CN113667858B - Preparation method of spinel-coated nano-alumina reinforced aluminum-based composite material in situ - Google Patents
Preparation method of spinel-coated nano-alumina reinforced aluminum-based composite material in situ Download PDFInfo
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Abstract
The invention relates to a preparation method of a spinel-coated nano alumina reinforced aluminum-based composite material, which comprises the steps of firstly preparing spinel-coated nano alumina, then putting an aluminum alloy and the powder into a crucible for heating, heating to 800-850 ℃ at a certain speed, and preserving heat for 30-50 min; introducing ultrasonic vibration into the metal melt and maintaining; pouring the composite melt into a preheated mold to obtain an as-cast composite material; unidirectionally compressing 5-10% at a deformation rate of 0-5 mm/min in the same direction at 90 degrees per rotation, and circulating for 1-3 times; and (3) putting the composite material into a heat preservation furnace, heating the composite material to 250-500 ℃ at a heating rate of 15-20 ℃/min, preserving the heat for 1-3 h, and cooling by water to obtain the in-situ spinel-coated nano aluminum oxide reinforced aluminum matrix composite material. The invention has the characteristics of easy operation, safety, effectiveness, low cost, controllable quality and the like.
Description
Technical Field
The invention belongs to the field of metal material preparation, and particularly relates to a preparation method of a spinel-coated nano aluminum oxide reinforced aluminum matrix composite material.
Background
In recent years, particle reinforced aluminum matrix composites have attracted great attention and are widely applied to the fields of aerospace, rail transit, automobile manufacturing, electronic instruments and the like due to the characteristics of high specific strength, wear resistance, high temperature resistance, creep resistance and the like.
Ceramic particles, such as alumina, silicon carbide, magnesia, boron carbide, and the like, are widely used to reinforce aluminum alloy materials. Because these materials have the characteristics of high temperature resistance, high hardness, high compressive strength, wear resistance and the like, the materials are relatively suitable for being used as a reinforcement of a matrix material. The nano-scale reinforcement can obviously improve the comprehensive mechanical property of the matrix alloy while keeping the low content, thereby being widely concerned. However, due to their large surface-to-volume ratio and poor wettability, nanoceramic particles are very dispersible and exhibit poor interfacial bonding with the matrix, which directly affects the performance of the composite. It is therefore important to improve the wettability of the ceramic particles with the matrix.
The existing methods for improving the wettability of ceramic particles include an ultrasonic treatment method, surface metallization and the like. In the ultrasonic treatment method, the cavitation effect generated in the medium solution by ultrasonic vibration is used for removing the coated gas and pollutants on the surface of the ceramic particles, thereby improving the wettability of the ceramic particles and the metal solution. However, for powder metallurgy techniques or large volumes of metal solutions, ultrasonic vibrations are not effective or require higher power ultrasonic equipment. The metallization of the surface of the ceramic particle is commonly carried out by chemical plating, sol method, hydrothermal method and the like. Patent CN103464742A discloses a method for preparing copper-coated silver-coated tungsten composite coated powder, which is easy to generate chemical reaction to change the size of powder particles and even consume the powder particles in the process of coarsening the powder. Patents CN106367737A, CN106350753A, CN106350695A and CN106367630A disclose methods for coating elemental copper on the surface of carbon nanotubes, which are methods for obtaining elemental metal layers by chemical reaction of a solution in a hydrothermal reaction kettle. Due to invisibility, the quality of the coating is difficult to control and there are also safety issues.
In general, the composite material prepared by adding the nano ceramic material into the metal matrix needs to be subjected to subsequent processes of pressing, hot extrusion, hot rolling, forging and the like so as to improve the performance of the material. Although the surface coating or coating of the simple substance metal layer can improve the wettability of the ceramic particles and the metal solution, under the subsequent mechanical forming condition, the simple substance monolayer is easy to fall off from the surface of the body particles under the action of shearing force to form microcracks, which seriously weakens the mechanical property of the material.
Spinel (MgAl2O4) is a novel ceramic material, has the advantages of good mechanical property and thermal impedance, superior chemical inertness and the like, and is applied to the fields of metallurgy, electronics, chemical industry and the like. It is worth noting that the degree of mismatch between MgAl2O4 and Al in the (100) crystal plane is only 0.25%, which means that there is good interfacial bonding between the two, and effective heterogeneous nucleation points can be provided for Al crystals, which has positive effects on refining crystal grains and improving mechanical properties of materials. Thus being a suitable aluminum alloy reinforcement. However, the spinel is generally in a whisker shape or a regular block shape, so that there is a certain limitation on improving the mechanical property of the metal alloy, and there is a certain difficulty in controlling how the spinel is uniformly coated on the surface of the nano ceramic particles and in atomic scale bonding.
On the other hand, the dispersibility of the ceramic particles in the matrix is a key factor affecting the properties of the alloy. The control of the particle dispersion is embodied in the metal material preparation process. Currently, the dispersion problem of the reinforcement is solved by using stirring casting methods (mechanical stirring, ultrasonic dispersion, electromagnetic stirring, etc.), in-situ synthesis, powder metallurgy, and the like. However, interfacial bonding of particles to the substrate, casting defects, and densification of the powdered metallurgy itself remain to be addressed.
In the publication No. CN106367630A, in a preparation method of a multi-walled carbon nanotube reinforced aluminum matrix composite coated with elemental copper, the problems of carbon nanotube dispersion and material compactness are solved through ball milling dispersion, solid heating and die forging forming, but the uniform distribution of carbon nanotubes on a micro scale has great potential. In the publication No. CN103614672A, a method for preparing a carbon nanotube reinforced aluminum matrix composite, conventional means such as ball milling, cold pressing, sintering, extruding, etc. are used to prepare the carbon nanotube reinforced aluminum matrix composite, however, the interface bonding, compactness, etc. are not well solved. It is worth noting that while the problems of reinforcement dispersion, interface bonding, compactness and the like are solved, the composite material still has the characteristics of high strength, low plasticity and the like.
Therefore, in summary, an effective method for preparing the aluminum matrix composite material is still lacking. In view of this, the present application is specifically made.
Disclosure of Invention
The invention aims to provide a preparation method of a nano-alumina reinforced aluminum-based composite material with spinel coated in situ, and solves the problem that an effective preparation method of an aluminum-based composite material is still lacked at present.
The embodiment of the invention is realized by the following steps:
a preparation method of a nano-alumina reinforced aluminum-based composite material with spinel coated in situ comprises the following steps:
step S1: uniformly dispersing nano aluminum oxide in trisodium citrate solution;
step S2: adding stannous chloride into 0.4-0.8 mol/L hydrochloric acid, continuously adding sodium chloride after the stannous chloride is completely dissolved, then adding the nano-alumina suspension obtained in the step S1, wherein the molar ratio of the nano-alumina to the stannous chloride to the sodium chloride is 1:1: 4-1: 1:6, and simultaneously applying magnetic force to stir for 30-50 min;
step S3: adding palladium chloride into 0.7-1.0 mol/L hydrochloric acid, mixing with the mixed suspension obtained in the step S2, magnetically stirring for 10-20 min, standing, and removing the upper-layer mixed solution after powder is precipitated to obtain powder;
step S4: cleaning and centrifuging the powder obtained in the step S3 in distilled water, and repeating for 3-5 times;
step S5: under the stirring action, adding 1-5 mol/L potassium sodium tartrate solution into 2-6 mol/L magnesium sulfate solution, adding 0.5-1.0 vol.% of methanol, and adjusting the pH value of the solution to 9-10 by using 0.01-0.03 mol/L sodium hydroxide solution;
step S6: adding the solution obtained in the step S5 into the powder obtained in the step S4, ultrasonically vibrating for 30-60 min, simultaneously dripping formaldehyde, and controlling the pH of the solution to be 11-12 by using sodium hydroxide particles;
step S7: washing with distilled water, and centrifuging the solution obtained in the step S6 to obtain simple substance magnesium-coated nano alumina particles;
step S8: drying the powder obtained in the step S7 in a vacuum drying furnace, and then preserving heat for 1-2 hours at 780-850 ℃ in an air environment to obtain nano-alumina surface in-situ coated spinel;
step S9: putting the powder obtained in the step S8 and aluminum alloy into a crucible for heating, heating to 800-850 ℃ at the speed of 10-20 ℃/min, and preserving heat for 30-50 min;
step S10: introducing ultrasonic vibration of 1-2 kW and 20kHz into the metal melt obtained in the step S9, and performing intermittent ultrasonic for 10-15 min by taking 2-8S as a gap time;
step S11: pouring the composite melt obtained in the step S10 into a mold at 350-450 ℃ to obtain an as-cast composite material;
step S12: compressing and deforming the cast blank obtained in the step S11, unidirectionally compressing 5-10% at a deformation rate of 0-5 mm/min along the same direction at 90 degrees per rotation, and circulating for 1-3 times;
step S13: and (4) putting the deformation body obtained in the step (S12) into a heat preservation furnace, heating to 250-500 ℃ at a heating rate of 15-20 ℃/min, preserving heat for 1-3 h, and then cooling with water to obtain the in-situ spinel-coated nano aluminum oxide reinforced aluminum-based composite material.
Further, the size of the nano alumina particles in the step S1 is 80-200 nm.
Further, the nano-alumina in the step S1 is subjected to heat preservation for 1-2 hours at the temperature of 600-700 ℃.
Further, in the step S1, the nano aluminum oxide is dispersed in the trisodium citrate solution under the ultrasonic action of 150-400W and 40kHz, wherein the molar ratio of the trisodium citrate to the nano aluminum oxide is 0.001-0.003, and the ultrasonic dispersion is carried out for 40-60 min.
In step S3, the concentration of palladium chloride in the hydrochloric acid solution is 0.02-0.04 mol/L, and the molar ratio of palladium chloride to nano-alumina is 0.01-0.06.
Further, in the step S4, the centrifugation is performed for 5-10 min at a speed of 2000-2500 r/min.
Further, in the step S5, the molar ratio of the sodium potassium tartrate to the magnesium sulfate is 2:1 to 9: 1.
Further, the molar ratio of the magnesium sulfate to the powder in the step S6 is 0.1 to 0.3, and the addition amount of formaldehyde is 8 to 10 times the mole number of the magnesium ions.
Further, a riser is provided at the top end of the mold cavity in step S11.
The embodiment of the invention has the beneficial effects that:
(1) the proportioning of the amount is easy, and the reaction time is short;
(2) the method adopts conventional simple equipment, is convenient to operate, has low reaction temperature, and is safe and reliable;
(3) the method is simple to operate, has high coating rate and can realize batch production;
(4) the coating and the nano ceramic particles can be combined at an atomic level without considering the problem of oxidation of the coating;
(5) the structure characteristics of the grain boundary are controllable;
(6) the method can realize the synergistic improvement of strength and plasticity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a microstructure diagram of in-situ coated spinel on the surface of nano-alumina prepared in example 3;
FIG. 2 is an EDS analysis spectrum of the nano alumina surface in-situ coated spinel prepared in example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. 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.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
The terms "first," "second," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1.
Keeping the temperature of 80nm of aluminum oxide at 600 ℃ for 1h, and dispersing the aluminum oxide in trisodium citrate solution under the ultrasonic action of 150W and 40kHz, wherein the molar ratio of trisodium citrate to nano aluminum oxide is 0.001, and performing ultrasonic dispersion for 40 min; adding stannous chloride into 0.4mol/L hydrochloric acid, continuously adding sodium chloride after the stannous chloride is completely dissolved, then adding the obtained nano-alumina suspension, wherein the molar ratio of the nano-alumina to the stannous chloride to the sodium chloride is 1:1:4, and simultaneously applying magnetic force to stir for 30 min; adding palladium chloride into 0.7mol/L hydrochloric acid, mixing with the mixed suspension obtained in the previous step, wherein the concentration of the palladium chloride in the hydrochloric acid solution is 0.02mol/L, the molar ratio of the palladium chloride to the nano-alumina is 0.01, magnetically stirring for 10min, standing, and removing the upper mixed solution after powder precipitation to obtain powder; washing the obtained powder in distilled water, centrifuging at 2000r/min for 5min, and repeating for 3 times; adding 3.6mol/L potassium sodium tartrate solution into 5mol/L magnesium sulfate solution under the stirring action, adding 0.5 vol.% of methanol, and adjusting the pH value of the solution to 9 by using 0.017mol/L sodium hydroxide solution, wherein the molar ratio of potassium sodium tartrate to magnesium sulfate is 2: 1; adding the obtained solution into the cleaned powder, performing ultrasonic vibration for 30min, and simultaneously dripping formaldehyde, wherein the molar ratio of magnesium sulfate to the powder is 0.1, the addition amount of the formaldehyde is 8 times of the mole number of magnesium ions, and the pH of the solution is controlled to be 11 by using sodium hydroxide particles; washing the obtained solution by distilled water, and centrifuging to obtain simple substance magnesium coated nano alumina particles; drying the obtained powder in a vacuum drying furnace, and then preserving heat for 1h at 780 ℃ in an air environment to obtain nano-alumina surface in-situ coated spinel; 2 wt.% of 2024 aluminum alloy is added into the obtained spinel-in-situ coated nano alumina powder, the nano alumina powder and the 2024 aluminum alloy are put into a crucible to be heated, the temperature is increased to 800 ℃ at the speed of 10 ℃/min, and the temperature is kept for 30 min; introducing ultrasonic vibration of 1kW and 20kHz into the metal melt, and intermittently performing ultrasonic treatment for 10min by taking 2s as gap time; pouring the obtained composite melt into a die at 350 ℃ to obtain an as-cast composite material; compressing and deforming the obtained as-cast blank, performing unidirectional compression on the blank by 5 percent at a deformation rate of 1mm/min along the same direction and at 90 degrees per rotation, and circulating for 1 time; and putting the obtained deformation body into a heat preservation furnace, heating to 250 ℃ at a heating rate of 15 ℃/min, preserving heat for 2h, and then cooling by water to obtain the nano aluminum oxide reinforced aluminum matrix composite material coated with the spinel in situ.
Example 2
Keeping the temperature of 100nm of aluminum oxide at 700 ℃ for 1h, and dispersing the aluminum oxide in trisodium citrate solution under the ultrasonic action of 200W and 40kHz, wherein the molar ratio of trisodium citrate to nano aluminum oxide is 0.002, and performing ultrasonic dispersion for 50 min; adding stannous chloride into 0.5mol/L hydrochloric acid, continuously adding sodium chloride after the stannous chloride is completely dissolved, then adding the obtained nano-alumina suspension, wherein the molar ratio of the nano-alumina to the stannous chloride to the sodium chloride is 1:1:5, and simultaneously applying magnetic force to stir for 30 min; adding palladium chloride into 0.7mol/L hydrochloric acid, mixing with the mixed suspension obtained in the previous step, wherein the concentration of the palladium chloride in the hydrochloric acid solution is 0.03mol/L, the molar ratio of the palladium chloride to the nano-alumina is 0.02, magnetically stirring for 10min, standing, and removing the upper mixed solution after powder precipitation to obtain powder; washing the obtained powder in distilled water, centrifuging at 2500r/min for 5min, and repeating for 4 times; adding 3mol/L potassium sodium tartrate solution into 4.5mol/L magnesium sulfate solution under the stirring action, adding 0.5 vol.% of methanol, and adjusting the pH value of the solution to 9 by using 0.01mol/L sodium hydroxide solution, wherein the molar ratio of potassium sodium tartrate to magnesium sulfate is 2: 1; adding the obtained solution into the cleaned powder, performing ultrasonic vibration for 30min, and simultaneously dripping formaldehyde, wherein the molar ratio of magnesium sulfate to the powder is 0.2, the addition amount of the formaldehyde is 9 times of the mole number of magnesium ions, and the pH of the solution is controlled to be 11 by using sodium hydroxide particles; washing the obtained solution by distilled water, and centrifuging to obtain simple substance magnesium coated nano alumina particles; drying the obtained powder in a vacuum drying furnace, and then preserving heat for 1h at 800 ℃ in an air environment to obtain nano-alumina surface in-situ coated spinel; adding the nano aluminum oxide powder coated with the spinel in situ, wherein the adding amount is 3 wt.% of that of 5083 aluminum alloy, putting the nano aluminum oxide powder and 5083 aluminum alloy into a crucible for heating, heating to 850 ℃ at the speed of 15 ℃/min, and preserving heat for 40 min; introducing ultrasonic vibration of 2kW and 20kHz into the obtained metal melt, and intermittently performing ultrasonic treatment for 10min by taking 4s as gap time; pouring the obtained composite melt into a die at 350 ℃ to obtain an as-cast composite material; compressing and deforming the obtained as-cast blank, performing unidirectional compression on the blank by 10 percent at a deformation rate of 2mm/min along the same direction and at 90 degrees per rotation, and circulating for 1 time; and putting the obtained deformation body into a heat preservation furnace, heating to 480 ℃ at a heating rate of 20 ℃/min, preserving heat for 1h, and then cooling by water to obtain the nano aluminum oxide reinforced aluminum matrix composite material coated with the spinel in situ.
Example 3
Keeping the temperature of 100nm of aluminum oxide at 700 ℃ for 1h, dispersing the aluminum oxide in trisodium citrate solution under the ultrasonic action of 250W and 40kHz, wherein the molar ratio of trisodium citrate to nano aluminum oxide is 0.003, and performing ultrasonic dispersion for 60 min; adding stannous chloride into 0.7mol/L hydrochloric acid, continuously adding sodium chloride after the stannous chloride is completely dissolved, then adding the obtained nano-alumina suspension, wherein the molar ratio of the nano-alumina to the stannous chloride to the sodium chloride is 1:1:6, and simultaneously applying magnetic force to stir for 50 min; adding palladium chloride into 0.8mol/L hydrochloric acid, mixing with the mixed suspension obtained in the previous step, wherein the concentration of the palladium chloride in the hydrochloric acid solution is 0.03mol/L, the molar ratio of the palladium chloride to the nano-alumina is 0.02, magnetically stirring for 20min, standing, and removing the upper mixed solution after powder precipitation to obtain powder; washing the obtained powder in distilled water, centrifuging at 2100r/min for 5min, and repeating for 5 times; adding 3.6mol/L potassium sodium tartrate solution into 5mol/L magnesium sulfate solution under the stirring action, adding 0.5 vol.% of methanol, and adjusting the pH value of the solution to 10 by using 0.017mol/L sodium hydroxide solution, wherein the molar ratio of potassium sodium tartrate to magnesium sulfate is 9: 1; adding the obtained solution into the cleaned powder, performing ultrasonic vibration for 30min, and simultaneously dripping formaldehyde, wherein the molar ratio of magnesium sulfate to the powder is 0.1, the addition amount of the formaldehyde is 10 times of the mole number of magnesium ions, and the pH of the solution is controlled to be 12 by using sodium hydroxide particles; washing the obtained solution by distilled water, and centrifuging to obtain simple substance magnesium coated nano alumina particles; drying the obtained powder in a vacuum drying furnace, and then preserving heat for 1h at 800 ℃ in an air environment to obtain nano-alumina surface in-situ coated spinel; adding the nano aluminum oxide powder coated with the spinel in situ, wherein the adding amount is 5 wt.% of 7075 aluminum alloy, putting the nano aluminum oxide powder and 7075 aluminum alloy into a crucible for heating, heating to 850 ℃ at the speed of 20 ℃/min, and preserving heat for 50 min; introducing ultrasonic vibration of 2kW and 20kHz into the obtained metal melt, and performing intermittent ultrasonic treatment for 10min by taking 2s as gap time; pouring the obtained composite melt into a mold at 450 ℃ to obtain an as-cast composite material; compressing and deforming the obtained as-cast blank, performing unidirectional compression on the blank by 10 percent at a deformation rate of 1mm/min along the same direction and at 90 degrees per rotation, and circulating for 2 times; and putting the obtained deformation body into a heat preservation furnace, heating to 500 ℃ at a heating rate of 15 ℃/min, preserving heat for 2h, and then cooling by water to obtain the nano aluminum oxide reinforced aluminum matrix composite material coated with spinel in situ.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of a spinel-coated nano aluminum oxide reinforced aluminum-based composite material in situ is characterized by comprising the following steps:
step S1: uniformly dispersing nano aluminum oxide in trisodium citrate solution;
step S2: adding stannous chloride into 0.4-0.8 mol/L hydrochloric acid, continuously adding sodium chloride after the stannous chloride is completely dissolved, then adding the nano-alumina suspension obtained in the step S1, wherein the molar ratio of the nano-alumina to the stannous chloride to the sodium chloride is 1:1: 4-1: 1:6, and simultaneously applying magnetic force to stir for 30-50 min;
step S3: adding palladium chloride into 0.7-1.0 mol/L hydrochloric acid, mixing with the mixed suspension obtained in the step S2, magnetically stirring for 10-20 min, standing, and removing the upper-layer mixed solution after powder is precipitated to obtain powder;
step S4: cleaning and centrifuging the powder obtained in the step S3 in distilled water, and repeating for 3-5 times;
step S5: under the stirring action, adding 1-5 mol/L potassium sodium tartrate solution into 2-6 mol/L magnesium sulfate solution, adding 0.5-1.0 vol.% of methanol, and adjusting the p H value of the solution to 9-10 by using 0.01-0.03 mol/L sodium hydroxide solution;
step S6: adding the solution obtained in the step S5 into the powder obtained in the step S4, ultrasonically vibrating for 30-60 min, simultaneously dripping formaldehyde, and controlling p H of the solution to be 11-12 by using sodium hydroxide particles;
step S7: washing with distilled water, and centrifuging the solution obtained in the step S6 to obtain simple substance magnesium-coated nano alumina particles;
step S8: drying the powder obtained in the step S7 in a vacuum drying furnace, and then preserving heat for 1-2 hours at 780-850 ℃ in an air environment to obtain nano-alumina surface in-situ coated spinel;
step S9: putting the powder obtained in the step S8 and aluminum alloy into a crucible for heating, heating to 800-850 ℃ at the speed of 10-20 ℃/min, and preserving heat for 30-50 min;
step S10: introducing ultrasonic vibration of 1-2 kW and 20kHz into the metal melt obtained in the step S9, and performing intermittent ultrasonic for 10-15 min by taking 2-8S as a gap time;
step S11: pouring the composite melt obtained in the step S10 into a mold at 350-450 ℃ to obtain an as-cast composite material;
step S12: compressing and deforming the cast blank obtained in the step S11, unidirectionally compressing 5-10% at a deformation rate of 0-5 mm/min along the same direction at 90 degrees per rotation, and circulating for 1-3 times;
step S13: and (4) putting the deformation body obtained in the step (S12) into a heat preservation furnace, heating to 250-500 ℃ at a heating rate of 15-20 ℃/min, preserving heat for 1-3 h, and then cooling with water to obtain the nano aluminum oxide reinforced aluminum-based composite material coated with the spinel in situ.
2. The method for preparing the spinel-coated nano aluminum oxide reinforced aluminum-based composite material in situ according to claim 1, wherein the method comprises the following steps: the size of the nano alumina particles in the step S1 is 80-200 nm.
3. The method of claim 1, wherein: and (3) insulating the nano alumina in the step S1 for 1-2 hours at 600-700 ℃.
4. The method for preparing the spinel-coated nano aluminum oxide reinforced aluminum-based composite material in situ according to claim 1, wherein the method comprises the following steps: and in the step S1, dispersing the nano aluminum oxide in a trisodium citrate solution under the ultrasonic action of 150-400W and 40kHz, wherein the molar ratio of the trisodium citrate to the nano aluminum oxide is 0.001-0.003, and performing ultrasonic dispersion for 40-60 min.
5. The method for preparing the spinel-coated nano aluminum oxide reinforced aluminum-based composite material in situ according to claim 1, wherein the method comprises the following steps: in the step S3, the concentration of the palladium chloride in the hydrochloric acid solution is 0.02-0.04 mol/L, and the molar ratio of the palladium chloride to the nano-alumina is 0.01-0.06.
6. The method for preparing the spinel-coated nano aluminum oxide reinforced aluminum-based composite material in situ according to claim 1, wherein the method comprises the following steps: and centrifuging at a speed of 2000-2500 r/min for 5-10 min in the step S4.
7. The method for preparing the spinel-coated nano aluminum oxide reinforced aluminum-based composite material in situ according to claim 1, wherein the method comprises the following steps: the molar ratio of the potassium sodium tartrate to the magnesium sulfate in the step S5 is 2: 1-9: 1.
8. The method for preparing the spinel-coated nano aluminum oxide reinforced aluminum-based composite material in situ according to claim 1, wherein the method comprises the following steps: the molar ratio of the magnesium sulfate to the powder in the step S6 is 0.1-0.3, and the addition amount of the formaldehyde is 8-10 times of the mole number of the magnesium ions.
9. The method for preparing the spinel-coated nano aluminum oxide reinforced aluminum-based composite material in situ according to claim 1, wherein the method comprises the following steps: and a riser is arranged at the top end of the die cavity in the step S11.
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