CN109385551B - Preparation method of titanium oxide/graphene oxide coated enhanced aluminum-magnesium-containing base material - Google Patents
Preparation method of titanium oxide/graphene oxide coated enhanced aluminum-magnesium-containing base material Download PDFInfo
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- 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
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- 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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
Abstract
A preparation method of a titanium oxide/graphene oxide coated reinforced aluminum-magnesium-containing base material comprises the steps of utilizing hydrothermal high pressure in an anhydrous environment, adsorbing Ti ions under the action of functional groups of graphene oxide, and roasting at a later stage to obtain anatase type GO @ TiO 2. The obtained powder and magnesium powder are mixed, ultrasonically treated and ball-milled. And carrying out cold pressing and hot extrusion on the mixed material to obtain an intermediate phase, then introducing the intermediate phase into the melt in an ultrasonic environment, and carrying out ultrasonic treatment on the melt with the temperature controlled near a liquidus line. And introducing the obtained composite melt into a preheated precoated sand mold, and then carrying out ultrasonic treatment until the composite melt is solidified. And then carrying out channel-changing shaping hot extrusion on the obtained blank to obtain a rod-shaped blank, and then carrying out equal-radius-angle multiple extrusion to obtain the titanium oxide/graphene oxide coated reinforced aluminum-magnesium-containing composite material. The preparation technology of the aluminum matrix composite material treated by the invention is simple, safe and low in cost. The obtained Mg17Al12 phase and crystal grains are fine, the graphene oxide is well distributed in multiple extrusion dispersion, and meanwhile, the GO in the coating layer is better combined with the matrix due to the improved wettability of the GO.
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.
The magnesium-based material, especially magnesium-aluminum alloy, has the advantages of small density, light weight, high strength, strong shock absorption performance and the like, and is widely applied to the transportation industry of aviation, automobiles and the like. The alloy is a typical eutectic alloy, has better casting performance, and has the advantages of high specific strength, low price and the like. Typically, Mg in the alloy17Al12The alloy is easy to present a floating island shape or a thick block shape, which is easy to crack the matrix in the stress process and seriously affects the mechanical property of the matrix, so the refinement of the phase is one of the important research points of magnesium-aluminum alloy. On the other hand, the research of enhancing the strength and other mechanical properties of metal-based materials by using carbon materials such as carbon nanotubes or graphene is currently on the spot and has achieved a great deal of researchProgression to a certain extent. However, the application defect of Graphene Oxide (GO) in metal is also obvious. Graphene oxide exhibits very poor wettability, which directly results in poor bonding with metal interfaces, and is not favorable for preparation of composite materials. Thus, improving its wettability with the substrate and choosing the right process method become the key to using graphene to enhance the wear of aluminum-based materials.
The existing method for improving the wettability of graphene comprises surface coating and the like, such as chemical nickel plating, and mainly comprises the steps of sensitizing and activating carboxylated graphene, then putting the activated carboxylated graphene into chemical plating solution for plating, and obtaining a granular coating on the surface of the carboxylated graphene along with the reaction.
Control of the carbon material dispersion is typically present in the metal preparation process. At present, the carbon material aluminum matrix composite material is prepared by an in-situ synthesis method and a powder metallurgy method commonly. However, the drawbacks of these methods are also obvious, and powder metallurgy is the hot research direction, but the problems of interfacial bonding and compactness are not effectively solved. The in-situ synthesis method has short plates such as excessively complex process and difficult process control. The problem of dispersion by the stirring method is not effectively solved.
In a preparation method of a graphene reinforced aluminum matrix composite material, which is disclosed as 108060321a, a semi-solid casting and extrusion method is adopted to promote dispersion of graphene, and the graphene reinforced aluminum matrix composite material is prepared. However, the method cannot effectively improve the wettability problem of graphene, and the graphene is easily agglomerated again in the solidification process, so that the quality cannot be kept in good consistency.
In the preparation method of the magnesium-based graphene composite material named as 107058786a, a method of mesophase briquetting and ultrasonic fusion casting is adopted to prepare the graphene magnesium-based material, but the method does not solve the problems of wettability of graphene and re-agglomeration of graphene in the casting process. At the same time, Mg is not involved17Al12The thinning of the film and the like.
In the patent publication No. 106702193a entitled "method for preparing graphene/aluminum composite material", conventional powder metallurgy methods such as mixing, drying, ball milling, cold pressing, sintering and extruding are used to prepare the graphene reinforced aluminum-based composite material, although the wettability is improved, the material does not involve melting, and the problems of compactness and the like are still outstanding.
Therefore, in summary, an economical and effective graphene-reinforced magnesium-aluminum alloy material preparation technology is still lacking at present.
Disclosure of Invention
The invention aims to provide a novel preparation technology of a reinforced silicon phase magnesium alloy material. It is prepared by adding TiO coating into magnesium-aluminum alloy material2The wettability of the treated graphene oxide is improved due to the coating layer. The ultrasound is continued during the solidification process to resolve re-agglomeration during the solidification process. Re-dispersing the graphene oxide by a secondary hot extrusion method at a later stage to achieve a dispersion strengthening phase and refine Mg17Al12The purpose of the phases. Compared with the traditional casting or pressure casting, the method has the advantages of wide selection range of applicable base materials, strong customization performance, good bonding performance and the like. In addition, it is known from the current experimental results that Mg is caused to be solidified due to the excellent thermal conductivity of graphene oxide17Al12The phase heat can be quickly transferred out, and the supercooling degree is increased, so that the Mg can be enabled to be added by the graphene added by the method17Al12The phases are refined to a certain degree and are crushed, rounded and dispersed in the extrusion process.
The invention is realized by the following technical scheme.
The method for reinforcing the magnesium-aluminum matrix composite by using the titanium oxide coated graphene oxide comprises the following steps.
(1) Carrying out ultrasonic pre-dispersion on graphene oxide in analytically pure ethanol for 1-3 h at room temperature, and controlling the whole process to be free of water vapor. The ratio of the graphene oxide to the ethanol is 0.2-0.4 g to 50 ml.
(2) Pouring the graphene oxide 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 h. 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. Putting the whole reaction kettle into a reaction furnace for heating, heating to 70-110 ℃ at a speed of 1-5 ℃/min, preserving heat for 1-2 h, heating to 175-180 ℃ at a speed of 1-3 ℃/min, preserving heat for 10-15 h, and taking out the reaction kettle; the reaction kettle can be opened after air cooling to room temperature.
(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 roasting the powder at 450-500 ℃ under the protection of argon. The time is controlled to be 1-3 h. The graphene oxide with the needle-shaped anatase titanium oxide coating on the surface can be obtained.
(6) Placing the graphene oxide with the titanium oxide coating, the mass fraction of which is 4-15% of the magnesium alloy powder, in methanol for low-time ultrasonic oscillation to obtain mixed powder suspension, wherein the time is not more than 30min, and then drying in a vacuum drying oven.
(7) And (4) introducing the mixed material obtained in the step (6) into a ball milling crucible for ball milling, introducing argon for protection in the ball milling process, and controlling the rotating speed to be 300-350 rpm.
(8) And (4) carrying out cold pressing treatment on the mixed material obtained in the step (7) to obtain a round bar-shaped blank, carrying out hot extrusion on the blank in a temperature field of 100-150 ℃, controlling the extrusion ratio to be 32-45, cutting the obtained bar-shaped blank into a graphene oxide prefabricated body with the height of about 5mm, and keeping for later use.
(9) Melting the corresponding magnesium-aluminum-based material in a muffle furnace, then transferring the melt into a self-made crucible with bottom ultrasonic equipment for constant temperature treatment, controlling the temperature near a liquidus line, and controlling the ultrasonic power to be 0.7-2.1 Kw. Controlling the temperature to be near the liquidus line of the corresponding alloy, introducing the prefabricated body obtained in the step (8) into the melt in different directions at the speed of 0.7-1.0 g/min, and carrying out argon protection in the whole process.
(10) And (4) introducing the melt obtained in the step (9) into a groove of a precoated sand mold for cooling, wherein the mold is preheated to 150-250 ℃, the mold is also continuously subjected to ultrasonic treatment in the melt introduction process until the melt is solidified, the ultrasonic power is controlled to be 0.7-2.8 Kw, and the process needs to be laterally introduced by argon to prevent combustion.
(11) And (3) carrying out channel-changing plastic hot extrusion treatment on the molded material obtained in the step (10), controlling the temperature to be 150-200 ℃, controlling the pressure head to be 0.4-1.2 mm/s, and controlling the extrusion ratio to be 11-32.
(12) And (3) carrying out equal-diameter angular hot extrusion on the bar obtained in the step (11) for 2-8 times, controlling the temperature to be 100-250 ℃, controlling the pressure head to be at the speed of 0.2-1.5 mm/s, and controlling the rotation angle to be 90-150 degrees.
The inner lining of the hydrothermal reaction kettle in the step (3) is made of polytetrafluoroethylene.
The invention has the following technical effects: (1) the solution adopts ethanol instead of water, participates in the reaction per se, increases the volatility, has higher pressure intensity, and is beneficial to reducing the surface tension of the solution. (2) The method is simple and effective and is suitable for batch production. (3) The method does not need expensive instruments, and has lower reaction temperature and low danger coefficient. (4) The graphene oxide is continuously dispersed under the action of ultrasound in the solidification process of the aluminum alloy material, has a better interface, and avoids the agglomeration of the graphene oxide under the fusion casting condition. (5) Due to the structural particularity of the graphene oxide, the graphene oxide is extremely difficult to disperse, the material defects are reduced in the secondary extrusion process, the graphene oxide is re-dispersed in the extrusion process, and simultaneously, Mg17Al12The phase is also better refined and rounded, and the crystal grains are also better refined. (6) The graphene oxide absorbs Ti ions by utilizing functional groups on the surface and forms TiO in the later vacuum roasting process2The coating layer effectively improves the wettability and the associativity of the graphene oxide in the matrix.
Detailed Description
The invention will be further illustrated by the following examples.
Example 1.
Carrying out ultrasonic pre-dispersion on graphene oxide in an analytically pure ethanol clock for 1h, wherein the temperature is room temperature, and the whole process is controlled to be free of water vapor. 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 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 graphene oxide with the needle-shaped anatase titanium oxide coating on the surface can be obtained.
Melting the AM60 magnesium-aluminum material in a muffle furnace, and then transferring the melt into a self-made crucible with a bottom ultrasonic device for constant temperature treatment. Controlling the temperature at 650 ℃, introducing the obtained intermediate alloy extruded by the graphene oxide and the magnesium powder into the melt at a speed of 0.7g/min in different directions, and controlling the ultrasonic treatment at 0.7Kw under the protection of argon in the whole process. The material obtained is introduced into the corresponding sand-coated mold recess and cooled, the mold being preheated to 150 ℃ and the mold likewise being subjected to ultrasound treatment during the introduction of the melt until the melt solidifies. Then, the obtained section material is subjected to secondary hot extrusion treatment, the temperature is controlled to be 200 ℃, the pressure head is controlled to be 0.4mm/s, the extrusion ratio is controlled to be 45, then, 3 times of equal channel angular extrusion is carried out under the condition of 100 ℃, and the rotation angle is controlled to be 130 degrees.
Example 2.
Carrying out ultrasonic pre-dispersion on graphene oxide in an analytically pure ethanol clock for 3 hours at room temperature, and controlling the whole process to be free of water vapor. 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: 0.8. 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, heating to 90 ℃ at the speed of 3 ℃/min, preserving heat for 1h, heating to 180 ℃ at the speed of 2 ℃/min, and preserving heat for 12 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 1 h. The graphene oxide with the needle-shaped anatase titanium oxide coating on the surface can be obtained.
And melting the AZ61 magnesium-aluminum material in a muffle furnace, and then transferring the melt into a self-made crucible with a bottom ultrasonic device for constant-temperature treatment. Controlling the temperature at 660 ℃, introducing the obtained intermediate alloy extruded by the graphene oxide and the magnesium powder into the melt in different directions at the speed of 1g/min, and controlling the ultrasonic treatment at 1.4Kw under the protection of argon in the whole process. The material obtained is introduced into the groove of a corresponding precoated sand mold for cooling, wherein the mold is preheated to 150 ℃, and the ultrasonic treatment is also continuously carried out on the mold during the introduction of the melt until the melt is solidified, and the ultrasonic treatment is controlled at 1.4 Kw. Then, the obtained section material is subjected to secondary hot extrusion treatment, the temperature is controlled to be 150 ℃, the pressure head is controlled to be at the speed of 0.7mm/s, the extrusion ratio is controlled to be 11, then, the equal-diameter angular extrusion is carried out for 3 times under the condition of 230 ℃, and the rotation angle is controlled to be 100 degrees.
Example 3.
Carrying out ultrasonic pre-dispersion on graphene oxide in an analytically pure ethanol clock for 2 hours at room temperature, and controlling the whole process to be free of water vapor. The volume ratio is strictly controlled at 0.4:50, 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, 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 1 ℃/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 500 ℃ under the protection of argon. The time is controlled to be 1 h. The graphene oxide with the needle-shaped anatase titanium oxide coating on the surface can be obtained.
And melting the AZ91D magnesium-aluminum material in a muffle furnace, and then transferring the molten magnesium-aluminum material into a self-made crucible with a bottom ultrasonic device for constant-temperature treatment. Controlling the temperature at 660 ℃, introducing the obtained GO and the intermediate alloy extruded by the magnesium powder into the aluminum liquid in different directions at the speed of 0.6g/min, and controlling the ultrasonic wave at 2.1Kw under the protection of argon in the whole process. The material obtained is introduced into a groove of a corresponding precoated sand mold for cooling, wherein the mold is preheated to 200 ℃, and the ultrasonic treatment is also continuously carried out on the mold during the introduction of the melt until the melt is solidified, and the ultrasonic treatment is controlled at 2.1 Kw. Then, the obtained section material is subjected to secondary hot extrusion treatment, the temperature is controlled to be 150 ℃, the pressure head is controlled to be at the speed of 1mm/s, the extrusion ratio is controlled to be 16, then, 6 times of equal-diameter angular extrusion is carried out at the temperature of 200 ℃, and the rotation angle is controlled to be 90 degrees.
Claims (1)
1. A preparation method of a titanium oxide/graphene oxide coated reinforced aluminum-magnesium-containing base material is characterized by comprising the following steps:
(1) carrying out ultrasonic pre-dispersion on graphene oxide in analytically pure ethanol for 1-3 h at room temperature, controlling no water vapor in the whole process, wherein the ratio of the graphene oxide to the ethanol is 0.2-0.4 g: 50 ml;
(2) pouring the graphene oxide dispersion liquid pretreated in the step (1) into a precursor liquid composed of glycerol and tetraisopropyl titanate, sealing, and carrying out ultrasonic treatment for 1-1.5 h again, wherein the volume ratio of the glycerol to the tetraisopropyl titanate is 10:0.4 to 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 whole reaction kettle in a reaction furnace, heating to 70-110 ℃ at 1-5 ℃/min, preserving heat for 1-2 h, heating to 175-180 ℃ at 1-3 ℃/min, preserving heat for 10-15 h, taking out the reaction kettle, and air cooling the reaction kettle to room temperature;
(4) taking out the solution obtained in the step (3), centrifuging, pouring analytically pure ethanol, centrifuging for multiple times until the solution is colorless, controlling the rotating speed at 9000-16000 rpm, and sealing the whole process 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; controlling the time to be 1-3 h, and obtaining graphene oxide with a needle-shaped anatase titanium oxide coating on the surface;
(6) putting graphene oxide with a titanium oxide coating layer, the mass fraction of which is 4-15% of magnesium alloy powder, into methanol, performing low-power ultrasonic oscillation to obtain a mixed powder suspension, wherein the time is less than or equal to 30min, and then drying in a vacuum drying oven;
(7) introducing the mixed material obtained in the step (6) into a ball milling crucible for ball milling, introducing argon for protection in the ball milling process, and controlling the rotating speed to be 300-350 rpm;
(8) performing cold pressing treatment on the mixed material obtained in the step (7) to obtain a round bar-shaped blank, performing hot extrusion in a temperature field of 100-150 ℃, controlling the extrusion ratio to be 32-45, and cutting the obtained bar-shaped blank into a graphene oxide prefabricated body with the height of 5mm for later use;
(9) melting the corresponding magnesium-aluminum-based material in a muffle furnace, then transferring the melt into a self-made crucible with bottom ultrasonic equipment for constant temperature treatment, controlling the temperature to be near a liquidus, controlling the ultrasonic power to be 0.7-2.1 kW, controlling the temperature to be near the liquidus of the corresponding alloy, guiding the preform obtained in the step (8) into a melt in different directions at the speed of 0.7-1.0 g/min, and carrying out argon protection in the whole process;
(10) introducing the melt obtained in the step (9) into a groove of a precoated sand mold for cooling, preheating the mold to 150-250 ℃, continuously carrying out ultrasonic treatment on the mold in the melt introduction process until the melt is solidified, controlling the ultrasonic power at 0.7-2.8 kW, and introducing the melt into the side of the mold by using argon to prevent combustion;
(11) carrying out channel-changing plastic hot extrusion treatment on the molded material obtained in the step (10), controlling the temperature to be 150-200 ℃, controlling the pressure head to be 0.4-1.2 mm/s, and controlling the extrusion ratio to be 11-32;
(12) carrying out equal-diameter angular hot extrusion on the bar obtained in the step (11), wherein the times are 2-8, the temperature is controlled to be 100-250 ℃, the pressure head is controlled to be at the speed of 0.2-1.5 mm/s, and the rotation angle can be controlled to be 90-150 degrees;
and (4) the lining of the hydrothermal reaction kettle in the step (3) is polytetrafluoroethylene.
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