CN110358943B - Method for preparing aluminum-based composite material by cooperation of alterant and carbon nano material - Google Patents
Method for preparing aluminum-based composite material by cooperation of alterant and carbon nano material Download PDFInfo
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Abstract
A method for preparing an aluminum-based composite material by the cooperation of a modifier and a carbon nano material comprises the steps of putting a matrix alloy into a crucible, heating to 740-750 ℃, adding Al-Sr intermediate blocks in batches after melting, wherein the addition amount of Sr accounts for 0.04-0.06 wt% of the total weight of a melt, and simultaneously applying ultrasound, wherein an ultrasonic probe extends into the melt by about 3-5mm, the ultrasonic power is 1.4-2.8kW, the frequency is 20kHZ, and the time is 5-10 min. After the ultrasonic treatment is finished, the temperature of the melt is raised to 770-780 ℃ and the temperature is kept for 30-40 min. And then under the protection of argon, adding Al-C intermediate blocks into the melt in batches at different angles, wherein the addition amount of carbon accounts for 0.5-1.0 wt% of the total weight of the melt, simultaneously applying ultrasonic waves for 10-15min, and pouring when the temperature of the melt is reduced to 700 ℃ after the ultrasonic waves are finished. The invention has stable process, safety and reliability, and the prepared material has uniform tissue refinement and greatly improved performance.
Description
Technical Field
The invention belongs to the technical field of metal material manufacturing, and particularly relates to a method for preparing an Al-Si-Cu composite material by the cooperation of a modifier and carbon nanofibers.
Background
The Al-Si-Cu alloy has excellent casting performance, high specific strength, small thermal expansion coefficient, good corrosion resistance and excellent electric and heat conducting performance, but alpha-Al dendrites in a casting structure are coarse, silicon phases are coarse plate-shaped or strip-shaped, and iron-rich phases are coarse long needles, which all cause the reduction of mechanical properties of the alloy, and greatly limit the application of the alloy. Research shows that the addition of a small amount of modifier in the aluminum-silicon alloy not only can achieve better refining and modification effects, but also has the effects of melt purification and degassing. Therefore, the selection of modified elements to improve the structure and the performance of the aluminum-silicon alloy has important significance. Sr is a long-acting alterant, and the aluminum-silicon alloy alterant has the advantages of less oxidation burning loss, long modification time, easy absorption, high casting yield, no corrosion to smelting tools and equipment and the like. Therefore, Sr is a good choice as the modifier of Al-Si-Cu alloy.
In published patent No. CN101871067A, the name is: in the 'strontium modified silicon-containing high-strength magnesium alloy and the preparation method thereof', the strong hydrogen absorption tendency of Sr modified alloy melt is not considered in the experimental process, and the hydrogen absorption of the melt can cause a large amount of precipitated hydrogen pores on a casting, reduce the surface quality and various properties of the casting, and cause hydrogen embrittlement when the surface quality and various properties of the casting are serious; in addition, this patent does not consider the uniformity of Sr modification, and segregation is likely to occur.
Research shows that high-energy ultrasonic waves are introduced into the metal melt, so that the acoustic cavitation effect, the acoustic flow effect and the exhaust impurity removal effect can be generated. The transient high temperature and high pressure generated by the acoustic cavitation effect change the local balance, reduce the surface tension of the liquid surface and generate strong local impact, and can generate strong scattering effect on the agglomerated phase. Meanwhile, the jet and circulation effect generated by the acoustic flow effect promotes the further separation and homogenization of the dispersed reinforced phase in the melt. In addition, high energy ultrasound can also promote grain refinement and melt degassing.
In recent years, the application of nano-sized reinforcing phase on aluminum matrix composite materials has become a hot point of research of many scientists, and carbon nanotubes (CNTs for short) are favored because of their unique structure and excellent physicochemical properties. CNTs, a nanoscale one-dimensional carbon material, exhibits extremely excellent specific strength and specific stiffness, and has tensile strength about 100 times that of steel, and density only about 1/6 times that of steel. CNTs also have good toughness and structural stability, so the CNTs are considered as an ideal aluminum matrix composite reinforcing phase.
Under publication number CN101565782A, named: in the method for adding the carbon nano tube into the metal melt, the carbon nano tube, the metal powder and the stearic acid are subjected to ball milling in the experimental process, and the carbon nano tube is damaged in different degrees in the ball milling process; in addition, when the stearic acid as the binder is added into the high-temperature melt, the stearic acid can be strongly combusted, so that potential safety hazards exist.
In the publication No. CN101376932, entitled "carbon nanotube reinforced magnesium and aluminum matrix composite material and preparation method thereof", the carbon nanotube reinforced magnesium and aluminum matrix composite material is prepared by a powder heating and mixing rheological forming method. The method has the defect that the carbon nano tubes are easy to agglomerate under the rheological condition, which reduces the mechanical property of the material to a certain extent.
Disclosure of Invention
The invention aims to provide a preparation method of an aluminum matrix composite material synergistically enhanced by a modifier and a carbon nano material.
The invention is realized by the following technical scheme.
The method for preparing the aluminum-based composite material by the cooperation of the alterant and the carbon nano material comprises the following steps.
(1) Preparation of experimental materials. The Al-Si-Cu alloy comprises the following elements in percentage by weight: the mass percent of Si is 10.5-11.5%, the mass percent of Cu is 3.0-3.5%, and the balance is Al. The modifier Sr is added in the form of Al-Sr intermediate alloy: the weight percentage of Sr is 8% -10%, and the rest is Al. The carbon nano tube is added in the form of Al-C intermediate precast block: the mass percent of C is 5-7%, and the balance is Al. And putting the Al-Si-Cu matrix alloy, the Al-Sr intermediate alloy and the Al-C intermediate precast block material into a vacuum drying oven for drying for later use.
(2) Placing the Al-Si-Cu matrix alloy into a graphite crucible, heating to 740 and 750 ℃, and removing the surface scum after the Al-Si-Cu matrix alloy is completely melted. Then, the Al-Sr intermediate alloy is coated by aluminum foil paper and added into a graphite crucible in batches, and the total addition amount of Sr accounts for 0.04-0.06 wt% of the total weight of the melt. Adding Al-Sr and simultaneously applying high-energy ultrasonic assistance, wherein the depth of the ultrasonic horn probe extending into the melt is about 3-5mm, the ultrasonic power is 1.4-2.8kW, the ultrasonic frequency is 20kHZ, and the ultrasonic time is 5-10 min. After the ultrasonic treatment is finished, the temperature of the alloy melt is raised to 770-780 ℃, and the temperature is kept for 30-40min, so that Sr is completely dissolved in the melt.
(3) After heat preservation, adding the Al-C intermediate precast blocks cut into particles in batches according to different angles into the alloy melt, wherein the addition amount of the carbon nano fibers accounts for 0.5-1.0 wt% of the total weight of the alloy melt, applying high-energy ultrasound in the adding process, extending an ultrasonic amplitude transformer probe into the melt by about 3-5mm, wherein the ultrasound power is 1.4-2.8kW, the ultrasound frequency is 20kHZ, and the ultrasound time is 10-15 min. Argon is filled in the whole process of the casting process for protection. After the ultrasonic treatment is finished, when the temperature of the melt is reduced to 700 ℃, the melt is poured into a metal mold preheated to 300 ℃, and the aluminum matrix composite material cooperatively enhanced by the alterant Sr and the carbon nanofibers can be prepared.
The carbon nano tube is a conventional carbon nano tube sold in the market.
Preferably, the carbon nanotube of the present invention may be a vacuum vapor phase carbon nanofiber prepared by a CVD method, and the carbon nanotube has the advantages of low curvature, small diameter change, and less possibility of winding on the basis of having similar high elastic modulus and strength. The purity of the carbon nano fiber is more than 98%, the diameter is 50-200nm, and the length is 1-10 mu m. The purity of the aluminum powder is more than 99.5 percent, and the particle size is 200-300 meshes.
Further, as a preferred method for preparing the Al — C intermediate precast block according to the present invention, the following steps may be adopted: the carbon nanofibers are proportioned according to the proportion of 5-7wt.% of the mass fraction of the mixed powder (aluminum powder and carbon powder), the carbon nanofibers and absolute ethyl alcohol are mixed in a beaker, and then the beaker is placed in an ultrasonic cleaning instrument for ultrasonic dispersion treatment for 80-100min, wherein the ultrasonic power is 120W, and the frequency is 42 kHz. And then uniformly scattering aluminum powder into the alcohol and carbon nanofiber solution after ultrasonic treatment, and continuing ultrasonic treatment for 40-60 min. And after the ultrasonic treatment, putting the mixed powder alcohol solution into a constant-temperature heating magnetic stirrer for stirring, wherein the heating temperature is 50 ℃, the stirring speed is 1000r/min, and the stirring time is 60-80 min. And then putting the mixed powder into a vacuum drying oven for drying. And then putting the dried powder into a vacuum hot-pressing sintering furnace for sintering, wherein the sintering temperature is 430-450 ℃, the hot-pressing pressure is 60-80Mpa, finally obtaining an aluminum-carbon intermediate precast block, and finally cutting the precast block into small particles for later use.
According to the invention, the Al-Sr intermediate alloy is added in batches under the condition of high-energy ultrasound assistance, so that the burning loss rate is reduced, the uniformity of modification is promoted, and the hydrogen absorption phenomenon in the modification process of Sr can be effectively eliminated. For the carbon nano tube, the vacuum gas phase carbon nano fiber prepared by the CVD method is selected, is the carbon nano tube with a special structure, and has the advantages of low curvature, small diameter change, difficult winding and the like on the basis of similar high elastic modulus and strength. For the addition of the carbon nano-fiber, the Al-C intermediate precast block is added in batches at different angles along with the high-energy ultrasound, and the preparation route of the Al-C intermediate precast block is realized by a pre-dispersion and vacuum hot-pressing sintering mode, so that the structural damage of the carbon nano-fiber is effectively reduced, and the dispersion uniformity of the carbon nano-fiber in a melt is ensured. The invention integrates the advantages of the strontium and the carbon nano-fiber, and has the advantages of stable process, safety, reliability and convenient operation. The structure of the prepared aluminum matrix composite is obviously refined, the carbon nanofibers are well combined with the matrix alloy interface and are distributed uniformly, and the comprehensive mechanical property of the prepared aluminum matrix composite is greatly improved.
Drawings
FIG. 1 is a photograph showing the microstructure of an aluminum-based composite material obtained in example 2 of the present invention.
Detailed Description
The invention will be further illustrated by the following examples.
Example 1.
(1) Respectively putting Al-Si-Cu alloy (the mass percent of Si is 10.5%, the mass percent of Cu is 3.5%, and the balance is Al), Al-8Sr intermediate alloy (the mass percent of Sr is 8%), and Al-5C intermediate precast block (the mass percent of C is 5%) into a vacuum drying oven for drying and standby.
(2) Putting the matrix alloy into a graphite crucible, heating to 740 ℃, and removing the surface scum after the matrix alloy is completely melted. And then adding Al-8Sr intermediate alloy coated by aluminum foil paper in batches according to the mixture ratio, wherein the total addition amount of Sr accounts for 0.04 wt% of the total weight of the melt, and high-energy ultrasound is applied while adding Sr, the depth of the ultrasonic horn probe extending into the melt is about 3mm, the ultrasonic power is 1.4kW, the ultrasonic frequency is 20kHZ, and the ultrasonic time is 5 min. After the ultrasonic treatment is finished, the temperature of the alloy melt is raised to 770 ℃ and kept for 30min, so as to ensure that Sr is completely dissolved in the melt.
(3) After heat preservation, adding the Al-5C intermediate precast blocks cut into particles into the alloy melt in batches according to different angles, wherein the addition amount of the carbon nanofibers accounts for 0.6 wt% of the total weight of the alloy melt, applying high-energy ultrasound in the adding process, extending an ultrasonic amplitude transformer probe into the melt by about 3mm, wherein the ultrasound power is 1.4kW, the ultrasound frequency is 20kHZ, and the ultrasound time is 10 min. Argon is filled in the whole process of the casting process for protection. After the ultrasonic treatment is finished, when the temperature of the melt is reduced to 700 ℃, the melt is poured into a metal mold preheated to 300 ℃, and the aluminum matrix composite material cooperatively enhanced by the alterant Sr and the carbon fiber can be prepared.
The tensile strength and yield strength of the aluminum matrix composite material prepared under the experimental condition are respectively increased by 56.4% and 32.7% compared with those of the matrix alloy under the same condition.
Example 2.
(1) Respectively putting Al-Si-Cu alloy (the mass percent of Si is 11.0%, the mass percent of Cu is 3.2%, and the balance is Al), Al-9Sr intermediate alloy (the mass percent of Sr is 9%), and Al-6C intermediate precast block (the mass percent of carbon nano fiber is 6%) into a vacuum drying oven for drying and standby.
(2) Putting the matrix alloy into a graphite crucible, heating to 750 ℃, and removing the surface scum after the matrix alloy is completely melted. And then adding Al-9Sr intermediate alloy coated by aluminum foil paper in batches according to the mixture ratio, wherein the total addition amount of Sr accounts for 0.05 wt% of the total weight of the melt, and high-energy ultrasound is applied while adding Sr, the depth of the ultrasonic horn probe extending into the melt is about 4mm, the ultrasonic power is 2.1kW, the ultrasonic frequency is 20kHZ, and the ultrasonic time is 8 min. And then heating the alloy melt to 780 ℃ and preserving the temperature for 35min to ensure that Sr is completely dissolved into the melt.
(3) After heat preservation, adding the Al-6C intermediate precast blocks cut into particles into the alloy melt in batches according to different angles, wherein the addition amount of C accounts for 0.8 wt% of the total weight of the alloy melt, applying high-energy ultrasound in the adding process, extending an ultrasonic horn probe into the melt for about 4mm, the ultrasound power is 2.1kW, the ultrasound frequency is 20kHZ, and the ultrasound time is 13 min.
Argon is filled in the whole process of the casting process for protection. After the ultrasonic treatment is finished, when the temperature of the melt is reduced to 700 ℃, the melt is poured into a metal mold preheated to 300 ℃, and the aluminum matrix composite material cooperatively enhanced by the alterant strontium and the carbon fiber can be prepared.
The tensile strength and yield strength of the aluminum matrix composite material prepared under the experimental condition are respectively increased by 67.8% and 40.3% compared with those of the matrix alloy under the same condition.
As can be seen from the attached figure 1, the crystal grains are fine and round, the carbon nano fibers are distributed more uniformly, the structure is refined to a greater degree, and therefore, the comprehensive mechanical property of the material is greatly improved.
Example 3.
(1) Respectively putting Al-Si-Cu alloy (the mass percent of Si is 11.5%, the mass percent of Cu is 3.0%, and the balance is Al), Al-10Sr intermediate alloy (the mass percent of Sr is 10%), and Al-7C intermediate precast block (the mass percent of carbon nano fiber is 7%) into a vacuum drying oven for drying and standby.
(2) Putting the matrix alloy into a graphite crucible, heating to 740 ℃, and removing the surface scum after the matrix alloy is completely melted. And then adding Al-10Sr intermediate alloy coated by aluminum foil paper in batches according to the mixture ratio, wherein the total addition amount of Sr accounts for 0.06 wt% of the total weight of the melt, high-energy ultrasound is applied while adding Sr, the depth of the ultrasonic horn probe extending into the melt is about 5mm, the ultrasonic power is 2.8kW, the ultrasonic frequency is 20kHZ, and the ultrasonic time is 10 min. And then heating the alloy melt to 780 ℃ and preserving the temperature for 40min to ensure that Sr is completely dissolved into the melt.
(3) After heat preservation is finished, adding the Al-7C intermediate precast blocks cut into particles into the alloy melt in batches according to different angles, wherein the addition amount of the carbon nano fibers accounts for 1.0 wt% of the total weight of the alloy melt, applying high-energy ultrasound in the adding process, extending an ultrasonic amplitude transformer probe into the melt by about 5mm, the ultrasound power is 2.8kW, the ultrasound frequency is 20kHZ, and the ultrasound time is 15 min. Argon is filled in the whole process of the casting process for protection. After the ultrasonic treatment is finished, when the temperature of the melt is reduced to 700 ℃, the melt is poured into a metal mold preheated to 300 ℃, and the aluminum matrix composite material cooperatively enhanced by the alterant strontium and the carbon fiber can be prepared.
The tensile strength and yield strength of the aluminum matrix composite material prepared under the experimental condition are respectively increased by 62.9% and 35.5% compared with those of the matrix alloy under the same condition.
Claims (2)
1. A method for preparing an aluminum matrix composite material by the cooperation of a modifier and a carbon nano material is characterized by comprising the following steps:
(1) preparing materials: the Al-Si-Cu alloy comprises the following elements in percentage by weight: the mass percent of Si is 10.5-11.5%, the mass percent of Cu is 3.0-3.5%, and the balance is Al; the modifier Sr is added in the form of Al-Sr intermediate alloy: the mass percent of Sr is 8-10%, and the balance is Al; the carbon nano material is added in the form of an Al-C intermediate precast block: the mass percent of C is 5-7%, and the balance is Al; putting the Al-Si-Cu matrix alloy, the Al-Sr intermediate alloy and the Al-C intermediate precast block material into a vacuum drying oven to be dried for later use;
(2) placing the Al-Si-Cu matrix alloy into a graphite crucible, heating to 740 and 750 ℃, and removing the surface scum after the Al-Si-Cu matrix alloy is completely melted; then coating Al-Sr intermediate alloy with aluminum foil paper, and adding the Al-Sr intermediate alloy into a graphite crucible in batches, wherein the total addition of Sr accounts for 0.04-0.06 wt% of the total weight of the melt; adding Al-Sr and simultaneously applying high-energy ultrasonic assistance, wherein the depth of the ultrasonic horn probe extending into the melt is 3-5mm, the ultrasonic power is 1.4-2.8kW, the ultrasonic frequency is 20kHz, and the ultrasonic time is 5-10 min; after the ultrasonic treatment is finished, heating the alloy melt to 770-780 ℃, and preserving the heat for 30-40min to ensure that Sr is completely dissolved in the melt;
(3) after heat preservation, adding the Al-C intermediate precast blocks cut into particles in batches according to different angles into the alloy melt, wherein the addition amount of the carbon nano material accounts for 0.5-1.0 wt% of the total weight of the alloy melt, applying high-energy ultrasound in the adding process, extending an ultrasonic horn probe into the melt for 3-5mm, the ultrasound power is 1.4-2.8kW, the ultrasound frequency is 20kHz, and the ultrasound time is 10-15 min; filling argon gas in the whole process of the casting process for protection; after the ultrasonic treatment is finished, when the temperature of the melt is reduced to 700 ℃, pouring the melt into a metal mold preheated to 300 ℃, thus obtaining the aluminum matrix composite material cooperatively enhanced by the alterant Sr and the carbon nano material;
the carbon nano material is vacuum gas phase carbon nano fiber prepared by a CVD method.
2. The method for preparing aluminum matrix composite material by using alterant and carbon nano material in cooperation as claimed in claim 1, wherein said Al-C intermediate precast block is prepared by the following steps: mixing carbon nanofibers and absolute ethyl alcohol in a beaker, and then putting the mixture into an ultrasonic cleaning instrument for ultrasonic dispersion treatment for 80-100min, wherein the ultrasonic power is 120W, and the frequency is 42 kHz; then uniformly scattering aluminum powder into the anhydrous ethanol and carbon nanofiber solution after ultrasonic treatment, and continuing ultrasonic treatment for 40-60 min; after the ultrasonic treatment, the mixed material is stirred under the action of a constant-temperature heating magnetic stirrer, the heating temperature is 50 ℃, the stirring speed is 1000r/min, and the stirring time is 60-80 min; then putting the mixed powder into a vacuum drying oven for drying; and then putting the dried powder into a vacuum hot-pressing sintering furnace for sintering, wherein the sintering temperature is 430-450 ℃, the hot-pressing pressure is 60-80MPa, finally obtaining an aluminum-carbon intermediate precast block, and finally cutting the precast block into small particles for later use.
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| CN112941360B (en) * | 2021-01-11 | 2022-05-20 | 南昌大学 | Preparation method of carbon nano tube reinforced aluminum alloy semi-solid slurry |
| CN112941359A (en) * | 2021-01-11 | 2021-06-11 | 南昌大学 | Preparation method of refined aluminum alloy semi-solid structure |
| CN113088742B (en) * | 2021-02-20 | 2022-05-20 | 南昌大学 | Preparation method of modifier and graphene composite refined magnesium alloy semi-solid structure |
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