respectively worn for 5min at 4 different temperatures of 25 ℃, 100 ℃, 200 ℃ and 300 ℃, and the load is all 100N. Before formal friction, each sample is pre-ground on 800-mesh sand paper for 5min to improve the fit degree of the wear surface of the sample with a friction wheel. The samples were ultrasonically cleaned with acetone before abrasion and blown dry before measurement with an analytical balance with an accuracy of 0.01 mg. And describing the wear resistance of the material to be tested by adopting the friction mass loss.
The results are shown in tables 2 and 3.
TABLE 2
TABLE 3
As can be seen from the table, the alloy material flange prepared by the embodiment of the invention has better friction resistance.
Test example 3
The aluminum-based composite material forgings prepared in examples 1 to 5 and comparative examples 1 to 8 of the invention and aluminum-based composite material forgings sold in the market are subjected to mechanical property tests, and the results are shown in table 4.
TABLE 4
| Group of | Modulus of elasticity (GPa) | Elongation (%) | Density (g/cm)3) |
| Example 1 | 154 | 6.92 | 2.4522 |
| Example 2 | 157 | 7.10 | 2.4135 |
| Example 3 | 152 | 7.02 | 2.4311 |
| Example 4 | 159 | 7.22 | 2.4573 |
| Example 5 | 162 | 7.25 | 2.4312 |
| Comparative example 1 | 135 | 6.32 | 2.6235 |
| Comparative example 2 | 142 | 6.75 | 2.5673 |
| Comparative example 3 | 125 | 5.72 | 2.5352 |
| Comparative example 4 | 137 | 5.93 | 2.4673 |
| Comparative example 5 | 102 | 5.24 | 2.5345 |
| Comparative example 6 | 98 | 5.02 | 2.4562 |
| Comparative example 7 | 87 | 4.98 | 2.5266 |
| Comparative example 8 | 79 | 4.22 | 2.5356 |
| Is commercially available | 85 | 3.54 | 2.6463 |
As can be seen from the table, the alloy material flange prepared by the embodiment of the invention has better mechanical property.
Compared with the example 5, the high temperature resistance of the comparative example 1 and the comparative example 2 is obviously reduced without adding Cu or Ni respectively, and the Cu and the Ni are added, wherein the Cu and the Ni play roles of oxidation resistance and high temperature resistance, and have higher strength and oxidation resistance at the high temperature of 750-1200 ℃, and the Cu and the Ni have synergistic effect.
Compared with the embodiment 5, the wear resistance of the comparative example 3 and the comparative example 4 is obviously reduced without adding V or Si respectively, the capability of resisting various chemical corrosion and stress corrosion can be improved by adding V and Si, the friction loss of the material is reduced, the wear resistance of the material is improved, and the V and the Si have synergistic effect.
Compared with the embodiment 5, the comparative example 5 and the comparative example 6 have the advantages that La or Pr is not added respectively, the mechanical property is obviously reduced, the rare earth elements La and Pr are added into the alloy material, the effects of refining, desulfurizing and neutralizing low-melting-point harmful impurities can be achieved, the processing property of the alloy can be improved, the physicochemical property of the alloy can be improved to a great extent, the room-temperature and high-temperature mechanical property of the alloy can be improved, and the La and Pr have the synergistic effect.
Comparative examples 7 and 8 compared to example 5, with no addition of adamantane or TiB, respectively2The mechanical property, the high-temperature tensile property, the room-temperature tensile property and the wear resistance of the ceramic fiber modified graphene oxide are all remarkably reduced, adamantane is a white needle-shaped crystal of all carbon with a special microstructure, the crystal is added into aluminum alloy, hard reinforced crystal particles are dispersed and distributed in a matrix through the Orowan reinforcing effect to block dislocation movement, the spacing of the hard reinforced crystal particles is large enough, when the particles are hard enough to resist the cutting effect of dislocation, the dislocation movement is blocked, dislocation lines only protrude from the reinforced particles and finally are connected together to continue to move, dislocation rings are left around the reinforced particles, and the dislocation lines moving next through the dislocation lines are blocked, so that the function of reinforcing the matrix is achieved, TB2The graphene reinforced by the ceramic material can obviously improve the mechanical property, the high-temperature oxidation resistance and the thermal shock resistance of the aluminum alloy composite material, and the ceramic fiber prepared by electrostatic spinning has a series of excellent characteristics, and the addition of the graphene and the ceramic fiber also has the synergistic effect.
Compared with the prior art, the aluminum-based composite material forging contains Cu and Ni, wherein the Cu and Ni play roles in oxidation resistance and high temperature resistance and have higher strength and oxidation resistance at the high temperature of 750-; v, Si is contained in the material, so that the capability of resisting various chemical corrosion and stress corrosion can be improved, the friction loss of the material is reduced, and the wear resistance of the material is improved; the rare earth elements La and Pr are added into the alloy material, so that the effects of refining, desulfurizing, neutralizing low-melting-point harmful impurities can be achieved, the processing performance of the alloy can be improved, the physical and chemical properties of the alloy can be improved to a great extent, and the room-temperature and high-temperature mechanical properties of the alloy can be improved;
graphene (Graphene) is a two-dimensional material with a hexagonal structure formed by carbon atoms, and belongs to allotropes of carbon with graphite, carbon nanotubes and the like, so that the Graphene has excellent physical and chemical properties and mechanical properties, plays an important role in improving alloy tissues and alloy properties, and is an ideal reinforcement of an aluminum-based composite material, namely TB2Ceramic material reinforced graphene, kongmingThe mechanical property, the high-temperature oxidation resistance and the thermal shock resistance of the aluminum alloy composite material are obviously improved, and the ceramic fiber prepared by electrostatic spinning has a series of excellent characteristics, such as high specific surface area, high heat resistance, high insulation and high modulus, wherein TB2The ceramic material keeps a better fiber state in the preparation process, Ti4+Hydroxyl in glucose, carboxyl in citric acid and hydroxyl in boric acid may react to form a cross-linking or coupling structure, which is favorable for combination between C and C after high-temperature cracking and also favorable for uniform distribution of Ti and B, and mutually and timely participate in carbothermic reduction reaction, when the cracking temperature is raised to about 300-400 ℃, glucose is decomposed into carbon which is combined to keep the state of fiber; when Ti is oxidized to form-Ti-O-Ti-, the precursor can still keep fibrous; with the start of carbothermic reduction reaction, Ti and B form a gap phase covalent bond TiB2Finally obtaining the TiB after pyrolysis2Ceramic fibers; the good fiber structure is coupled with graphene oxide to obtain a lamellar and fiber composite reinforced composite, the composite reinforced composite is added into aluminum alloy, and due to the fact that the elastic modulus of a matrix is small, stress can be effectively transmitted to the reinforced composite with high elastic modulus from the matrix through an interface, load is transferred, and the reinforced composite can bear partial load and restrain deformation of the matrix, so that the material is reinforced, the mechanical property of the aluminum alloy is obviously improved, and the wear resistance of the aluminum alloy is improved to a certain extent.
Adamantane is a white acicular crystal of all carbon with a special microstructure, is added into aluminum alloy, and under the Orowan strengthening action, hard strengthening crystal particles are dispersed in a matrix to block dislocation movement, the spacing between the hard strengthening crystal particles is large enough, the particles are hard enough to resist the cutting action of dislocation, the dislocation movement is blocked, dislocation lines only can protrude from the strengthening particles and finally are connected together to continue moving, dislocation rings are left around the strengthening particles, and the dislocation lines moving next through the dislocation rings are blocked, so that the function of strengthening the matrix is achieved, the matrix is forged at a higher temperature, the plasticity of the material is better, and the deformation rate of pass is favorably improved. Meanwhile, the forging is specified at a higher speed, so that the heat released by plastic deformation can be increased, the temperature drop during free forging is compensated, and the temperature uniformity of the forged piece is controlled.
The aluminum alloy composite material forging piece has good mechanical property, wear resistance and high-temperature forging property, and has wide application prospect.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The aluminum-based composite material forging is characterized by comprising the following components in percentage by mass: 0.1-5% of adamantane and TiB21-5% of ceramic fiber modified graphene oxide, 1-5% of Si, 0.5-2% of Cu, 0.2-0.5% of Ni, 0.1-0.5% of V, 0.2-0.4% of Fe0.01-0.1% of La0.03-0.07% of Pr0.03-0.07% of Al in balance;
the TiB2The ceramic fiber modified graphene oxide is prepared by the following method:
s1, preparing graphene oxide: weighing graphite flakes, dropwise adding concentrated sulfuric acid and mechanically stirring for 10-20min under an ice bath condition, simultaneously adding potassium permanganate in batches to enable the reaction temperature to be not higher than 5 ℃, reacting for 1-3H at normal temperature after the materials are added, heating to 30-40 ℃, reacting for 1-3H at constant temperature, then adding deionized water, controlling the temperature to be 90-100 ℃, cooling after keeping for 10-40min, finally adding deionized water for dilution, and dropwise adding 20-40 wt% of H2O2When the liquid turns from brown to yellow, standing for 5-10h, centrifugally washing with 5-10 wt% hydrochloric acid and proper deionized water until no sulfate ions exist, and collecting a sample for later use;
S2.TiB2preparing ceramic fibers: TiOCl2Dissolving in water, adding into boric acid-ethanol-water solution while stirring, adding glucose-citric acid water solution, mixing, adjusting pH to 2-5, stirring and reacting for 2-4h to obtain precursor solution; at room temperature, the precursor solution and the surfactant are mixed uniformly to obtain TiB2Ceramic fiber electrostatic spinning solution and electrostatic spinningFilamentizing to obtain TiB2Precursor of ceramic fiber, cracking the precursor fiber in a static furnace under argon atmosphere to obtain TiB2Ceramic fibers;
S3.TiB2preparing ceramic fiber modified graphene oxide: weighing graphene oxide, ultrasonically dispersing in water, adding a silane coupling agent, mixing and stirring uniformly, adjusting the pH to 3-5, reacting in a constant-temperature water bath for 2-5h, and adding TiB2Adding ceramic fiber into the system, stirring for 10-30min, heating to 50-70 deg.C, reacting for 30-50min to obtain TiB2Ceramic fiber modified graphene oxide.
2. The aluminum matrix composite forging of claim 1, wherein the aluminum matrix composite forging comprises the following components in percentage by mass: 0.5-3.5% of adamantane and TiB22-4% of ceramic fiber modified graphene oxide, 2-4% of Si, 1-1.5% of Cu, 0.3-0.4% of Ni0.2-0.4% of V, 0.25-0.35% of Fe0.05-0.07% of La0.04-0.06% of Pr0.04-0.06% of Al, and the balance of Al.
3. The aluminum matrix composite forging of claim 2, wherein the aluminum matrix composite forging comprises the following components in percentage by mass: 2.5% of adamantane and TiB23% of ceramic fiber modified graphene oxide, 3% of Si, 1.2% of Cu1, 0.35% of Ni0, 0.3% of V, 0.3% of Fe0.06%, 0.05% of La0, and the balance of Al.
4. The aluminum matrix composite forging as claimed in claim 1, wherein the judgment method of no sulfate ions is that a small amount of water washing liquid is added into 1-2mol/L barium chloride solution, and if no precipitate is generated, no sulfate ions are generated.
5. The aluminum matrix composite forging of claim 1, wherein the graphite flakes, concentrated sulfuric acid, potassium permanganate, 20-40 wt% H2O2The mass ratio of (A) to (B) is 10: (1-5): (0.2-1): (10-20); the mass percent of the concentrated sulfuric acid is more than 98%.
6. According to claim 1The aluminum-based composite material forging is characterized in that TiOCl2And the solid-to-liquid ratio of the boric acid-ethanol-water solution is 1: (3-5) g/mL, wherein the boric acid content in the boric acid-ethanol-water solution is 15-30 wt%, the ethanol content is 5-25 wt%, and the balance is water; the volume ratio of the glucose-citric acid aqueous solution to the boric acid-ethanol-aqueous solution is (3-5): 1; the content of glucose in the glucose-citric acid aqueous solution is 35-55 wt%, and the content of citric acid is 12-25 wt%; the mass ratio of the TiOCl2 to the surfactant is 10: (1-2); the cracking temperature is 300-400 ℃.
7. The aluminum matrix composite forging as set forth in claim 1, wherein the surfactant is selected from one or more of disodium lauryl sulfosuccinate, disodium cocomonoethanolamide sulfosuccinate, monolauryl phosphate, potassium lauryl alcohol ether phosphate, cocomonoethanolamide, cocodiethanolamide, cocamidopropyl betaine, and lauramidopropyl betaine; the silane coupling agent is selected from one or a mixture of KH550, KH560, KH570, KH580, KH602 and KH 792.
8. The aluminum-based composite forging of claim 1, wherein the graphene oxide, TiB2The mass ratio of the ceramic fiber to the silane coupling agent is 10: (3-5): (0.1-0.5).
9. A method of making an aluminium matrix composite forging as claimed in any one of claims 1 to 8, comprising the steps of:
s1, weighing simple substances of Si, Cu, Ni, V, Fe, La, Pr and Al raw materials in proportion, adding the simple substances into an induction furnace for heating, melting, refining and degassing, circularly flowing molten metal into a device through a leakage nozzle by adopting a supersonic gas atomization method, spraying supersonic gas to alloy liquid flow, cooling and solidifying to form fine powder to obtain aluminum alloy powder;
s2, mixing TiB2Ceramic fiber modified graphene oxide packingIntroducing liquid nitrogen or liquid argon into a stirring type ball mill for low-temperature ball milling, drying powder slurry subjected to ball milling, and then filling the powder slurry into an aluminum sheath;
s3, mixing adamantane and aluminum alloy powder, adding an organic solvent which does not react with the raw materials, stirring and mixing for 60-90min by adopting an ultrasonic dispersion method, and carrying out vacuum drying on the mixed liquid for 12-15h at the drying temperature of 50-70 ℃ to obtain mixed powder;
s4, screening the mixed powder prepared in the step S3, mixing, primarily loading, compacting, loading into the aluminum sheath obtained in the step S2, degassing in vacuum, welding the sheath, heating the sheath, preserving heat, and extruding on a hydraulic press to obtain the aluminum-based composite material forging blank.
10. The preparation method according to claim 9, wherein the ball milling process parameters are as follows: the ball milling rotation speed is 100-500r/min, the ball milling time is 2-5h, the ball material mass ratio is 1:5-50, the grinding ball material is steel or ceramic, and the diameter is 3-15 mm; the supersonic gas is provided by a supersonic nozzle vortex tube, the flow is 50-300m3/h, the pressure is 1-1.5 atmospheric pressures, and the temperature is 120-; the particle size of the screen is 100 meshes, the heating temperature of the sheath is 400-500 ℃, the heat preservation time is 1-2h, the extrusion ratio is 15-20, the extrusion speed is 0.5-1cm/min, and the extrusion cone angle is 90 degrees.
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